guidelines for trouble shooting and maintenance of icp-ms ... for... · guidelines for trouble...
TRANSCRIPT
Guidelines for
Trouble Shooting and
Maintenance of ICP-MS Systems
ICP-MS Maintenance amp Trouble Shooting
May 2012
Flame AAS
ICP-MS
AAS instruments can be
flame only furnace only or
combined (switchable)
4100 MP-AES
ICP-OES
Graphite Furnace AAS
ICP-QQQ
Todayrsquos Agilent Atomic Spectroscopy Worldrsquos best most complete atomic spectroscopy portfolio
ICP-MS Maintenance amp Trouble Shooting
May 2012 2
Agilentrsquos Atomic Spectroscopy Portfolio - Features
Lowest price
bull Single element
bull DLs typically ~100rsquos ppb
bull Fast (for 1 element)
bull Good elemental coverage
bull Low running cost
Lowest running cost
bull Multi element
bull DLs typically single to 10rsquos ppb
bull Faster
bull Broader elemental coverage
bull Lowest running cost
Trace levels at lowest price
bull Single element
bull DLs typically 10rsquos to 100rsquos ppt
bull Very slow
bull Limited elemental coverage
bull Moderate running cost
Fastest measurement
bull Multi element
bull DLs typically single ppb
bull Very fast
bull Can measure most elements
bull High running cost
Broadest coverage
bull Multi element
bull DLs typically single or sub-ppt
bull Fast
bull Can measure almost all elements
bull Highest running cost
Lowest Selling Price Highest
Flame AA MP-AES Furnace AA ICP-OES ICP-MS
3
ICP-MS Maintenance amp Trouble Shooting
May 2012
Common ICP-MS Problems Reported by Users
Sensitivity
bull Sensitivity is worse than it used to be
bull I have a new application and I canrsquot get the sensitivity I need
bull How come I canrsquot get the instrument to meet published detection limits
Precision
bull Sensitivity is acceptable but precision is terrible
Accuracy
bull Instrument does not give the ldquorightrdquo results
Poor Sample Throughput
bull The instrument throughput needs to improve
bull Nebulizer andor Injector of the Torch blocks too quickly
4
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sensitivity - What Impacts This
4 areas of the instrument can affect sensitivity
ndash Sample introduction system
ndash Method parameters
ndash Cleanliness
ndash Quality of standards used for calibration
Remember ndash SMCQ
Or
ldquoSystem Must Create Qualityrdquo
5
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sensitivity ndash Quality of Standards
ndash What concentration are they
bull Low concentration standards have a finite life
ndash Prepare ppb (ugL) concentration standards daily from high conc stock
ndash Prepare low ppm (mgL) concentration standards weekly
ndash How are they prepared
bull Ensure purchased standards are still within ldquoUse Byrdquo date when used
bull Use calibrated pipettes and class lsquoArsquo volumetric flasks for dilutions
bull Use de-ionized water (Type I - conductivity gt 18 Mcm3) ndash lower grades may have
contamination
bull Please donrsquot do that 1100000 dilution
bull Donrsquot pipette direct from the bottle or return excess standard back to the bottle
ndash How are they stored
bull Plastic vessels ensure better stability
bull Stabilize with acid ndash low pH ensures better stability
6
ICP-MS Maintenance amp Trouble Shooting
May 2012
Detector
③Ion Transmission
Efficiency
②Plasma Ionization
Efficiency
①Nebulizer
Efficiency
7
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sensitivity ndash Itrsquos Determined Byhellip
Low ICP-MS Sensitivity
What to Check
ndash Standards prepared correctly and fresh
ndash Check the pump tubing (see tips on later slide)
and confirm pumping liquid smoothly
ndash Check for nebulizer blockage (use ldquonebulizer testrdquo in SW)
bull If required remove nebulizer and check liquid flowaerosol formation
ndash Check for blockage in the injector of the torch
bull Aspirate a Y solution
bull Check the position of ldquobulletrdquo in the plasma
bull Should be stable
ndash Check the interface cones (see tips on later slide)
ndash Check the ion lens (use ldquoion lens testrdquo in SW)
ndash Check torch positioning and tuning
ndash Check sensitivity in ldquono gas moderdquo ndash if OK suspect reaction gas purity
8
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sensitivity - Peristaltic Pump Tubing
bull Selection of tubing used for an application based on 2 key factors
ndash Resistance to the solvent in use
ndash ID of the tubing required (indicated by the coloured tabs)
bull Usersrsquo usually know what size they need
ndash Sample ndash 102 mm ID or whitewhite tabs
ndash Drain ndash 152 mm ID or yellowblue tabs
bull Smaller sizes used when application demands it
ndash Internal standard ndash 019 mm ID with orangered tabs
or 025 mm ID with orangeblue tabs
9
ICP-MS Maintenance amp Trouble Shooting
May 2012
Trim to 5-10mm to
reduce washout
and contamination
Potential Pump Tube Problems
10
ICP-MS Maintenance amp Trouble Shooting
May 2012
What to Check
ndash Tubing diameters
bull Want tubing used for waste to be larger ID than sample ID
ndash Chemical compatibility
bull Ensure tubing is resistant to the solvent being used
ndash Tube lifetime
bull Typical lifetime is ~1 week based on normal 8 hour working day
ndash Detach from tube holder after use ndash allows tube to ldquorelaxrdquo
bull Check 2 key things on pump tubing
ndash Roundness of tube ndash should not be any ldquoflatrdquo spots
ndash Tubing should still be elastic ndash replace if obviously stretched
bull Using ldquooldrdquo tubing can lead to problems with precision and stability
bull Installation and tensioning critical
ndash Donrsquot overtighten ndash just need smooth and even sample flow
ndash Remember to check other tubing for wear leaks and crimps
Normal wear amp tear
(~5 days) needs
replacing
ICP-MS Sensitivity ndash Method Parameters
What to Check
ndash Isotope selection
bull Using the most sensitive isotope
ndash Pump speed
bull Use the default speed as guide
bull Change pump tubing to give resistance to the solvent
ndash Interferences
bull Check for polyatomic interferences ndash try an alternate isotope first (if required)
ndash Otherwise use ORS3 to remove
bull Physical interferences can affect aerosol formation
ndash Use internal standard matched standards or standard additions
bull Chemical interferences can reduce atom formation and ionization
ndash Use higher RF power optimize neb flow + appropriate matrix modifiers
11
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sensitivity ndash Automated ldquoExpertrdquo Tuning
bull Startup provides a simple
user-configured schedule of
system optimization and
performance checks
bull One-click expert autotuning for
simple plasma optimization
bull Ensures consistent
performance from day to day
bull Independent of operator
experience
bull Automatically generate a
Performance Report
bull Provides a continuing record of
system performance
12
ICP-MS Maintenance amp Trouble Shooting
May 2012
13
Hardware Performance Report
is run under ldquostandardrdquo (factory
check-out) conditions
Gives record of performance
history under consistent default
tuning conditions
Note this is different to the ldquoTune
Reportrdquo which is generated
using Batch tune conditions
Sensitivity ndash Performance Report
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS specific contamination concerns -This is a topic of its own often leads to the clean room
conversation
But remember its not just where your instrument
is located ndash itrsquos everything the sample encounters
on its way to the instrument
ICP-MS Maintenance amp Trouble Shooting
May 2012 14
Sensitivity ndash Cleanliness amp Contamination
Sensitivity ndash Contamination Sources
bull Use high purity or ICP-MS grade reagents
bull Acid purity
ndash Buy only what you need to do the job
ndash Check the certificate of analysis
ndash Donrsquot insert pipette tips into your acids
ndash Use contaminated acid for cleaning
bull Sample containers
ndash Borosilicate glass introduces boron
ndash FEP containers preferred
bull Pipette tips
ndash Colors add interest ndash but increase contamination (Cu Fe Zn Cd)
bull Gloves
ndash Powder free unless you like Zn
Anything that touches sample during prep dilution
transfer analysis and storage
ICP-MS Maintenance amp Trouble Shooting
May 2012 15
PFA spray
chamber
PFA
endcap
PFA
nebulizer
PFA
connector
tube
Quartz torch with sapphire
or platinum injector
Complete sample introduction can be
changed to a system specifically
designed to reduce contamination
bull Usually used for semi-con applications
Clean integrated Auto-Sampler ndash I-AS
Clean sample introduction system - PFA
16
Cleanliness ndash The Ultimate for Contamination Free
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sensitivity ndash System Cleanliness
What to Check
ndash Sample Introduction System
bull Deposits in nebulizer can reduce
sample uptake rate
ndash Soak in aqua regia or use a nebulizer
cleaning tool to back flush
bull Solid material in torch injector
affects aerosol introduction into
plasma and increases noise
bull Contamination in spray chamber
impacts on aerosol formation ndash
increases noise
bull If seeing poor precision may be
due to beading in spray chamber
ndash Soak in 25 detergent solution
overnight (preferably for 24 hours)
17
ICP-MS Maintenance amp Trouble Shooting
May 2012
Nebulizer cleaner
Agilent PN G3266-80020
ICP-MS Sensitivity ndash System Cleanliness
What to Check
ndash Interface cones
bull Deposits or discoloration indicates
cleaning is required
bull Other indicators that cone cleaning
is required
ndash Poor sensitivity
ndash High background
ndash Distorted peak shapes
ndash Changes in interface vacuum reading
(deposition or build-up)
18
ICP-MS Maintenance amp Trouble Shooting
May 2012
Close up
Sample cone after measuring 75 undiluted sea water
samples using HMI Some deposition on outer edges
away from the orifice ndash no blockage of the sampling
orifice ndash but cleaning still recommended
System Cleanliness - Sampling Cone
1 mm Orifice Nickel or Platinum Centres
bull Nickel
bull Physically stronger
bull Tip runs hotter ndash less sample deposition
bull Platinum
bull Chemically stronger
bull Used for higher acid conc (incl HF)
bull 2 centre sizes 10-18 mm
bull Higher cost
Potential Problems
bull Biggest risk is physical damage to the orifice due to excessively aggressive cleaning
bull Cones also affected by sample matrix (acid strength amp type) and number of samples analyzed each day
bull Nickel - Typically replace 3 or 5 each year (assumes measuring 250-350 environmental samples each day)
bull Platinum - Typically replace 1 or 2 each year (assumes measuring 20-50 semiconductor samples each day)
bull If not clean then can result in analytical problems eg poor signal stability elemental contamination
ICP-MS Maintenance amp Trouble Shooting
May 2012 19
System Cleanliness - Skimmer Cone
04 mm Orifice Nickel or Platinum
bull The Nickel skimmer cone is the standard interface
bull The skimmer cone is relatively robust to samples containing high concentrations of matrix and salts and is suitable for a wide variety of samples It is usually used with the Nickel sampling cone
bull The Platinum skimmer cone is usually used for introduction of hydrofluoric acid and other reagents It is usually used with the Platinum sampling cone
Potential Problems
bull Biggest risk is from physical damage to the orifice due to excessively aggressive cleaning
bull Cones also affected by sample matrix (acid strength amp type) and number of samples analyzed each day
bull Nickel ndash Typically replace 3 or 5 each year (assumes measuring 250-350 environmental samples each day)
bull Platinum ndash Typically replace 1 or 2 each year (assumes measuring 20-50 semiconductor samples each day)
bull If not clean then can result in analytical problems eg poor signal stability elemental contamination
20
ICP-MS Maintenance amp Trouble Shooting
May 2012
System Cleanliness - Cone Cleaning Procedure
Caution - Take care to avoid damage to the cone tip when removing ndash and place base down - Check the graphite gasket and replace if creased or damaged - Sonicate in a 2 Citranox or 2 Nitric Acid solution for a few minutes - Rinse well with de-ionized water - If still dirty or memory problems remain polish using an alumina powder slurry on a Q-tip then sonicate in 2 Citranox solution and rinse well with de-ionized water - Dry with nitrogen before installing
22
ICP-MS Maintenance amp Trouble Shooting
May 2012
Precision - Why is This Important
What does ldquoPrecisionrdquo mean
ndash Ability to get the same result for the same
sample when measured multiple times
ndash Usually measured as RSD or sometimes SD
RSD = (SD Mean Result) 100
ndash Low values indicate good precision
bull For ICP-MS expect 1-2 RSD
Why is this important
ndash User loses confidence in the system
What impacts on precision
ndash Nebulizerplasma stability
ndash Sample introduction system
ndash Method parameters
23
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash System stabilized
bull Allow 10 mins for plasma warm-up before
analysis
ndash Plasma status
bull ldquoBulletrdquo in the plasma should be stable
bull Check for deposits in the injector of the torch
ndash Check condition of interface cones and
clean if necessary
ndash Clean the Extraction Lens - Omega Lens
assembly
ndash Method parameters
bull Appropriate times set for sample uptake
delay and stabilization times
24
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash Sample Intro
What to Check ndash Nebulizer
bull Nebulizer type used can impact on sensitivity and precision
ndash MicroMist (glass concentric type) is the standard nebulizer ndash handles most sample
types
ndash PFA MicroFlow nebulizer best for low volume samples aggressive samples (HF
digests) and when low contamination required (semi-con)
ndash Babington gives poorer precision - best for high TDS samples
bull Check nebulizer condition regularly
ndash Chips in the nebulizer tip impact on aerosol formation ndash poor precision
(use a magnifying glass if necessary)
ndash Check for deposits or blockage in the tip
bull Sample uptake or flow rate
ndash Lower pump speed or using narrow bore pump tubing will reduce uptake rate
- better for high TDS samples
25
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Sample Introduction bull Contamination in the spray chamber
ndash When was the spray chamber cleaned
bull Any blockages in the nebulizer injector
ndash Check for stable aerosol formation
bull Air leaks in spray chamber end cap or connecting tubes
ndash Are they in good condition with tight connections
bull Damaged pump tubes
ndash When did you check the pump tubes
bull Is the pump speed too slow
ndash Low pump speeds may cause signal pulsation
ndash If required use narrower bore pump tube and increase pump speed
bull Samples have a high TDS content
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
26
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Memory effects
bull If possible avoid running high concentrations of these analytes
(Ag Au B Hg Mo Si Sn W Zn Zr)
ndash Maybe necessary to pre-dilute samples (if known to be high in concentration)
bull Ensure an adequate rinse time
ndash Should be at least equal to the sample uptake delay
(30-40 seconds typical)
bull May require an acidified rinse solution between samples
(2 HNO3)
bull Other strategies to minimize memory effects
ndash Use an inert spray chamber
ndash Use the ISIS to introduce discrete amounts of sample This means
bull Cones are exposed to less sample matrix = improved stability
bull Less memorycarry-over
bull Reduced uptake amp rinse times = faster measurement
27
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy - Why is This Important
What does ldquoAccuracyrdquo mean
ndash Ability to get the ldquorightrdquo answer for the sample
ndash Heavily dependent on operatorrsquos skill
Why is this important
ndash User loses confidence in the system
ndash Your reputationhellip
bull Customerrsquos question the results
bull Poor performance in ldquoround robinrdquo comparisons
How do You Confirm Accuracy
ndash Check the result for a prepared standard
ndash Measure a certified reference material
ndash Use other quality control checks to check analysis
28
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Calibration standards properly prepared
bull See earlier recommendations ndash important to match to samples prepare
accurately and use them ldquofreshrdquo
ndash Any interferences impacting on results
ndash Use matched standards or standard additions
ndash Ensure isotope selected has no polyatomic interferences
ndash If necessary use ORS3
ndash Precision optimized
bull Optimum signal to noise performance improves accuracy
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
29
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Reprocess data post
run using an
alternate internal
standard
bull Ensure Internal
Standard used is
similar in mass
bull Check whether the
Internal Standard is
present in the
sample
ndash If necessary do a Semi-
Quant measurement
bull Dilute with cal blk
matrix
30
Accuracy ndash Suspect Internal Standard Recovery
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Sample preparation
bull Is the most appropriate digestion being used
bull Are all of the analytes being quantitatively (and reproducibly) extracted and
dissolved
ndash Many digestions are only partial extracts ndash efficiency will vary with the
sample matrix
ndash Some volatile analytes may be ldquolostrdquo during digestion
bull Confirm by taking a solid certified reference material
through your preparation and analysis procedure
bull Is the digest stable ndash or are you seeing any precipitates or a suspension
bull Do you see any potential contamination from either reagents or the digestion
equipment eg especially with Si B or Ca
bull Include a ldquoReagent Blankrdquo with every sample batch to
monitor
31
ICP-MS Maintenance amp Trouble Shooting
May 2012
Laboratory environment can have
direct impact on quality of results
bull Clean uncluttered work area
bull Proper ventilation
bull Safety considerations
bull Instrument lifetime consideration
ICP-MS Maintenance amp Trouble Shooting
May 2012 32
Laboratory Environment
ICP-MS ndash Potential Autosampler Issues
ndash More customers use autosamplers with ICP for automation
ndash Issues to consider
bull Long transfer tube between sampler and ICP-MS
ndash May need to program a longer sample uptake delay
ndash May exacerbate problems with memory effects
ndash Use ldquoFast Pumprdquo during sample uptake delay
bull Caution ndash not always possible
Not recommended with high TDS samples and organics
bull Ensure probe diameter is appropriate for sample matrix
ndash Use wider bore for high TDS or viscous samples
bull Sample stability - potential for sample changes while uncovered in racks ndash impacts accuracy
ndash Dust ingress can introduce contamination
ndash Sample evaporation may occur during long unattended runs
ndash Sediment in the sample may settle out esp with wear metals or suspensions
bull Ensure transfer line to ICP-MS is in good condition
ndash Kinks in the line may cause poor uptake or pulsing in the sample
ndash Impacts on precision and accuracy
33
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sample Throughput ndash What to Check
ndash Samples fully digested
bull No excess particulates in the sample that may cause blockage
ndash Sample Introduction System optimized
ndash Capable of handling the TDS levels in the sample
ndash TorchNebulizer cleaned and ready for analysis
ndash Method parameters optimized
bull Sample uptake delay and stabilization times are appropriate ndash optimized
bull Integration time is appropriate for the expected concentration
ndash Use a longer integration time at low concentrations
bull Rinse time is appropriate
bull Use ldquoISISrdquo discrete sampling for faster measurement and faster washout
34
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Handles tough sample matrices better
than any other ICP-MS
ndash Highest plasma temperature (lowest
CeOCe) as standard
ndash HMI (high matrix introduction) allows direct
analysis of difficult samples
eg sea water
bull ORS3 operates in He collision mode to
remove ALL polyatomic interferences
ndash Enables reliable removal of all polyatomic
interferences using a single set of
conditions
ndash Gives lower levels of interference and
better long-term stability HMI gives lower suppression and
better long-term stability
Relative signal (suppression) in undiluted seawater
Long-term stability in undiluted seawater
35
Agilent ICP-MS Performance - Benefits
Best matrix tolerance amp less interferences
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS ndash Recommended Maintenance Schedule
ICP-MS Maintenance amp Trouble Shooting
May 2012 37
These functions
(and more) are
completed as part
of a Preventative
Maintenance
program by an
Agilent Field
Service Engineer
Summary ndash Key Consumables for ICP-MS
Sample preparationpresentation
ndash Peristaltic pump tubing
ndash Transfer and drain tubing
ndash ICP-MS standard solutions
ndash Internal Standard solutions
ndash Torches
ndash Spray chambers
ndash Nebulizers
Ion Extraction
ndash Sampler and skimmer cones
Autosampling
ndash Sample tubes racks probes and transfer tubing
ISIS
ndash Peristaltic pump tubing ferrules amp fittings
38
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sample Introduction
Key consumables requiring frequent replacement
bull Pump tubing
bull Torches and quartz transfer tube
bull Nebulizers
bull Spray chambers
bull Interface cones (skimmer amp sampler)
bull Transfer amp connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalogue
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24406(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 39
Autosampler Supplies
Key consumables requiring frequent replacement
ndash Peristaltic pump tubing
ndash Sample racks
ndash Sample tubes
ndash Spare probes
ndash Standard racks
ndash Connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24407(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 40
ISIS Supplies
Key consumables requiring frequent replacement
bull Peristaltic pump tubing
bull Ferrules and fittings
bull Valving
For ISIS Hydride Generation Accessory
bull Membrane filter
bull Concentric nebulizer
bull Gas-liquid separator
bull Other tubing and connectors
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceProductListingaspxcat=SubCat2ECS_24437(Agilent)amppcat=SubCat1ECS_24407(Agilent)amprcat=ClassECS_22674(Agilent)
41
ICP-MS Maintenance amp Trouble Shooting
May 2012
Where to Find the Right Consumable Analytical Consumables Agilent Assist
Consumables amp Supplies Instrument Sales ampServices 1-800-227-9770 (Option 11) 1-800-227-9770 (Option 13) wwwagilentcomchemcontactus wwwagilentcomchemcontactus
On-Line resources
ICP-MS Supplies
2nd Edition Speciation Handbook
ICP-MS Journal Archives
Recorded Agilent e-Seminars
ICP-OES Supplies
Atomic Absorption Supplies
Instrument Parts amp Supplies
Atomic Spec Application Notes
Agilent Quick Reference Guide for 77008800 ICP-MS (pub 5990-8182EN)
Agilent Atomic Spec Supplies Catalogue (pub 5990-8767EN)
Agilent Consumables Catalogue (pub 5990-6674EN)
Instrument User Manuals
42
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
Flame AAS
ICP-MS
AAS instruments can be
flame only furnace only or
combined (switchable)
4100 MP-AES
ICP-OES
Graphite Furnace AAS
ICP-QQQ
Todayrsquos Agilent Atomic Spectroscopy Worldrsquos best most complete atomic spectroscopy portfolio
ICP-MS Maintenance amp Trouble Shooting
May 2012 2
Agilentrsquos Atomic Spectroscopy Portfolio - Features
Lowest price
bull Single element
bull DLs typically ~100rsquos ppb
bull Fast (for 1 element)
bull Good elemental coverage
bull Low running cost
Lowest running cost
bull Multi element
bull DLs typically single to 10rsquos ppb
bull Faster
bull Broader elemental coverage
bull Lowest running cost
Trace levels at lowest price
bull Single element
bull DLs typically 10rsquos to 100rsquos ppt
bull Very slow
bull Limited elemental coverage
bull Moderate running cost
Fastest measurement
bull Multi element
bull DLs typically single ppb
bull Very fast
bull Can measure most elements
bull High running cost
Broadest coverage
bull Multi element
bull DLs typically single or sub-ppt
bull Fast
bull Can measure almost all elements
bull Highest running cost
Lowest Selling Price Highest
Flame AA MP-AES Furnace AA ICP-OES ICP-MS
3
ICP-MS Maintenance amp Trouble Shooting
May 2012
Common ICP-MS Problems Reported by Users
Sensitivity
bull Sensitivity is worse than it used to be
bull I have a new application and I canrsquot get the sensitivity I need
bull How come I canrsquot get the instrument to meet published detection limits
Precision
bull Sensitivity is acceptable but precision is terrible
Accuracy
bull Instrument does not give the ldquorightrdquo results
Poor Sample Throughput
bull The instrument throughput needs to improve
bull Nebulizer andor Injector of the Torch blocks too quickly
4
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sensitivity - What Impacts This
4 areas of the instrument can affect sensitivity
ndash Sample introduction system
ndash Method parameters
ndash Cleanliness
ndash Quality of standards used for calibration
Remember ndash SMCQ
Or
ldquoSystem Must Create Qualityrdquo
5
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sensitivity ndash Quality of Standards
ndash What concentration are they
bull Low concentration standards have a finite life
ndash Prepare ppb (ugL) concentration standards daily from high conc stock
ndash Prepare low ppm (mgL) concentration standards weekly
ndash How are they prepared
bull Ensure purchased standards are still within ldquoUse Byrdquo date when used
bull Use calibrated pipettes and class lsquoArsquo volumetric flasks for dilutions
bull Use de-ionized water (Type I - conductivity gt 18 Mcm3) ndash lower grades may have
contamination
bull Please donrsquot do that 1100000 dilution
bull Donrsquot pipette direct from the bottle or return excess standard back to the bottle
ndash How are they stored
bull Plastic vessels ensure better stability
bull Stabilize with acid ndash low pH ensures better stability
6
ICP-MS Maintenance amp Trouble Shooting
May 2012
Detector
③Ion Transmission
Efficiency
②Plasma Ionization
Efficiency
①Nebulizer
Efficiency
7
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sensitivity ndash Itrsquos Determined Byhellip
Low ICP-MS Sensitivity
What to Check
ndash Standards prepared correctly and fresh
ndash Check the pump tubing (see tips on later slide)
and confirm pumping liquid smoothly
ndash Check for nebulizer blockage (use ldquonebulizer testrdquo in SW)
bull If required remove nebulizer and check liquid flowaerosol formation
ndash Check for blockage in the injector of the torch
bull Aspirate a Y solution
bull Check the position of ldquobulletrdquo in the plasma
bull Should be stable
ndash Check the interface cones (see tips on later slide)
ndash Check the ion lens (use ldquoion lens testrdquo in SW)
ndash Check torch positioning and tuning
ndash Check sensitivity in ldquono gas moderdquo ndash if OK suspect reaction gas purity
8
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sensitivity - Peristaltic Pump Tubing
bull Selection of tubing used for an application based on 2 key factors
ndash Resistance to the solvent in use
ndash ID of the tubing required (indicated by the coloured tabs)
bull Usersrsquo usually know what size they need
ndash Sample ndash 102 mm ID or whitewhite tabs
ndash Drain ndash 152 mm ID or yellowblue tabs
bull Smaller sizes used when application demands it
ndash Internal standard ndash 019 mm ID with orangered tabs
or 025 mm ID with orangeblue tabs
9
ICP-MS Maintenance amp Trouble Shooting
May 2012
Trim to 5-10mm to
reduce washout
and contamination
Potential Pump Tube Problems
10
ICP-MS Maintenance amp Trouble Shooting
May 2012
What to Check
ndash Tubing diameters
bull Want tubing used for waste to be larger ID than sample ID
ndash Chemical compatibility
bull Ensure tubing is resistant to the solvent being used
ndash Tube lifetime
bull Typical lifetime is ~1 week based on normal 8 hour working day
ndash Detach from tube holder after use ndash allows tube to ldquorelaxrdquo
bull Check 2 key things on pump tubing
ndash Roundness of tube ndash should not be any ldquoflatrdquo spots
ndash Tubing should still be elastic ndash replace if obviously stretched
bull Using ldquooldrdquo tubing can lead to problems with precision and stability
bull Installation and tensioning critical
ndash Donrsquot overtighten ndash just need smooth and even sample flow
ndash Remember to check other tubing for wear leaks and crimps
Normal wear amp tear
(~5 days) needs
replacing
ICP-MS Sensitivity ndash Method Parameters
What to Check
ndash Isotope selection
bull Using the most sensitive isotope
ndash Pump speed
bull Use the default speed as guide
bull Change pump tubing to give resistance to the solvent
ndash Interferences
bull Check for polyatomic interferences ndash try an alternate isotope first (if required)
ndash Otherwise use ORS3 to remove
bull Physical interferences can affect aerosol formation
ndash Use internal standard matched standards or standard additions
bull Chemical interferences can reduce atom formation and ionization
ndash Use higher RF power optimize neb flow + appropriate matrix modifiers
11
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sensitivity ndash Automated ldquoExpertrdquo Tuning
bull Startup provides a simple
user-configured schedule of
system optimization and
performance checks
bull One-click expert autotuning for
simple plasma optimization
bull Ensures consistent
performance from day to day
bull Independent of operator
experience
bull Automatically generate a
Performance Report
bull Provides a continuing record of
system performance
12
ICP-MS Maintenance amp Trouble Shooting
May 2012
13
Hardware Performance Report
is run under ldquostandardrdquo (factory
check-out) conditions
Gives record of performance
history under consistent default
tuning conditions
Note this is different to the ldquoTune
Reportrdquo which is generated
using Batch tune conditions
Sensitivity ndash Performance Report
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS specific contamination concerns -This is a topic of its own often leads to the clean room
conversation
But remember its not just where your instrument
is located ndash itrsquos everything the sample encounters
on its way to the instrument
ICP-MS Maintenance amp Trouble Shooting
May 2012 14
Sensitivity ndash Cleanliness amp Contamination
Sensitivity ndash Contamination Sources
bull Use high purity or ICP-MS grade reagents
bull Acid purity
ndash Buy only what you need to do the job
ndash Check the certificate of analysis
ndash Donrsquot insert pipette tips into your acids
ndash Use contaminated acid for cleaning
bull Sample containers
ndash Borosilicate glass introduces boron
ndash FEP containers preferred
bull Pipette tips
ndash Colors add interest ndash but increase contamination (Cu Fe Zn Cd)
bull Gloves
ndash Powder free unless you like Zn
Anything that touches sample during prep dilution
transfer analysis and storage
ICP-MS Maintenance amp Trouble Shooting
May 2012 15
PFA spray
chamber
PFA
endcap
PFA
nebulizer
PFA
connector
tube
Quartz torch with sapphire
or platinum injector
Complete sample introduction can be
changed to a system specifically
designed to reduce contamination
bull Usually used for semi-con applications
Clean integrated Auto-Sampler ndash I-AS
Clean sample introduction system - PFA
16
Cleanliness ndash The Ultimate for Contamination Free
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sensitivity ndash System Cleanliness
What to Check
ndash Sample Introduction System
bull Deposits in nebulizer can reduce
sample uptake rate
ndash Soak in aqua regia or use a nebulizer
cleaning tool to back flush
bull Solid material in torch injector
affects aerosol introduction into
plasma and increases noise
bull Contamination in spray chamber
impacts on aerosol formation ndash
increases noise
bull If seeing poor precision may be
due to beading in spray chamber
ndash Soak in 25 detergent solution
overnight (preferably for 24 hours)
17
ICP-MS Maintenance amp Trouble Shooting
May 2012
Nebulizer cleaner
Agilent PN G3266-80020
ICP-MS Sensitivity ndash System Cleanliness
What to Check
ndash Interface cones
bull Deposits or discoloration indicates
cleaning is required
bull Other indicators that cone cleaning
is required
ndash Poor sensitivity
ndash High background
ndash Distorted peak shapes
ndash Changes in interface vacuum reading
(deposition or build-up)
18
ICP-MS Maintenance amp Trouble Shooting
May 2012
Close up
Sample cone after measuring 75 undiluted sea water
samples using HMI Some deposition on outer edges
away from the orifice ndash no blockage of the sampling
orifice ndash but cleaning still recommended
System Cleanliness - Sampling Cone
1 mm Orifice Nickel or Platinum Centres
bull Nickel
bull Physically stronger
bull Tip runs hotter ndash less sample deposition
bull Platinum
bull Chemically stronger
bull Used for higher acid conc (incl HF)
bull 2 centre sizes 10-18 mm
bull Higher cost
Potential Problems
bull Biggest risk is physical damage to the orifice due to excessively aggressive cleaning
bull Cones also affected by sample matrix (acid strength amp type) and number of samples analyzed each day
bull Nickel - Typically replace 3 or 5 each year (assumes measuring 250-350 environmental samples each day)
bull Platinum - Typically replace 1 or 2 each year (assumes measuring 20-50 semiconductor samples each day)
bull If not clean then can result in analytical problems eg poor signal stability elemental contamination
ICP-MS Maintenance amp Trouble Shooting
May 2012 19
System Cleanliness - Skimmer Cone
04 mm Orifice Nickel or Platinum
bull The Nickel skimmer cone is the standard interface
bull The skimmer cone is relatively robust to samples containing high concentrations of matrix and salts and is suitable for a wide variety of samples It is usually used with the Nickel sampling cone
bull The Platinum skimmer cone is usually used for introduction of hydrofluoric acid and other reagents It is usually used with the Platinum sampling cone
Potential Problems
bull Biggest risk is from physical damage to the orifice due to excessively aggressive cleaning
bull Cones also affected by sample matrix (acid strength amp type) and number of samples analyzed each day
bull Nickel ndash Typically replace 3 or 5 each year (assumes measuring 250-350 environmental samples each day)
bull Platinum ndash Typically replace 1 or 2 each year (assumes measuring 20-50 semiconductor samples each day)
bull If not clean then can result in analytical problems eg poor signal stability elemental contamination
20
ICP-MS Maintenance amp Trouble Shooting
May 2012
System Cleanliness - Cone Cleaning Procedure
Caution - Take care to avoid damage to the cone tip when removing ndash and place base down - Check the graphite gasket and replace if creased or damaged - Sonicate in a 2 Citranox or 2 Nitric Acid solution for a few minutes - Rinse well with de-ionized water - If still dirty or memory problems remain polish using an alumina powder slurry on a Q-tip then sonicate in 2 Citranox solution and rinse well with de-ionized water - Dry with nitrogen before installing
22
ICP-MS Maintenance amp Trouble Shooting
May 2012
Precision - Why is This Important
What does ldquoPrecisionrdquo mean
ndash Ability to get the same result for the same
sample when measured multiple times
ndash Usually measured as RSD or sometimes SD
RSD = (SD Mean Result) 100
ndash Low values indicate good precision
bull For ICP-MS expect 1-2 RSD
Why is this important
ndash User loses confidence in the system
What impacts on precision
ndash Nebulizerplasma stability
ndash Sample introduction system
ndash Method parameters
23
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash System stabilized
bull Allow 10 mins for plasma warm-up before
analysis
ndash Plasma status
bull ldquoBulletrdquo in the plasma should be stable
bull Check for deposits in the injector of the torch
ndash Check condition of interface cones and
clean if necessary
ndash Clean the Extraction Lens - Omega Lens
assembly
ndash Method parameters
bull Appropriate times set for sample uptake
delay and stabilization times
24
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash Sample Intro
What to Check ndash Nebulizer
bull Nebulizer type used can impact on sensitivity and precision
ndash MicroMist (glass concentric type) is the standard nebulizer ndash handles most sample
types
ndash PFA MicroFlow nebulizer best for low volume samples aggressive samples (HF
digests) and when low contamination required (semi-con)
ndash Babington gives poorer precision - best for high TDS samples
bull Check nebulizer condition regularly
ndash Chips in the nebulizer tip impact on aerosol formation ndash poor precision
(use a magnifying glass if necessary)
ndash Check for deposits or blockage in the tip
bull Sample uptake or flow rate
ndash Lower pump speed or using narrow bore pump tubing will reduce uptake rate
- better for high TDS samples
25
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Sample Introduction bull Contamination in the spray chamber
ndash When was the spray chamber cleaned
bull Any blockages in the nebulizer injector
ndash Check for stable aerosol formation
bull Air leaks in spray chamber end cap or connecting tubes
ndash Are they in good condition with tight connections
bull Damaged pump tubes
ndash When did you check the pump tubes
bull Is the pump speed too slow
ndash Low pump speeds may cause signal pulsation
ndash If required use narrower bore pump tube and increase pump speed
bull Samples have a high TDS content
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
26
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Memory effects
bull If possible avoid running high concentrations of these analytes
(Ag Au B Hg Mo Si Sn W Zn Zr)
ndash Maybe necessary to pre-dilute samples (if known to be high in concentration)
bull Ensure an adequate rinse time
ndash Should be at least equal to the sample uptake delay
(30-40 seconds typical)
bull May require an acidified rinse solution between samples
(2 HNO3)
bull Other strategies to minimize memory effects
ndash Use an inert spray chamber
ndash Use the ISIS to introduce discrete amounts of sample This means
bull Cones are exposed to less sample matrix = improved stability
bull Less memorycarry-over
bull Reduced uptake amp rinse times = faster measurement
27
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy - Why is This Important
What does ldquoAccuracyrdquo mean
ndash Ability to get the ldquorightrdquo answer for the sample
ndash Heavily dependent on operatorrsquos skill
Why is this important
ndash User loses confidence in the system
ndash Your reputationhellip
bull Customerrsquos question the results
bull Poor performance in ldquoround robinrdquo comparisons
How do You Confirm Accuracy
ndash Check the result for a prepared standard
ndash Measure a certified reference material
ndash Use other quality control checks to check analysis
28
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Calibration standards properly prepared
bull See earlier recommendations ndash important to match to samples prepare
accurately and use them ldquofreshrdquo
ndash Any interferences impacting on results
ndash Use matched standards or standard additions
ndash Ensure isotope selected has no polyatomic interferences
ndash If necessary use ORS3
ndash Precision optimized
bull Optimum signal to noise performance improves accuracy
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
29
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Reprocess data post
run using an
alternate internal
standard
bull Ensure Internal
Standard used is
similar in mass
bull Check whether the
Internal Standard is
present in the
sample
ndash If necessary do a Semi-
Quant measurement
bull Dilute with cal blk
matrix
30
Accuracy ndash Suspect Internal Standard Recovery
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Sample preparation
bull Is the most appropriate digestion being used
bull Are all of the analytes being quantitatively (and reproducibly) extracted and
dissolved
ndash Many digestions are only partial extracts ndash efficiency will vary with the
sample matrix
ndash Some volatile analytes may be ldquolostrdquo during digestion
bull Confirm by taking a solid certified reference material
through your preparation and analysis procedure
bull Is the digest stable ndash or are you seeing any precipitates or a suspension
bull Do you see any potential contamination from either reagents or the digestion
equipment eg especially with Si B or Ca
bull Include a ldquoReagent Blankrdquo with every sample batch to
monitor
31
ICP-MS Maintenance amp Trouble Shooting
May 2012
Laboratory environment can have
direct impact on quality of results
bull Clean uncluttered work area
bull Proper ventilation
bull Safety considerations
bull Instrument lifetime consideration
ICP-MS Maintenance amp Trouble Shooting
May 2012 32
Laboratory Environment
ICP-MS ndash Potential Autosampler Issues
ndash More customers use autosamplers with ICP for automation
ndash Issues to consider
bull Long transfer tube between sampler and ICP-MS
ndash May need to program a longer sample uptake delay
ndash May exacerbate problems with memory effects
ndash Use ldquoFast Pumprdquo during sample uptake delay
bull Caution ndash not always possible
Not recommended with high TDS samples and organics
bull Ensure probe diameter is appropriate for sample matrix
ndash Use wider bore for high TDS or viscous samples
bull Sample stability - potential for sample changes while uncovered in racks ndash impacts accuracy
ndash Dust ingress can introduce contamination
ndash Sample evaporation may occur during long unattended runs
ndash Sediment in the sample may settle out esp with wear metals or suspensions
bull Ensure transfer line to ICP-MS is in good condition
ndash Kinks in the line may cause poor uptake or pulsing in the sample
ndash Impacts on precision and accuracy
33
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sample Throughput ndash What to Check
ndash Samples fully digested
bull No excess particulates in the sample that may cause blockage
ndash Sample Introduction System optimized
ndash Capable of handling the TDS levels in the sample
ndash TorchNebulizer cleaned and ready for analysis
ndash Method parameters optimized
bull Sample uptake delay and stabilization times are appropriate ndash optimized
bull Integration time is appropriate for the expected concentration
ndash Use a longer integration time at low concentrations
bull Rinse time is appropriate
bull Use ldquoISISrdquo discrete sampling for faster measurement and faster washout
34
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Handles tough sample matrices better
than any other ICP-MS
ndash Highest plasma temperature (lowest
CeOCe) as standard
ndash HMI (high matrix introduction) allows direct
analysis of difficult samples
eg sea water
bull ORS3 operates in He collision mode to
remove ALL polyatomic interferences
ndash Enables reliable removal of all polyatomic
interferences using a single set of
conditions
ndash Gives lower levels of interference and
better long-term stability HMI gives lower suppression and
better long-term stability
Relative signal (suppression) in undiluted seawater
Long-term stability in undiluted seawater
35
Agilent ICP-MS Performance - Benefits
Best matrix tolerance amp less interferences
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS ndash Recommended Maintenance Schedule
ICP-MS Maintenance amp Trouble Shooting
May 2012 37
These functions
(and more) are
completed as part
of a Preventative
Maintenance
program by an
Agilent Field
Service Engineer
Summary ndash Key Consumables for ICP-MS
Sample preparationpresentation
ndash Peristaltic pump tubing
ndash Transfer and drain tubing
ndash ICP-MS standard solutions
ndash Internal Standard solutions
ndash Torches
ndash Spray chambers
ndash Nebulizers
Ion Extraction
ndash Sampler and skimmer cones
Autosampling
ndash Sample tubes racks probes and transfer tubing
ISIS
ndash Peristaltic pump tubing ferrules amp fittings
38
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sample Introduction
Key consumables requiring frequent replacement
bull Pump tubing
bull Torches and quartz transfer tube
bull Nebulizers
bull Spray chambers
bull Interface cones (skimmer amp sampler)
bull Transfer amp connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalogue
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24406(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 39
Autosampler Supplies
Key consumables requiring frequent replacement
ndash Peristaltic pump tubing
ndash Sample racks
ndash Sample tubes
ndash Spare probes
ndash Standard racks
ndash Connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24407(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 40
ISIS Supplies
Key consumables requiring frequent replacement
bull Peristaltic pump tubing
bull Ferrules and fittings
bull Valving
For ISIS Hydride Generation Accessory
bull Membrane filter
bull Concentric nebulizer
bull Gas-liquid separator
bull Other tubing and connectors
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceProductListingaspxcat=SubCat2ECS_24437(Agilent)amppcat=SubCat1ECS_24407(Agilent)amprcat=ClassECS_22674(Agilent)
41
ICP-MS Maintenance amp Trouble Shooting
May 2012
Where to Find the Right Consumable Analytical Consumables Agilent Assist
Consumables amp Supplies Instrument Sales ampServices 1-800-227-9770 (Option 11) 1-800-227-9770 (Option 13) wwwagilentcomchemcontactus wwwagilentcomchemcontactus
On-Line resources
ICP-MS Supplies
2nd Edition Speciation Handbook
ICP-MS Journal Archives
Recorded Agilent e-Seminars
ICP-OES Supplies
Atomic Absorption Supplies
Instrument Parts amp Supplies
Atomic Spec Application Notes
Agilent Quick Reference Guide for 77008800 ICP-MS (pub 5990-8182EN)
Agilent Atomic Spec Supplies Catalogue (pub 5990-8767EN)
Agilent Consumables Catalogue (pub 5990-6674EN)
Instrument User Manuals
42
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
Agilentrsquos Atomic Spectroscopy Portfolio - Features
Lowest price
bull Single element
bull DLs typically ~100rsquos ppb
bull Fast (for 1 element)
bull Good elemental coverage
bull Low running cost
Lowest running cost
bull Multi element
bull DLs typically single to 10rsquos ppb
bull Faster
bull Broader elemental coverage
bull Lowest running cost
Trace levels at lowest price
bull Single element
bull DLs typically 10rsquos to 100rsquos ppt
bull Very slow
bull Limited elemental coverage
bull Moderate running cost
Fastest measurement
bull Multi element
bull DLs typically single ppb
bull Very fast
bull Can measure most elements
bull High running cost
Broadest coverage
bull Multi element
bull DLs typically single or sub-ppt
bull Fast
bull Can measure almost all elements
bull Highest running cost
Lowest Selling Price Highest
Flame AA MP-AES Furnace AA ICP-OES ICP-MS
3
ICP-MS Maintenance amp Trouble Shooting
May 2012
Common ICP-MS Problems Reported by Users
Sensitivity
bull Sensitivity is worse than it used to be
bull I have a new application and I canrsquot get the sensitivity I need
bull How come I canrsquot get the instrument to meet published detection limits
Precision
bull Sensitivity is acceptable but precision is terrible
Accuracy
bull Instrument does not give the ldquorightrdquo results
Poor Sample Throughput
bull The instrument throughput needs to improve
bull Nebulizer andor Injector of the Torch blocks too quickly
4
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sensitivity - What Impacts This
4 areas of the instrument can affect sensitivity
ndash Sample introduction system
ndash Method parameters
ndash Cleanliness
ndash Quality of standards used for calibration
Remember ndash SMCQ
Or
ldquoSystem Must Create Qualityrdquo
5
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sensitivity ndash Quality of Standards
ndash What concentration are they
bull Low concentration standards have a finite life
ndash Prepare ppb (ugL) concentration standards daily from high conc stock
ndash Prepare low ppm (mgL) concentration standards weekly
ndash How are they prepared
bull Ensure purchased standards are still within ldquoUse Byrdquo date when used
bull Use calibrated pipettes and class lsquoArsquo volumetric flasks for dilutions
bull Use de-ionized water (Type I - conductivity gt 18 Mcm3) ndash lower grades may have
contamination
bull Please donrsquot do that 1100000 dilution
bull Donrsquot pipette direct from the bottle or return excess standard back to the bottle
ndash How are they stored
bull Plastic vessels ensure better stability
bull Stabilize with acid ndash low pH ensures better stability
6
ICP-MS Maintenance amp Trouble Shooting
May 2012
Detector
③Ion Transmission
Efficiency
②Plasma Ionization
Efficiency
①Nebulizer
Efficiency
7
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sensitivity ndash Itrsquos Determined Byhellip
Low ICP-MS Sensitivity
What to Check
ndash Standards prepared correctly and fresh
ndash Check the pump tubing (see tips on later slide)
and confirm pumping liquid smoothly
ndash Check for nebulizer blockage (use ldquonebulizer testrdquo in SW)
bull If required remove nebulizer and check liquid flowaerosol formation
ndash Check for blockage in the injector of the torch
bull Aspirate a Y solution
bull Check the position of ldquobulletrdquo in the plasma
bull Should be stable
ndash Check the interface cones (see tips on later slide)
ndash Check the ion lens (use ldquoion lens testrdquo in SW)
ndash Check torch positioning and tuning
ndash Check sensitivity in ldquono gas moderdquo ndash if OK suspect reaction gas purity
8
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sensitivity - Peristaltic Pump Tubing
bull Selection of tubing used for an application based on 2 key factors
ndash Resistance to the solvent in use
ndash ID of the tubing required (indicated by the coloured tabs)
bull Usersrsquo usually know what size they need
ndash Sample ndash 102 mm ID or whitewhite tabs
ndash Drain ndash 152 mm ID or yellowblue tabs
bull Smaller sizes used when application demands it
ndash Internal standard ndash 019 mm ID with orangered tabs
or 025 mm ID with orangeblue tabs
9
ICP-MS Maintenance amp Trouble Shooting
May 2012
Trim to 5-10mm to
reduce washout
and contamination
Potential Pump Tube Problems
10
ICP-MS Maintenance amp Trouble Shooting
May 2012
What to Check
ndash Tubing diameters
bull Want tubing used for waste to be larger ID than sample ID
ndash Chemical compatibility
bull Ensure tubing is resistant to the solvent being used
ndash Tube lifetime
bull Typical lifetime is ~1 week based on normal 8 hour working day
ndash Detach from tube holder after use ndash allows tube to ldquorelaxrdquo
bull Check 2 key things on pump tubing
ndash Roundness of tube ndash should not be any ldquoflatrdquo spots
ndash Tubing should still be elastic ndash replace if obviously stretched
bull Using ldquooldrdquo tubing can lead to problems with precision and stability
bull Installation and tensioning critical
ndash Donrsquot overtighten ndash just need smooth and even sample flow
ndash Remember to check other tubing for wear leaks and crimps
Normal wear amp tear
(~5 days) needs
replacing
ICP-MS Sensitivity ndash Method Parameters
What to Check
ndash Isotope selection
bull Using the most sensitive isotope
ndash Pump speed
bull Use the default speed as guide
bull Change pump tubing to give resistance to the solvent
ndash Interferences
bull Check for polyatomic interferences ndash try an alternate isotope first (if required)
ndash Otherwise use ORS3 to remove
bull Physical interferences can affect aerosol formation
ndash Use internal standard matched standards or standard additions
bull Chemical interferences can reduce atom formation and ionization
ndash Use higher RF power optimize neb flow + appropriate matrix modifiers
11
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sensitivity ndash Automated ldquoExpertrdquo Tuning
bull Startup provides a simple
user-configured schedule of
system optimization and
performance checks
bull One-click expert autotuning for
simple plasma optimization
bull Ensures consistent
performance from day to day
bull Independent of operator
experience
bull Automatically generate a
Performance Report
bull Provides a continuing record of
system performance
12
ICP-MS Maintenance amp Trouble Shooting
May 2012
13
Hardware Performance Report
is run under ldquostandardrdquo (factory
check-out) conditions
Gives record of performance
history under consistent default
tuning conditions
Note this is different to the ldquoTune
Reportrdquo which is generated
using Batch tune conditions
Sensitivity ndash Performance Report
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS specific contamination concerns -This is a topic of its own often leads to the clean room
conversation
But remember its not just where your instrument
is located ndash itrsquos everything the sample encounters
on its way to the instrument
ICP-MS Maintenance amp Trouble Shooting
May 2012 14
Sensitivity ndash Cleanliness amp Contamination
Sensitivity ndash Contamination Sources
bull Use high purity or ICP-MS grade reagents
bull Acid purity
ndash Buy only what you need to do the job
ndash Check the certificate of analysis
ndash Donrsquot insert pipette tips into your acids
ndash Use contaminated acid for cleaning
bull Sample containers
ndash Borosilicate glass introduces boron
ndash FEP containers preferred
bull Pipette tips
ndash Colors add interest ndash but increase contamination (Cu Fe Zn Cd)
bull Gloves
ndash Powder free unless you like Zn
Anything that touches sample during prep dilution
transfer analysis and storage
ICP-MS Maintenance amp Trouble Shooting
May 2012 15
PFA spray
chamber
PFA
endcap
PFA
nebulizer
PFA
connector
tube
Quartz torch with sapphire
or platinum injector
Complete sample introduction can be
changed to a system specifically
designed to reduce contamination
bull Usually used for semi-con applications
Clean integrated Auto-Sampler ndash I-AS
Clean sample introduction system - PFA
16
Cleanliness ndash The Ultimate for Contamination Free
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sensitivity ndash System Cleanliness
What to Check
ndash Sample Introduction System
bull Deposits in nebulizer can reduce
sample uptake rate
ndash Soak in aqua regia or use a nebulizer
cleaning tool to back flush
bull Solid material in torch injector
affects aerosol introduction into
plasma and increases noise
bull Contamination in spray chamber
impacts on aerosol formation ndash
increases noise
bull If seeing poor precision may be
due to beading in spray chamber
ndash Soak in 25 detergent solution
overnight (preferably for 24 hours)
17
ICP-MS Maintenance amp Trouble Shooting
May 2012
Nebulizer cleaner
Agilent PN G3266-80020
ICP-MS Sensitivity ndash System Cleanliness
What to Check
ndash Interface cones
bull Deposits or discoloration indicates
cleaning is required
bull Other indicators that cone cleaning
is required
ndash Poor sensitivity
ndash High background
ndash Distorted peak shapes
ndash Changes in interface vacuum reading
(deposition or build-up)
18
ICP-MS Maintenance amp Trouble Shooting
May 2012
Close up
Sample cone after measuring 75 undiluted sea water
samples using HMI Some deposition on outer edges
away from the orifice ndash no blockage of the sampling
orifice ndash but cleaning still recommended
System Cleanliness - Sampling Cone
1 mm Orifice Nickel or Platinum Centres
bull Nickel
bull Physically stronger
bull Tip runs hotter ndash less sample deposition
bull Platinum
bull Chemically stronger
bull Used for higher acid conc (incl HF)
bull 2 centre sizes 10-18 mm
bull Higher cost
Potential Problems
bull Biggest risk is physical damage to the orifice due to excessively aggressive cleaning
bull Cones also affected by sample matrix (acid strength amp type) and number of samples analyzed each day
bull Nickel - Typically replace 3 or 5 each year (assumes measuring 250-350 environmental samples each day)
bull Platinum - Typically replace 1 or 2 each year (assumes measuring 20-50 semiconductor samples each day)
bull If not clean then can result in analytical problems eg poor signal stability elemental contamination
ICP-MS Maintenance amp Trouble Shooting
May 2012 19
System Cleanliness - Skimmer Cone
04 mm Orifice Nickel or Platinum
bull The Nickel skimmer cone is the standard interface
bull The skimmer cone is relatively robust to samples containing high concentrations of matrix and salts and is suitable for a wide variety of samples It is usually used with the Nickel sampling cone
bull The Platinum skimmer cone is usually used for introduction of hydrofluoric acid and other reagents It is usually used with the Platinum sampling cone
Potential Problems
bull Biggest risk is from physical damage to the orifice due to excessively aggressive cleaning
bull Cones also affected by sample matrix (acid strength amp type) and number of samples analyzed each day
bull Nickel ndash Typically replace 3 or 5 each year (assumes measuring 250-350 environmental samples each day)
bull Platinum ndash Typically replace 1 or 2 each year (assumes measuring 20-50 semiconductor samples each day)
bull If not clean then can result in analytical problems eg poor signal stability elemental contamination
20
ICP-MS Maintenance amp Trouble Shooting
May 2012
System Cleanliness - Cone Cleaning Procedure
Caution - Take care to avoid damage to the cone tip when removing ndash and place base down - Check the graphite gasket and replace if creased or damaged - Sonicate in a 2 Citranox or 2 Nitric Acid solution for a few minutes - Rinse well with de-ionized water - If still dirty or memory problems remain polish using an alumina powder slurry on a Q-tip then sonicate in 2 Citranox solution and rinse well with de-ionized water - Dry with nitrogen before installing
22
ICP-MS Maintenance amp Trouble Shooting
May 2012
Precision - Why is This Important
What does ldquoPrecisionrdquo mean
ndash Ability to get the same result for the same
sample when measured multiple times
ndash Usually measured as RSD or sometimes SD
RSD = (SD Mean Result) 100
ndash Low values indicate good precision
bull For ICP-MS expect 1-2 RSD
Why is this important
ndash User loses confidence in the system
What impacts on precision
ndash Nebulizerplasma stability
ndash Sample introduction system
ndash Method parameters
23
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash System stabilized
bull Allow 10 mins for plasma warm-up before
analysis
ndash Plasma status
bull ldquoBulletrdquo in the plasma should be stable
bull Check for deposits in the injector of the torch
ndash Check condition of interface cones and
clean if necessary
ndash Clean the Extraction Lens - Omega Lens
assembly
ndash Method parameters
bull Appropriate times set for sample uptake
delay and stabilization times
24
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash Sample Intro
What to Check ndash Nebulizer
bull Nebulizer type used can impact on sensitivity and precision
ndash MicroMist (glass concentric type) is the standard nebulizer ndash handles most sample
types
ndash PFA MicroFlow nebulizer best for low volume samples aggressive samples (HF
digests) and when low contamination required (semi-con)
ndash Babington gives poorer precision - best for high TDS samples
bull Check nebulizer condition regularly
ndash Chips in the nebulizer tip impact on aerosol formation ndash poor precision
(use a magnifying glass if necessary)
ndash Check for deposits or blockage in the tip
bull Sample uptake or flow rate
ndash Lower pump speed or using narrow bore pump tubing will reduce uptake rate
- better for high TDS samples
25
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Sample Introduction bull Contamination in the spray chamber
ndash When was the spray chamber cleaned
bull Any blockages in the nebulizer injector
ndash Check for stable aerosol formation
bull Air leaks in spray chamber end cap or connecting tubes
ndash Are they in good condition with tight connections
bull Damaged pump tubes
ndash When did you check the pump tubes
bull Is the pump speed too slow
ndash Low pump speeds may cause signal pulsation
ndash If required use narrower bore pump tube and increase pump speed
bull Samples have a high TDS content
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
26
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Memory effects
bull If possible avoid running high concentrations of these analytes
(Ag Au B Hg Mo Si Sn W Zn Zr)
ndash Maybe necessary to pre-dilute samples (if known to be high in concentration)
bull Ensure an adequate rinse time
ndash Should be at least equal to the sample uptake delay
(30-40 seconds typical)
bull May require an acidified rinse solution between samples
(2 HNO3)
bull Other strategies to minimize memory effects
ndash Use an inert spray chamber
ndash Use the ISIS to introduce discrete amounts of sample This means
bull Cones are exposed to less sample matrix = improved stability
bull Less memorycarry-over
bull Reduced uptake amp rinse times = faster measurement
27
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy - Why is This Important
What does ldquoAccuracyrdquo mean
ndash Ability to get the ldquorightrdquo answer for the sample
ndash Heavily dependent on operatorrsquos skill
Why is this important
ndash User loses confidence in the system
ndash Your reputationhellip
bull Customerrsquos question the results
bull Poor performance in ldquoround robinrdquo comparisons
How do You Confirm Accuracy
ndash Check the result for a prepared standard
ndash Measure a certified reference material
ndash Use other quality control checks to check analysis
28
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Calibration standards properly prepared
bull See earlier recommendations ndash important to match to samples prepare
accurately and use them ldquofreshrdquo
ndash Any interferences impacting on results
ndash Use matched standards or standard additions
ndash Ensure isotope selected has no polyatomic interferences
ndash If necessary use ORS3
ndash Precision optimized
bull Optimum signal to noise performance improves accuracy
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
29
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Reprocess data post
run using an
alternate internal
standard
bull Ensure Internal
Standard used is
similar in mass
bull Check whether the
Internal Standard is
present in the
sample
ndash If necessary do a Semi-
Quant measurement
bull Dilute with cal blk
matrix
30
Accuracy ndash Suspect Internal Standard Recovery
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Sample preparation
bull Is the most appropriate digestion being used
bull Are all of the analytes being quantitatively (and reproducibly) extracted and
dissolved
ndash Many digestions are only partial extracts ndash efficiency will vary with the
sample matrix
ndash Some volatile analytes may be ldquolostrdquo during digestion
bull Confirm by taking a solid certified reference material
through your preparation and analysis procedure
bull Is the digest stable ndash or are you seeing any precipitates or a suspension
bull Do you see any potential contamination from either reagents or the digestion
equipment eg especially with Si B or Ca
bull Include a ldquoReagent Blankrdquo with every sample batch to
monitor
31
ICP-MS Maintenance amp Trouble Shooting
May 2012
Laboratory environment can have
direct impact on quality of results
bull Clean uncluttered work area
bull Proper ventilation
bull Safety considerations
bull Instrument lifetime consideration
ICP-MS Maintenance amp Trouble Shooting
May 2012 32
Laboratory Environment
ICP-MS ndash Potential Autosampler Issues
ndash More customers use autosamplers with ICP for automation
ndash Issues to consider
bull Long transfer tube between sampler and ICP-MS
ndash May need to program a longer sample uptake delay
ndash May exacerbate problems with memory effects
ndash Use ldquoFast Pumprdquo during sample uptake delay
bull Caution ndash not always possible
Not recommended with high TDS samples and organics
bull Ensure probe diameter is appropriate for sample matrix
ndash Use wider bore for high TDS or viscous samples
bull Sample stability - potential for sample changes while uncovered in racks ndash impacts accuracy
ndash Dust ingress can introduce contamination
ndash Sample evaporation may occur during long unattended runs
ndash Sediment in the sample may settle out esp with wear metals or suspensions
bull Ensure transfer line to ICP-MS is in good condition
ndash Kinks in the line may cause poor uptake or pulsing in the sample
ndash Impacts on precision and accuracy
33
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sample Throughput ndash What to Check
ndash Samples fully digested
bull No excess particulates in the sample that may cause blockage
ndash Sample Introduction System optimized
ndash Capable of handling the TDS levels in the sample
ndash TorchNebulizer cleaned and ready for analysis
ndash Method parameters optimized
bull Sample uptake delay and stabilization times are appropriate ndash optimized
bull Integration time is appropriate for the expected concentration
ndash Use a longer integration time at low concentrations
bull Rinse time is appropriate
bull Use ldquoISISrdquo discrete sampling for faster measurement and faster washout
34
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Handles tough sample matrices better
than any other ICP-MS
ndash Highest plasma temperature (lowest
CeOCe) as standard
ndash HMI (high matrix introduction) allows direct
analysis of difficult samples
eg sea water
bull ORS3 operates in He collision mode to
remove ALL polyatomic interferences
ndash Enables reliable removal of all polyatomic
interferences using a single set of
conditions
ndash Gives lower levels of interference and
better long-term stability HMI gives lower suppression and
better long-term stability
Relative signal (suppression) in undiluted seawater
Long-term stability in undiluted seawater
35
Agilent ICP-MS Performance - Benefits
Best matrix tolerance amp less interferences
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS ndash Recommended Maintenance Schedule
ICP-MS Maintenance amp Trouble Shooting
May 2012 37
These functions
(and more) are
completed as part
of a Preventative
Maintenance
program by an
Agilent Field
Service Engineer
Summary ndash Key Consumables for ICP-MS
Sample preparationpresentation
ndash Peristaltic pump tubing
ndash Transfer and drain tubing
ndash ICP-MS standard solutions
ndash Internal Standard solutions
ndash Torches
ndash Spray chambers
ndash Nebulizers
Ion Extraction
ndash Sampler and skimmer cones
Autosampling
ndash Sample tubes racks probes and transfer tubing
ISIS
ndash Peristaltic pump tubing ferrules amp fittings
38
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sample Introduction
Key consumables requiring frequent replacement
bull Pump tubing
bull Torches and quartz transfer tube
bull Nebulizers
bull Spray chambers
bull Interface cones (skimmer amp sampler)
bull Transfer amp connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalogue
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24406(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 39
Autosampler Supplies
Key consumables requiring frequent replacement
ndash Peristaltic pump tubing
ndash Sample racks
ndash Sample tubes
ndash Spare probes
ndash Standard racks
ndash Connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24407(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 40
ISIS Supplies
Key consumables requiring frequent replacement
bull Peristaltic pump tubing
bull Ferrules and fittings
bull Valving
For ISIS Hydride Generation Accessory
bull Membrane filter
bull Concentric nebulizer
bull Gas-liquid separator
bull Other tubing and connectors
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceProductListingaspxcat=SubCat2ECS_24437(Agilent)amppcat=SubCat1ECS_24407(Agilent)amprcat=ClassECS_22674(Agilent)
41
ICP-MS Maintenance amp Trouble Shooting
May 2012
Where to Find the Right Consumable Analytical Consumables Agilent Assist
Consumables amp Supplies Instrument Sales ampServices 1-800-227-9770 (Option 11) 1-800-227-9770 (Option 13) wwwagilentcomchemcontactus wwwagilentcomchemcontactus
On-Line resources
ICP-MS Supplies
2nd Edition Speciation Handbook
ICP-MS Journal Archives
Recorded Agilent e-Seminars
ICP-OES Supplies
Atomic Absorption Supplies
Instrument Parts amp Supplies
Atomic Spec Application Notes
Agilent Quick Reference Guide for 77008800 ICP-MS (pub 5990-8182EN)
Agilent Atomic Spec Supplies Catalogue (pub 5990-8767EN)
Agilent Consumables Catalogue (pub 5990-6674EN)
Instrument User Manuals
42
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
Common ICP-MS Problems Reported by Users
Sensitivity
bull Sensitivity is worse than it used to be
bull I have a new application and I canrsquot get the sensitivity I need
bull How come I canrsquot get the instrument to meet published detection limits
Precision
bull Sensitivity is acceptable but precision is terrible
Accuracy
bull Instrument does not give the ldquorightrdquo results
Poor Sample Throughput
bull The instrument throughput needs to improve
bull Nebulizer andor Injector of the Torch blocks too quickly
4
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sensitivity - What Impacts This
4 areas of the instrument can affect sensitivity
ndash Sample introduction system
ndash Method parameters
ndash Cleanliness
ndash Quality of standards used for calibration
Remember ndash SMCQ
Or
ldquoSystem Must Create Qualityrdquo
5
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sensitivity ndash Quality of Standards
ndash What concentration are they
bull Low concentration standards have a finite life
ndash Prepare ppb (ugL) concentration standards daily from high conc stock
ndash Prepare low ppm (mgL) concentration standards weekly
ndash How are they prepared
bull Ensure purchased standards are still within ldquoUse Byrdquo date when used
bull Use calibrated pipettes and class lsquoArsquo volumetric flasks for dilutions
bull Use de-ionized water (Type I - conductivity gt 18 Mcm3) ndash lower grades may have
contamination
bull Please donrsquot do that 1100000 dilution
bull Donrsquot pipette direct from the bottle or return excess standard back to the bottle
ndash How are they stored
bull Plastic vessels ensure better stability
bull Stabilize with acid ndash low pH ensures better stability
6
ICP-MS Maintenance amp Trouble Shooting
May 2012
Detector
③Ion Transmission
Efficiency
②Plasma Ionization
Efficiency
①Nebulizer
Efficiency
7
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sensitivity ndash Itrsquos Determined Byhellip
Low ICP-MS Sensitivity
What to Check
ndash Standards prepared correctly and fresh
ndash Check the pump tubing (see tips on later slide)
and confirm pumping liquid smoothly
ndash Check for nebulizer blockage (use ldquonebulizer testrdquo in SW)
bull If required remove nebulizer and check liquid flowaerosol formation
ndash Check for blockage in the injector of the torch
bull Aspirate a Y solution
bull Check the position of ldquobulletrdquo in the plasma
bull Should be stable
ndash Check the interface cones (see tips on later slide)
ndash Check the ion lens (use ldquoion lens testrdquo in SW)
ndash Check torch positioning and tuning
ndash Check sensitivity in ldquono gas moderdquo ndash if OK suspect reaction gas purity
8
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sensitivity - Peristaltic Pump Tubing
bull Selection of tubing used for an application based on 2 key factors
ndash Resistance to the solvent in use
ndash ID of the tubing required (indicated by the coloured tabs)
bull Usersrsquo usually know what size they need
ndash Sample ndash 102 mm ID or whitewhite tabs
ndash Drain ndash 152 mm ID or yellowblue tabs
bull Smaller sizes used when application demands it
ndash Internal standard ndash 019 mm ID with orangered tabs
or 025 mm ID with orangeblue tabs
9
ICP-MS Maintenance amp Trouble Shooting
May 2012
Trim to 5-10mm to
reduce washout
and contamination
Potential Pump Tube Problems
10
ICP-MS Maintenance amp Trouble Shooting
May 2012
What to Check
ndash Tubing diameters
bull Want tubing used for waste to be larger ID than sample ID
ndash Chemical compatibility
bull Ensure tubing is resistant to the solvent being used
ndash Tube lifetime
bull Typical lifetime is ~1 week based on normal 8 hour working day
ndash Detach from tube holder after use ndash allows tube to ldquorelaxrdquo
bull Check 2 key things on pump tubing
ndash Roundness of tube ndash should not be any ldquoflatrdquo spots
ndash Tubing should still be elastic ndash replace if obviously stretched
bull Using ldquooldrdquo tubing can lead to problems with precision and stability
bull Installation and tensioning critical
ndash Donrsquot overtighten ndash just need smooth and even sample flow
ndash Remember to check other tubing for wear leaks and crimps
Normal wear amp tear
(~5 days) needs
replacing
ICP-MS Sensitivity ndash Method Parameters
What to Check
ndash Isotope selection
bull Using the most sensitive isotope
ndash Pump speed
bull Use the default speed as guide
bull Change pump tubing to give resistance to the solvent
ndash Interferences
bull Check for polyatomic interferences ndash try an alternate isotope first (if required)
ndash Otherwise use ORS3 to remove
bull Physical interferences can affect aerosol formation
ndash Use internal standard matched standards or standard additions
bull Chemical interferences can reduce atom formation and ionization
ndash Use higher RF power optimize neb flow + appropriate matrix modifiers
11
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sensitivity ndash Automated ldquoExpertrdquo Tuning
bull Startup provides a simple
user-configured schedule of
system optimization and
performance checks
bull One-click expert autotuning for
simple plasma optimization
bull Ensures consistent
performance from day to day
bull Independent of operator
experience
bull Automatically generate a
Performance Report
bull Provides a continuing record of
system performance
12
ICP-MS Maintenance amp Trouble Shooting
May 2012
13
Hardware Performance Report
is run under ldquostandardrdquo (factory
check-out) conditions
Gives record of performance
history under consistent default
tuning conditions
Note this is different to the ldquoTune
Reportrdquo which is generated
using Batch tune conditions
Sensitivity ndash Performance Report
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS specific contamination concerns -This is a topic of its own often leads to the clean room
conversation
But remember its not just where your instrument
is located ndash itrsquos everything the sample encounters
on its way to the instrument
ICP-MS Maintenance amp Trouble Shooting
May 2012 14
Sensitivity ndash Cleanliness amp Contamination
Sensitivity ndash Contamination Sources
bull Use high purity or ICP-MS grade reagents
bull Acid purity
ndash Buy only what you need to do the job
ndash Check the certificate of analysis
ndash Donrsquot insert pipette tips into your acids
ndash Use contaminated acid for cleaning
bull Sample containers
ndash Borosilicate glass introduces boron
ndash FEP containers preferred
bull Pipette tips
ndash Colors add interest ndash but increase contamination (Cu Fe Zn Cd)
bull Gloves
ndash Powder free unless you like Zn
Anything that touches sample during prep dilution
transfer analysis and storage
ICP-MS Maintenance amp Trouble Shooting
May 2012 15
PFA spray
chamber
PFA
endcap
PFA
nebulizer
PFA
connector
tube
Quartz torch with sapphire
or platinum injector
Complete sample introduction can be
changed to a system specifically
designed to reduce contamination
bull Usually used for semi-con applications
Clean integrated Auto-Sampler ndash I-AS
Clean sample introduction system - PFA
16
Cleanliness ndash The Ultimate for Contamination Free
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sensitivity ndash System Cleanliness
What to Check
ndash Sample Introduction System
bull Deposits in nebulizer can reduce
sample uptake rate
ndash Soak in aqua regia or use a nebulizer
cleaning tool to back flush
bull Solid material in torch injector
affects aerosol introduction into
plasma and increases noise
bull Contamination in spray chamber
impacts on aerosol formation ndash
increases noise
bull If seeing poor precision may be
due to beading in spray chamber
ndash Soak in 25 detergent solution
overnight (preferably for 24 hours)
17
ICP-MS Maintenance amp Trouble Shooting
May 2012
Nebulizer cleaner
Agilent PN G3266-80020
ICP-MS Sensitivity ndash System Cleanliness
What to Check
ndash Interface cones
bull Deposits or discoloration indicates
cleaning is required
bull Other indicators that cone cleaning
is required
ndash Poor sensitivity
ndash High background
ndash Distorted peak shapes
ndash Changes in interface vacuum reading
(deposition or build-up)
18
ICP-MS Maintenance amp Trouble Shooting
May 2012
Close up
Sample cone after measuring 75 undiluted sea water
samples using HMI Some deposition on outer edges
away from the orifice ndash no blockage of the sampling
orifice ndash but cleaning still recommended
System Cleanliness - Sampling Cone
1 mm Orifice Nickel or Platinum Centres
bull Nickel
bull Physically stronger
bull Tip runs hotter ndash less sample deposition
bull Platinum
bull Chemically stronger
bull Used for higher acid conc (incl HF)
bull 2 centre sizes 10-18 mm
bull Higher cost
Potential Problems
bull Biggest risk is physical damage to the orifice due to excessively aggressive cleaning
bull Cones also affected by sample matrix (acid strength amp type) and number of samples analyzed each day
bull Nickel - Typically replace 3 or 5 each year (assumes measuring 250-350 environmental samples each day)
bull Platinum - Typically replace 1 or 2 each year (assumes measuring 20-50 semiconductor samples each day)
bull If not clean then can result in analytical problems eg poor signal stability elemental contamination
ICP-MS Maintenance amp Trouble Shooting
May 2012 19
System Cleanliness - Skimmer Cone
04 mm Orifice Nickel or Platinum
bull The Nickel skimmer cone is the standard interface
bull The skimmer cone is relatively robust to samples containing high concentrations of matrix and salts and is suitable for a wide variety of samples It is usually used with the Nickel sampling cone
bull The Platinum skimmer cone is usually used for introduction of hydrofluoric acid and other reagents It is usually used with the Platinum sampling cone
Potential Problems
bull Biggest risk is from physical damage to the orifice due to excessively aggressive cleaning
bull Cones also affected by sample matrix (acid strength amp type) and number of samples analyzed each day
bull Nickel ndash Typically replace 3 or 5 each year (assumes measuring 250-350 environmental samples each day)
bull Platinum ndash Typically replace 1 or 2 each year (assumes measuring 20-50 semiconductor samples each day)
bull If not clean then can result in analytical problems eg poor signal stability elemental contamination
20
ICP-MS Maintenance amp Trouble Shooting
May 2012
System Cleanliness - Cone Cleaning Procedure
Caution - Take care to avoid damage to the cone tip when removing ndash and place base down - Check the graphite gasket and replace if creased or damaged - Sonicate in a 2 Citranox or 2 Nitric Acid solution for a few minutes - Rinse well with de-ionized water - If still dirty or memory problems remain polish using an alumina powder slurry on a Q-tip then sonicate in 2 Citranox solution and rinse well with de-ionized water - Dry with nitrogen before installing
22
ICP-MS Maintenance amp Trouble Shooting
May 2012
Precision - Why is This Important
What does ldquoPrecisionrdquo mean
ndash Ability to get the same result for the same
sample when measured multiple times
ndash Usually measured as RSD or sometimes SD
RSD = (SD Mean Result) 100
ndash Low values indicate good precision
bull For ICP-MS expect 1-2 RSD
Why is this important
ndash User loses confidence in the system
What impacts on precision
ndash Nebulizerplasma stability
ndash Sample introduction system
ndash Method parameters
23
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash System stabilized
bull Allow 10 mins for plasma warm-up before
analysis
ndash Plasma status
bull ldquoBulletrdquo in the plasma should be stable
bull Check for deposits in the injector of the torch
ndash Check condition of interface cones and
clean if necessary
ndash Clean the Extraction Lens - Omega Lens
assembly
ndash Method parameters
bull Appropriate times set for sample uptake
delay and stabilization times
24
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash Sample Intro
What to Check ndash Nebulizer
bull Nebulizer type used can impact on sensitivity and precision
ndash MicroMist (glass concentric type) is the standard nebulizer ndash handles most sample
types
ndash PFA MicroFlow nebulizer best for low volume samples aggressive samples (HF
digests) and when low contamination required (semi-con)
ndash Babington gives poorer precision - best for high TDS samples
bull Check nebulizer condition regularly
ndash Chips in the nebulizer tip impact on aerosol formation ndash poor precision
(use a magnifying glass if necessary)
ndash Check for deposits or blockage in the tip
bull Sample uptake or flow rate
ndash Lower pump speed or using narrow bore pump tubing will reduce uptake rate
- better for high TDS samples
25
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Sample Introduction bull Contamination in the spray chamber
ndash When was the spray chamber cleaned
bull Any blockages in the nebulizer injector
ndash Check for stable aerosol formation
bull Air leaks in spray chamber end cap or connecting tubes
ndash Are they in good condition with tight connections
bull Damaged pump tubes
ndash When did you check the pump tubes
bull Is the pump speed too slow
ndash Low pump speeds may cause signal pulsation
ndash If required use narrower bore pump tube and increase pump speed
bull Samples have a high TDS content
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
26
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Memory effects
bull If possible avoid running high concentrations of these analytes
(Ag Au B Hg Mo Si Sn W Zn Zr)
ndash Maybe necessary to pre-dilute samples (if known to be high in concentration)
bull Ensure an adequate rinse time
ndash Should be at least equal to the sample uptake delay
(30-40 seconds typical)
bull May require an acidified rinse solution between samples
(2 HNO3)
bull Other strategies to minimize memory effects
ndash Use an inert spray chamber
ndash Use the ISIS to introduce discrete amounts of sample This means
bull Cones are exposed to less sample matrix = improved stability
bull Less memorycarry-over
bull Reduced uptake amp rinse times = faster measurement
27
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy - Why is This Important
What does ldquoAccuracyrdquo mean
ndash Ability to get the ldquorightrdquo answer for the sample
ndash Heavily dependent on operatorrsquos skill
Why is this important
ndash User loses confidence in the system
ndash Your reputationhellip
bull Customerrsquos question the results
bull Poor performance in ldquoround robinrdquo comparisons
How do You Confirm Accuracy
ndash Check the result for a prepared standard
ndash Measure a certified reference material
ndash Use other quality control checks to check analysis
28
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Calibration standards properly prepared
bull See earlier recommendations ndash important to match to samples prepare
accurately and use them ldquofreshrdquo
ndash Any interferences impacting on results
ndash Use matched standards or standard additions
ndash Ensure isotope selected has no polyatomic interferences
ndash If necessary use ORS3
ndash Precision optimized
bull Optimum signal to noise performance improves accuracy
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
29
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Reprocess data post
run using an
alternate internal
standard
bull Ensure Internal
Standard used is
similar in mass
bull Check whether the
Internal Standard is
present in the
sample
ndash If necessary do a Semi-
Quant measurement
bull Dilute with cal blk
matrix
30
Accuracy ndash Suspect Internal Standard Recovery
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Sample preparation
bull Is the most appropriate digestion being used
bull Are all of the analytes being quantitatively (and reproducibly) extracted and
dissolved
ndash Many digestions are only partial extracts ndash efficiency will vary with the
sample matrix
ndash Some volatile analytes may be ldquolostrdquo during digestion
bull Confirm by taking a solid certified reference material
through your preparation and analysis procedure
bull Is the digest stable ndash or are you seeing any precipitates or a suspension
bull Do you see any potential contamination from either reagents or the digestion
equipment eg especially with Si B or Ca
bull Include a ldquoReagent Blankrdquo with every sample batch to
monitor
31
ICP-MS Maintenance amp Trouble Shooting
May 2012
Laboratory environment can have
direct impact on quality of results
bull Clean uncluttered work area
bull Proper ventilation
bull Safety considerations
bull Instrument lifetime consideration
ICP-MS Maintenance amp Trouble Shooting
May 2012 32
Laboratory Environment
ICP-MS ndash Potential Autosampler Issues
ndash More customers use autosamplers with ICP for automation
ndash Issues to consider
bull Long transfer tube between sampler and ICP-MS
ndash May need to program a longer sample uptake delay
ndash May exacerbate problems with memory effects
ndash Use ldquoFast Pumprdquo during sample uptake delay
bull Caution ndash not always possible
Not recommended with high TDS samples and organics
bull Ensure probe diameter is appropriate for sample matrix
ndash Use wider bore for high TDS or viscous samples
bull Sample stability - potential for sample changes while uncovered in racks ndash impacts accuracy
ndash Dust ingress can introduce contamination
ndash Sample evaporation may occur during long unattended runs
ndash Sediment in the sample may settle out esp with wear metals or suspensions
bull Ensure transfer line to ICP-MS is in good condition
ndash Kinks in the line may cause poor uptake or pulsing in the sample
ndash Impacts on precision and accuracy
33
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sample Throughput ndash What to Check
ndash Samples fully digested
bull No excess particulates in the sample that may cause blockage
ndash Sample Introduction System optimized
ndash Capable of handling the TDS levels in the sample
ndash TorchNebulizer cleaned and ready for analysis
ndash Method parameters optimized
bull Sample uptake delay and stabilization times are appropriate ndash optimized
bull Integration time is appropriate for the expected concentration
ndash Use a longer integration time at low concentrations
bull Rinse time is appropriate
bull Use ldquoISISrdquo discrete sampling for faster measurement and faster washout
34
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Handles tough sample matrices better
than any other ICP-MS
ndash Highest plasma temperature (lowest
CeOCe) as standard
ndash HMI (high matrix introduction) allows direct
analysis of difficult samples
eg sea water
bull ORS3 operates in He collision mode to
remove ALL polyatomic interferences
ndash Enables reliable removal of all polyatomic
interferences using a single set of
conditions
ndash Gives lower levels of interference and
better long-term stability HMI gives lower suppression and
better long-term stability
Relative signal (suppression) in undiluted seawater
Long-term stability in undiluted seawater
35
Agilent ICP-MS Performance - Benefits
Best matrix tolerance amp less interferences
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS ndash Recommended Maintenance Schedule
ICP-MS Maintenance amp Trouble Shooting
May 2012 37
These functions
(and more) are
completed as part
of a Preventative
Maintenance
program by an
Agilent Field
Service Engineer
Summary ndash Key Consumables for ICP-MS
Sample preparationpresentation
ndash Peristaltic pump tubing
ndash Transfer and drain tubing
ndash ICP-MS standard solutions
ndash Internal Standard solutions
ndash Torches
ndash Spray chambers
ndash Nebulizers
Ion Extraction
ndash Sampler and skimmer cones
Autosampling
ndash Sample tubes racks probes and transfer tubing
ISIS
ndash Peristaltic pump tubing ferrules amp fittings
38
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sample Introduction
Key consumables requiring frequent replacement
bull Pump tubing
bull Torches and quartz transfer tube
bull Nebulizers
bull Spray chambers
bull Interface cones (skimmer amp sampler)
bull Transfer amp connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalogue
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24406(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 39
Autosampler Supplies
Key consumables requiring frequent replacement
ndash Peristaltic pump tubing
ndash Sample racks
ndash Sample tubes
ndash Spare probes
ndash Standard racks
ndash Connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24407(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 40
ISIS Supplies
Key consumables requiring frequent replacement
bull Peristaltic pump tubing
bull Ferrules and fittings
bull Valving
For ISIS Hydride Generation Accessory
bull Membrane filter
bull Concentric nebulizer
bull Gas-liquid separator
bull Other tubing and connectors
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceProductListingaspxcat=SubCat2ECS_24437(Agilent)amppcat=SubCat1ECS_24407(Agilent)amprcat=ClassECS_22674(Agilent)
41
ICP-MS Maintenance amp Trouble Shooting
May 2012
Where to Find the Right Consumable Analytical Consumables Agilent Assist
Consumables amp Supplies Instrument Sales ampServices 1-800-227-9770 (Option 11) 1-800-227-9770 (Option 13) wwwagilentcomchemcontactus wwwagilentcomchemcontactus
On-Line resources
ICP-MS Supplies
2nd Edition Speciation Handbook
ICP-MS Journal Archives
Recorded Agilent e-Seminars
ICP-OES Supplies
Atomic Absorption Supplies
Instrument Parts amp Supplies
Atomic Spec Application Notes
Agilent Quick Reference Guide for 77008800 ICP-MS (pub 5990-8182EN)
Agilent Atomic Spec Supplies Catalogue (pub 5990-8767EN)
Agilent Consumables Catalogue (pub 5990-6674EN)
Instrument User Manuals
42
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sensitivity - What Impacts This
4 areas of the instrument can affect sensitivity
ndash Sample introduction system
ndash Method parameters
ndash Cleanliness
ndash Quality of standards used for calibration
Remember ndash SMCQ
Or
ldquoSystem Must Create Qualityrdquo
5
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sensitivity ndash Quality of Standards
ndash What concentration are they
bull Low concentration standards have a finite life
ndash Prepare ppb (ugL) concentration standards daily from high conc stock
ndash Prepare low ppm (mgL) concentration standards weekly
ndash How are they prepared
bull Ensure purchased standards are still within ldquoUse Byrdquo date when used
bull Use calibrated pipettes and class lsquoArsquo volumetric flasks for dilutions
bull Use de-ionized water (Type I - conductivity gt 18 Mcm3) ndash lower grades may have
contamination
bull Please donrsquot do that 1100000 dilution
bull Donrsquot pipette direct from the bottle or return excess standard back to the bottle
ndash How are they stored
bull Plastic vessels ensure better stability
bull Stabilize with acid ndash low pH ensures better stability
6
ICP-MS Maintenance amp Trouble Shooting
May 2012
Detector
③Ion Transmission
Efficiency
②Plasma Ionization
Efficiency
①Nebulizer
Efficiency
7
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sensitivity ndash Itrsquos Determined Byhellip
Low ICP-MS Sensitivity
What to Check
ndash Standards prepared correctly and fresh
ndash Check the pump tubing (see tips on later slide)
and confirm pumping liquid smoothly
ndash Check for nebulizer blockage (use ldquonebulizer testrdquo in SW)
bull If required remove nebulizer and check liquid flowaerosol formation
ndash Check for blockage in the injector of the torch
bull Aspirate a Y solution
bull Check the position of ldquobulletrdquo in the plasma
bull Should be stable
ndash Check the interface cones (see tips on later slide)
ndash Check the ion lens (use ldquoion lens testrdquo in SW)
ndash Check torch positioning and tuning
ndash Check sensitivity in ldquono gas moderdquo ndash if OK suspect reaction gas purity
8
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sensitivity - Peristaltic Pump Tubing
bull Selection of tubing used for an application based on 2 key factors
ndash Resistance to the solvent in use
ndash ID of the tubing required (indicated by the coloured tabs)
bull Usersrsquo usually know what size they need
ndash Sample ndash 102 mm ID or whitewhite tabs
ndash Drain ndash 152 mm ID or yellowblue tabs
bull Smaller sizes used when application demands it
ndash Internal standard ndash 019 mm ID with orangered tabs
or 025 mm ID with orangeblue tabs
9
ICP-MS Maintenance amp Trouble Shooting
May 2012
Trim to 5-10mm to
reduce washout
and contamination
Potential Pump Tube Problems
10
ICP-MS Maintenance amp Trouble Shooting
May 2012
What to Check
ndash Tubing diameters
bull Want tubing used for waste to be larger ID than sample ID
ndash Chemical compatibility
bull Ensure tubing is resistant to the solvent being used
ndash Tube lifetime
bull Typical lifetime is ~1 week based on normal 8 hour working day
ndash Detach from tube holder after use ndash allows tube to ldquorelaxrdquo
bull Check 2 key things on pump tubing
ndash Roundness of tube ndash should not be any ldquoflatrdquo spots
ndash Tubing should still be elastic ndash replace if obviously stretched
bull Using ldquooldrdquo tubing can lead to problems with precision and stability
bull Installation and tensioning critical
ndash Donrsquot overtighten ndash just need smooth and even sample flow
ndash Remember to check other tubing for wear leaks and crimps
Normal wear amp tear
(~5 days) needs
replacing
ICP-MS Sensitivity ndash Method Parameters
What to Check
ndash Isotope selection
bull Using the most sensitive isotope
ndash Pump speed
bull Use the default speed as guide
bull Change pump tubing to give resistance to the solvent
ndash Interferences
bull Check for polyatomic interferences ndash try an alternate isotope first (if required)
ndash Otherwise use ORS3 to remove
bull Physical interferences can affect aerosol formation
ndash Use internal standard matched standards or standard additions
bull Chemical interferences can reduce atom formation and ionization
ndash Use higher RF power optimize neb flow + appropriate matrix modifiers
11
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sensitivity ndash Automated ldquoExpertrdquo Tuning
bull Startup provides a simple
user-configured schedule of
system optimization and
performance checks
bull One-click expert autotuning for
simple plasma optimization
bull Ensures consistent
performance from day to day
bull Independent of operator
experience
bull Automatically generate a
Performance Report
bull Provides a continuing record of
system performance
12
ICP-MS Maintenance amp Trouble Shooting
May 2012
13
Hardware Performance Report
is run under ldquostandardrdquo (factory
check-out) conditions
Gives record of performance
history under consistent default
tuning conditions
Note this is different to the ldquoTune
Reportrdquo which is generated
using Batch tune conditions
Sensitivity ndash Performance Report
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS specific contamination concerns -This is a topic of its own often leads to the clean room
conversation
But remember its not just where your instrument
is located ndash itrsquos everything the sample encounters
on its way to the instrument
ICP-MS Maintenance amp Trouble Shooting
May 2012 14
Sensitivity ndash Cleanliness amp Contamination
Sensitivity ndash Contamination Sources
bull Use high purity or ICP-MS grade reagents
bull Acid purity
ndash Buy only what you need to do the job
ndash Check the certificate of analysis
ndash Donrsquot insert pipette tips into your acids
ndash Use contaminated acid for cleaning
bull Sample containers
ndash Borosilicate glass introduces boron
ndash FEP containers preferred
bull Pipette tips
ndash Colors add interest ndash but increase contamination (Cu Fe Zn Cd)
bull Gloves
ndash Powder free unless you like Zn
Anything that touches sample during prep dilution
transfer analysis and storage
ICP-MS Maintenance amp Trouble Shooting
May 2012 15
PFA spray
chamber
PFA
endcap
PFA
nebulizer
PFA
connector
tube
Quartz torch with sapphire
or platinum injector
Complete sample introduction can be
changed to a system specifically
designed to reduce contamination
bull Usually used for semi-con applications
Clean integrated Auto-Sampler ndash I-AS
Clean sample introduction system - PFA
16
Cleanliness ndash The Ultimate for Contamination Free
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sensitivity ndash System Cleanliness
What to Check
ndash Sample Introduction System
bull Deposits in nebulizer can reduce
sample uptake rate
ndash Soak in aqua regia or use a nebulizer
cleaning tool to back flush
bull Solid material in torch injector
affects aerosol introduction into
plasma and increases noise
bull Contamination in spray chamber
impacts on aerosol formation ndash
increases noise
bull If seeing poor precision may be
due to beading in spray chamber
ndash Soak in 25 detergent solution
overnight (preferably for 24 hours)
17
ICP-MS Maintenance amp Trouble Shooting
May 2012
Nebulizer cleaner
Agilent PN G3266-80020
ICP-MS Sensitivity ndash System Cleanliness
What to Check
ndash Interface cones
bull Deposits or discoloration indicates
cleaning is required
bull Other indicators that cone cleaning
is required
ndash Poor sensitivity
ndash High background
ndash Distorted peak shapes
ndash Changes in interface vacuum reading
(deposition or build-up)
18
ICP-MS Maintenance amp Trouble Shooting
May 2012
Close up
Sample cone after measuring 75 undiluted sea water
samples using HMI Some deposition on outer edges
away from the orifice ndash no blockage of the sampling
orifice ndash but cleaning still recommended
System Cleanliness - Sampling Cone
1 mm Orifice Nickel or Platinum Centres
bull Nickel
bull Physically stronger
bull Tip runs hotter ndash less sample deposition
bull Platinum
bull Chemically stronger
bull Used for higher acid conc (incl HF)
bull 2 centre sizes 10-18 mm
bull Higher cost
Potential Problems
bull Biggest risk is physical damage to the orifice due to excessively aggressive cleaning
bull Cones also affected by sample matrix (acid strength amp type) and number of samples analyzed each day
bull Nickel - Typically replace 3 or 5 each year (assumes measuring 250-350 environmental samples each day)
bull Platinum - Typically replace 1 or 2 each year (assumes measuring 20-50 semiconductor samples each day)
bull If not clean then can result in analytical problems eg poor signal stability elemental contamination
ICP-MS Maintenance amp Trouble Shooting
May 2012 19
System Cleanliness - Skimmer Cone
04 mm Orifice Nickel or Platinum
bull The Nickel skimmer cone is the standard interface
bull The skimmer cone is relatively robust to samples containing high concentrations of matrix and salts and is suitable for a wide variety of samples It is usually used with the Nickel sampling cone
bull The Platinum skimmer cone is usually used for introduction of hydrofluoric acid and other reagents It is usually used with the Platinum sampling cone
Potential Problems
bull Biggest risk is from physical damage to the orifice due to excessively aggressive cleaning
bull Cones also affected by sample matrix (acid strength amp type) and number of samples analyzed each day
bull Nickel ndash Typically replace 3 or 5 each year (assumes measuring 250-350 environmental samples each day)
bull Platinum ndash Typically replace 1 or 2 each year (assumes measuring 20-50 semiconductor samples each day)
bull If not clean then can result in analytical problems eg poor signal stability elemental contamination
20
ICP-MS Maintenance amp Trouble Shooting
May 2012
System Cleanliness - Cone Cleaning Procedure
Caution - Take care to avoid damage to the cone tip when removing ndash and place base down - Check the graphite gasket and replace if creased or damaged - Sonicate in a 2 Citranox or 2 Nitric Acid solution for a few minutes - Rinse well with de-ionized water - If still dirty or memory problems remain polish using an alumina powder slurry on a Q-tip then sonicate in 2 Citranox solution and rinse well with de-ionized water - Dry with nitrogen before installing
22
ICP-MS Maintenance amp Trouble Shooting
May 2012
Precision - Why is This Important
What does ldquoPrecisionrdquo mean
ndash Ability to get the same result for the same
sample when measured multiple times
ndash Usually measured as RSD or sometimes SD
RSD = (SD Mean Result) 100
ndash Low values indicate good precision
bull For ICP-MS expect 1-2 RSD
Why is this important
ndash User loses confidence in the system
What impacts on precision
ndash Nebulizerplasma stability
ndash Sample introduction system
ndash Method parameters
23
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash System stabilized
bull Allow 10 mins for plasma warm-up before
analysis
ndash Plasma status
bull ldquoBulletrdquo in the plasma should be stable
bull Check for deposits in the injector of the torch
ndash Check condition of interface cones and
clean if necessary
ndash Clean the Extraction Lens - Omega Lens
assembly
ndash Method parameters
bull Appropriate times set for sample uptake
delay and stabilization times
24
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash Sample Intro
What to Check ndash Nebulizer
bull Nebulizer type used can impact on sensitivity and precision
ndash MicroMist (glass concentric type) is the standard nebulizer ndash handles most sample
types
ndash PFA MicroFlow nebulizer best for low volume samples aggressive samples (HF
digests) and when low contamination required (semi-con)
ndash Babington gives poorer precision - best for high TDS samples
bull Check nebulizer condition regularly
ndash Chips in the nebulizer tip impact on aerosol formation ndash poor precision
(use a magnifying glass if necessary)
ndash Check for deposits or blockage in the tip
bull Sample uptake or flow rate
ndash Lower pump speed or using narrow bore pump tubing will reduce uptake rate
- better for high TDS samples
25
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Sample Introduction bull Contamination in the spray chamber
ndash When was the spray chamber cleaned
bull Any blockages in the nebulizer injector
ndash Check for stable aerosol formation
bull Air leaks in spray chamber end cap or connecting tubes
ndash Are they in good condition with tight connections
bull Damaged pump tubes
ndash When did you check the pump tubes
bull Is the pump speed too slow
ndash Low pump speeds may cause signal pulsation
ndash If required use narrower bore pump tube and increase pump speed
bull Samples have a high TDS content
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
26
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Memory effects
bull If possible avoid running high concentrations of these analytes
(Ag Au B Hg Mo Si Sn W Zn Zr)
ndash Maybe necessary to pre-dilute samples (if known to be high in concentration)
bull Ensure an adequate rinse time
ndash Should be at least equal to the sample uptake delay
(30-40 seconds typical)
bull May require an acidified rinse solution between samples
(2 HNO3)
bull Other strategies to minimize memory effects
ndash Use an inert spray chamber
ndash Use the ISIS to introduce discrete amounts of sample This means
bull Cones are exposed to less sample matrix = improved stability
bull Less memorycarry-over
bull Reduced uptake amp rinse times = faster measurement
27
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy - Why is This Important
What does ldquoAccuracyrdquo mean
ndash Ability to get the ldquorightrdquo answer for the sample
ndash Heavily dependent on operatorrsquos skill
Why is this important
ndash User loses confidence in the system
ndash Your reputationhellip
bull Customerrsquos question the results
bull Poor performance in ldquoround robinrdquo comparisons
How do You Confirm Accuracy
ndash Check the result for a prepared standard
ndash Measure a certified reference material
ndash Use other quality control checks to check analysis
28
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Calibration standards properly prepared
bull See earlier recommendations ndash important to match to samples prepare
accurately and use them ldquofreshrdquo
ndash Any interferences impacting on results
ndash Use matched standards or standard additions
ndash Ensure isotope selected has no polyatomic interferences
ndash If necessary use ORS3
ndash Precision optimized
bull Optimum signal to noise performance improves accuracy
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
29
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Reprocess data post
run using an
alternate internal
standard
bull Ensure Internal
Standard used is
similar in mass
bull Check whether the
Internal Standard is
present in the
sample
ndash If necessary do a Semi-
Quant measurement
bull Dilute with cal blk
matrix
30
Accuracy ndash Suspect Internal Standard Recovery
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Sample preparation
bull Is the most appropriate digestion being used
bull Are all of the analytes being quantitatively (and reproducibly) extracted and
dissolved
ndash Many digestions are only partial extracts ndash efficiency will vary with the
sample matrix
ndash Some volatile analytes may be ldquolostrdquo during digestion
bull Confirm by taking a solid certified reference material
through your preparation and analysis procedure
bull Is the digest stable ndash or are you seeing any precipitates or a suspension
bull Do you see any potential contamination from either reagents or the digestion
equipment eg especially with Si B or Ca
bull Include a ldquoReagent Blankrdquo with every sample batch to
monitor
31
ICP-MS Maintenance amp Trouble Shooting
May 2012
Laboratory environment can have
direct impact on quality of results
bull Clean uncluttered work area
bull Proper ventilation
bull Safety considerations
bull Instrument lifetime consideration
ICP-MS Maintenance amp Trouble Shooting
May 2012 32
Laboratory Environment
ICP-MS ndash Potential Autosampler Issues
ndash More customers use autosamplers with ICP for automation
ndash Issues to consider
bull Long transfer tube between sampler and ICP-MS
ndash May need to program a longer sample uptake delay
ndash May exacerbate problems with memory effects
ndash Use ldquoFast Pumprdquo during sample uptake delay
bull Caution ndash not always possible
Not recommended with high TDS samples and organics
bull Ensure probe diameter is appropriate for sample matrix
ndash Use wider bore for high TDS or viscous samples
bull Sample stability - potential for sample changes while uncovered in racks ndash impacts accuracy
ndash Dust ingress can introduce contamination
ndash Sample evaporation may occur during long unattended runs
ndash Sediment in the sample may settle out esp with wear metals or suspensions
bull Ensure transfer line to ICP-MS is in good condition
ndash Kinks in the line may cause poor uptake or pulsing in the sample
ndash Impacts on precision and accuracy
33
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sample Throughput ndash What to Check
ndash Samples fully digested
bull No excess particulates in the sample that may cause blockage
ndash Sample Introduction System optimized
ndash Capable of handling the TDS levels in the sample
ndash TorchNebulizer cleaned and ready for analysis
ndash Method parameters optimized
bull Sample uptake delay and stabilization times are appropriate ndash optimized
bull Integration time is appropriate for the expected concentration
ndash Use a longer integration time at low concentrations
bull Rinse time is appropriate
bull Use ldquoISISrdquo discrete sampling for faster measurement and faster washout
34
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Handles tough sample matrices better
than any other ICP-MS
ndash Highest plasma temperature (lowest
CeOCe) as standard
ndash HMI (high matrix introduction) allows direct
analysis of difficult samples
eg sea water
bull ORS3 operates in He collision mode to
remove ALL polyatomic interferences
ndash Enables reliable removal of all polyatomic
interferences using a single set of
conditions
ndash Gives lower levels of interference and
better long-term stability HMI gives lower suppression and
better long-term stability
Relative signal (suppression) in undiluted seawater
Long-term stability in undiluted seawater
35
Agilent ICP-MS Performance - Benefits
Best matrix tolerance amp less interferences
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS ndash Recommended Maintenance Schedule
ICP-MS Maintenance amp Trouble Shooting
May 2012 37
These functions
(and more) are
completed as part
of a Preventative
Maintenance
program by an
Agilent Field
Service Engineer
Summary ndash Key Consumables for ICP-MS
Sample preparationpresentation
ndash Peristaltic pump tubing
ndash Transfer and drain tubing
ndash ICP-MS standard solutions
ndash Internal Standard solutions
ndash Torches
ndash Spray chambers
ndash Nebulizers
Ion Extraction
ndash Sampler and skimmer cones
Autosampling
ndash Sample tubes racks probes and transfer tubing
ISIS
ndash Peristaltic pump tubing ferrules amp fittings
38
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sample Introduction
Key consumables requiring frequent replacement
bull Pump tubing
bull Torches and quartz transfer tube
bull Nebulizers
bull Spray chambers
bull Interface cones (skimmer amp sampler)
bull Transfer amp connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalogue
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24406(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 39
Autosampler Supplies
Key consumables requiring frequent replacement
ndash Peristaltic pump tubing
ndash Sample racks
ndash Sample tubes
ndash Spare probes
ndash Standard racks
ndash Connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24407(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 40
ISIS Supplies
Key consumables requiring frequent replacement
bull Peristaltic pump tubing
bull Ferrules and fittings
bull Valving
For ISIS Hydride Generation Accessory
bull Membrane filter
bull Concentric nebulizer
bull Gas-liquid separator
bull Other tubing and connectors
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceProductListingaspxcat=SubCat2ECS_24437(Agilent)amppcat=SubCat1ECS_24407(Agilent)amprcat=ClassECS_22674(Agilent)
41
ICP-MS Maintenance amp Trouble Shooting
May 2012
Where to Find the Right Consumable Analytical Consumables Agilent Assist
Consumables amp Supplies Instrument Sales ampServices 1-800-227-9770 (Option 11) 1-800-227-9770 (Option 13) wwwagilentcomchemcontactus wwwagilentcomchemcontactus
On-Line resources
ICP-MS Supplies
2nd Edition Speciation Handbook
ICP-MS Journal Archives
Recorded Agilent e-Seminars
ICP-OES Supplies
Atomic Absorption Supplies
Instrument Parts amp Supplies
Atomic Spec Application Notes
Agilent Quick Reference Guide for 77008800 ICP-MS (pub 5990-8182EN)
Agilent Atomic Spec Supplies Catalogue (pub 5990-8767EN)
Agilent Consumables Catalogue (pub 5990-6674EN)
Instrument User Manuals
42
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sensitivity ndash Quality of Standards
ndash What concentration are they
bull Low concentration standards have a finite life
ndash Prepare ppb (ugL) concentration standards daily from high conc stock
ndash Prepare low ppm (mgL) concentration standards weekly
ndash How are they prepared
bull Ensure purchased standards are still within ldquoUse Byrdquo date when used
bull Use calibrated pipettes and class lsquoArsquo volumetric flasks for dilutions
bull Use de-ionized water (Type I - conductivity gt 18 Mcm3) ndash lower grades may have
contamination
bull Please donrsquot do that 1100000 dilution
bull Donrsquot pipette direct from the bottle or return excess standard back to the bottle
ndash How are they stored
bull Plastic vessels ensure better stability
bull Stabilize with acid ndash low pH ensures better stability
6
ICP-MS Maintenance amp Trouble Shooting
May 2012
Detector
③Ion Transmission
Efficiency
②Plasma Ionization
Efficiency
①Nebulizer
Efficiency
7
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sensitivity ndash Itrsquos Determined Byhellip
Low ICP-MS Sensitivity
What to Check
ndash Standards prepared correctly and fresh
ndash Check the pump tubing (see tips on later slide)
and confirm pumping liquid smoothly
ndash Check for nebulizer blockage (use ldquonebulizer testrdquo in SW)
bull If required remove nebulizer and check liquid flowaerosol formation
ndash Check for blockage in the injector of the torch
bull Aspirate a Y solution
bull Check the position of ldquobulletrdquo in the plasma
bull Should be stable
ndash Check the interface cones (see tips on later slide)
ndash Check the ion lens (use ldquoion lens testrdquo in SW)
ndash Check torch positioning and tuning
ndash Check sensitivity in ldquono gas moderdquo ndash if OK suspect reaction gas purity
8
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sensitivity - Peristaltic Pump Tubing
bull Selection of tubing used for an application based on 2 key factors
ndash Resistance to the solvent in use
ndash ID of the tubing required (indicated by the coloured tabs)
bull Usersrsquo usually know what size they need
ndash Sample ndash 102 mm ID or whitewhite tabs
ndash Drain ndash 152 mm ID or yellowblue tabs
bull Smaller sizes used when application demands it
ndash Internal standard ndash 019 mm ID with orangered tabs
or 025 mm ID with orangeblue tabs
9
ICP-MS Maintenance amp Trouble Shooting
May 2012
Trim to 5-10mm to
reduce washout
and contamination
Potential Pump Tube Problems
10
ICP-MS Maintenance amp Trouble Shooting
May 2012
What to Check
ndash Tubing diameters
bull Want tubing used for waste to be larger ID than sample ID
ndash Chemical compatibility
bull Ensure tubing is resistant to the solvent being used
ndash Tube lifetime
bull Typical lifetime is ~1 week based on normal 8 hour working day
ndash Detach from tube holder after use ndash allows tube to ldquorelaxrdquo
bull Check 2 key things on pump tubing
ndash Roundness of tube ndash should not be any ldquoflatrdquo spots
ndash Tubing should still be elastic ndash replace if obviously stretched
bull Using ldquooldrdquo tubing can lead to problems with precision and stability
bull Installation and tensioning critical
ndash Donrsquot overtighten ndash just need smooth and even sample flow
ndash Remember to check other tubing for wear leaks and crimps
Normal wear amp tear
(~5 days) needs
replacing
ICP-MS Sensitivity ndash Method Parameters
What to Check
ndash Isotope selection
bull Using the most sensitive isotope
ndash Pump speed
bull Use the default speed as guide
bull Change pump tubing to give resistance to the solvent
ndash Interferences
bull Check for polyatomic interferences ndash try an alternate isotope first (if required)
ndash Otherwise use ORS3 to remove
bull Physical interferences can affect aerosol formation
ndash Use internal standard matched standards or standard additions
bull Chemical interferences can reduce atom formation and ionization
ndash Use higher RF power optimize neb flow + appropriate matrix modifiers
11
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sensitivity ndash Automated ldquoExpertrdquo Tuning
bull Startup provides a simple
user-configured schedule of
system optimization and
performance checks
bull One-click expert autotuning for
simple plasma optimization
bull Ensures consistent
performance from day to day
bull Independent of operator
experience
bull Automatically generate a
Performance Report
bull Provides a continuing record of
system performance
12
ICP-MS Maintenance amp Trouble Shooting
May 2012
13
Hardware Performance Report
is run under ldquostandardrdquo (factory
check-out) conditions
Gives record of performance
history under consistent default
tuning conditions
Note this is different to the ldquoTune
Reportrdquo which is generated
using Batch tune conditions
Sensitivity ndash Performance Report
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS specific contamination concerns -This is a topic of its own often leads to the clean room
conversation
But remember its not just where your instrument
is located ndash itrsquos everything the sample encounters
on its way to the instrument
ICP-MS Maintenance amp Trouble Shooting
May 2012 14
Sensitivity ndash Cleanliness amp Contamination
Sensitivity ndash Contamination Sources
bull Use high purity or ICP-MS grade reagents
bull Acid purity
ndash Buy only what you need to do the job
ndash Check the certificate of analysis
ndash Donrsquot insert pipette tips into your acids
ndash Use contaminated acid for cleaning
bull Sample containers
ndash Borosilicate glass introduces boron
ndash FEP containers preferred
bull Pipette tips
ndash Colors add interest ndash but increase contamination (Cu Fe Zn Cd)
bull Gloves
ndash Powder free unless you like Zn
Anything that touches sample during prep dilution
transfer analysis and storage
ICP-MS Maintenance amp Trouble Shooting
May 2012 15
PFA spray
chamber
PFA
endcap
PFA
nebulizer
PFA
connector
tube
Quartz torch with sapphire
or platinum injector
Complete sample introduction can be
changed to a system specifically
designed to reduce contamination
bull Usually used for semi-con applications
Clean integrated Auto-Sampler ndash I-AS
Clean sample introduction system - PFA
16
Cleanliness ndash The Ultimate for Contamination Free
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sensitivity ndash System Cleanliness
What to Check
ndash Sample Introduction System
bull Deposits in nebulizer can reduce
sample uptake rate
ndash Soak in aqua regia or use a nebulizer
cleaning tool to back flush
bull Solid material in torch injector
affects aerosol introduction into
plasma and increases noise
bull Contamination in spray chamber
impacts on aerosol formation ndash
increases noise
bull If seeing poor precision may be
due to beading in spray chamber
ndash Soak in 25 detergent solution
overnight (preferably for 24 hours)
17
ICP-MS Maintenance amp Trouble Shooting
May 2012
Nebulizer cleaner
Agilent PN G3266-80020
ICP-MS Sensitivity ndash System Cleanliness
What to Check
ndash Interface cones
bull Deposits or discoloration indicates
cleaning is required
bull Other indicators that cone cleaning
is required
ndash Poor sensitivity
ndash High background
ndash Distorted peak shapes
ndash Changes in interface vacuum reading
(deposition or build-up)
18
ICP-MS Maintenance amp Trouble Shooting
May 2012
Close up
Sample cone after measuring 75 undiluted sea water
samples using HMI Some deposition on outer edges
away from the orifice ndash no blockage of the sampling
orifice ndash but cleaning still recommended
System Cleanliness - Sampling Cone
1 mm Orifice Nickel or Platinum Centres
bull Nickel
bull Physically stronger
bull Tip runs hotter ndash less sample deposition
bull Platinum
bull Chemically stronger
bull Used for higher acid conc (incl HF)
bull 2 centre sizes 10-18 mm
bull Higher cost
Potential Problems
bull Biggest risk is physical damage to the orifice due to excessively aggressive cleaning
bull Cones also affected by sample matrix (acid strength amp type) and number of samples analyzed each day
bull Nickel - Typically replace 3 or 5 each year (assumes measuring 250-350 environmental samples each day)
bull Platinum - Typically replace 1 or 2 each year (assumes measuring 20-50 semiconductor samples each day)
bull If not clean then can result in analytical problems eg poor signal stability elemental contamination
ICP-MS Maintenance amp Trouble Shooting
May 2012 19
System Cleanliness - Skimmer Cone
04 mm Orifice Nickel or Platinum
bull The Nickel skimmer cone is the standard interface
bull The skimmer cone is relatively robust to samples containing high concentrations of matrix and salts and is suitable for a wide variety of samples It is usually used with the Nickel sampling cone
bull The Platinum skimmer cone is usually used for introduction of hydrofluoric acid and other reagents It is usually used with the Platinum sampling cone
Potential Problems
bull Biggest risk is from physical damage to the orifice due to excessively aggressive cleaning
bull Cones also affected by sample matrix (acid strength amp type) and number of samples analyzed each day
bull Nickel ndash Typically replace 3 or 5 each year (assumes measuring 250-350 environmental samples each day)
bull Platinum ndash Typically replace 1 or 2 each year (assumes measuring 20-50 semiconductor samples each day)
bull If not clean then can result in analytical problems eg poor signal stability elemental contamination
20
ICP-MS Maintenance amp Trouble Shooting
May 2012
System Cleanliness - Cone Cleaning Procedure
Caution - Take care to avoid damage to the cone tip when removing ndash and place base down - Check the graphite gasket and replace if creased or damaged - Sonicate in a 2 Citranox or 2 Nitric Acid solution for a few minutes - Rinse well with de-ionized water - If still dirty or memory problems remain polish using an alumina powder slurry on a Q-tip then sonicate in 2 Citranox solution and rinse well with de-ionized water - Dry with nitrogen before installing
22
ICP-MS Maintenance amp Trouble Shooting
May 2012
Precision - Why is This Important
What does ldquoPrecisionrdquo mean
ndash Ability to get the same result for the same
sample when measured multiple times
ndash Usually measured as RSD or sometimes SD
RSD = (SD Mean Result) 100
ndash Low values indicate good precision
bull For ICP-MS expect 1-2 RSD
Why is this important
ndash User loses confidence in the system
What impacts on precision
ndash Nebulizerplasma stability
ndash Sample introduction system
ndash Method parameters
23
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash System stabilized
bull Allow 10 mins for plasma warm-up before
analysis
ndash Plasma status
bull ldquoBulletrdquo in the plasma should be stable
bull Check for deposits in the injector of the torch
ndash Check condition of interface cones and
clean if necessary
ndash Clean the Extraction Lens - Omega Lens
assembly
ndash Method parameters
bull Appropriate times set for sample uptake
delay and stabilization times
24
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash Sample Intro
What to Check ndash Nebulizer
bull Nebulizer type used can impact on sensitivity and precision
ndash MicroMist (glass concentric type) is the standard nebulizer ndash handles most sample
types
ndash PFA MicroFlow nebulizer best for low volume samples aggressive samples (HF
digests) and when low contamination required (semi-con)
ndash Babington gives poorer precision - best for high TDS samples
bull Check nebulizer condition regularly
ndash Chips in the nebulizer tip impact on aerosol formation ndash poor precision
(use a magnifying glass if necessary)
ndash Check for deposits or blockage in the tip
bull Sample uptake or flow rate
ndash Lower pump speed or using narrow bore pump tubing will reduce uptake rate
- better for high TDS samples
25
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Sample Introduction bull Contamination in the spray chamber
ndash When was the spray chamber cleaned
bull Any blockages in the nebulizer injector
ndash Check for stable aerosol formation
bull Air leaks in spray chamber end cap or connecting tubes
ndash Are they in good condition with tight connections
bull Damaged pump tubes
ndash When did you check the pump tubes
bull Is the pump speed too slow
ndash Low pump speeds may cause signal pulsation
ndash If required use narrower bore pump tube and increase pump speed
bull Samples have a high TDS content
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
26
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Memory effects
bull If possible avoid running high concentrations of these analytes
(Ag Au B Hg Mo Si Sn W Zn Zr)
ndash Maybe necessary to pre-dilute samples (if known to be high in concentration)
bull Ensure an adequate rinse time
ndash Should be at least equal to the sample uptake delay
(30-40 seconds typical)
bull May require an acidified rinse solution between samples
(2 HNO3)
bull Other strategies to minimize memory effects
ndash Use an inert spray chamber
ndash Use the ISIS to introduce discrete amounts of sample This means
bull Cones are exposed to less sample matrix = improved stability
bull Less memorycarry-over
bull Reduced uptake amp rinse times = faster measurement
27
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy - Why is This Important
What does ldquoAccuracyrdquo mean
ndash Ability to get the ldquorightrdquo answer for the sample
ndash Heavily dependent on operatorrsquos skill
Why is this important
ndash User loses confidence in the system
ndash Your reputationhellip
bull Customerrsquos question the results
bull Poor performance in ldquoround robinrdquo comparisons
How do You Confirm Accuracy
ndash Check the result for a prepared standard
ndash Measure a certified reference material
ndash Use other quality control checks to check analysis
28
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Calibration standards properly prepared
bull See earlier recommendations ndash important to match to samples prepare
accurately and use them ldquofreshrdquo
ndash Any interferences impacting on results
ndash Use matched standards or standard additions
ndash Ensure isotope selected has no polyatomic interferences
ndash If necessary use ORS3
ndash Precision optimized
bull Optimum signal to noise performance improves accuracy
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
29
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Reprocess data post
run using an
alternate internal
standard
bull Ensure Internal
Standard used is
similar in mass
bull Check whether the
Internal Standard is
present in the
sample
ndash If necessary do a Semi-
Quant measurement
bull Dilute with cal blk
matrix
30
Accuracy ndash Suspect Internal Standard Recovery
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Sample preparation
bull Is the most appropriate digestion being used
bull Are all of the analytes being quantitatively (and reproducibly) extracted and
dissolved
ndash Many digestions are only partial extracts ndash efficiency will vary with the
sample matrix
ndash Some volatile analytes may be ldquolostrdquo during digestion
bull Confirm by taking a solid certified reference material
through your preparation and analysis procedure
bull Is the digest stable ndash or are you seeing any precipitates or a suspension
bull Do you see any potential contamination from either reagents or the digestion
equipment eg especially with Si B or Ca
bull Include a ldquoReagent Blankrdquo with every sample batch to
monitor
31
ICP-MS Maintenance amp Trouble Shooting
May 2012
Laboratory environment can have
direct impact on quality of results
bull Clean uncluttered work area
bull Proper ventilation
bull Safety considerations
bull Instrument lifetime consideration
ICP-MS Maintenance amp Trouble Shooting
May 2012 32
Laboratory Environment
ICP-MS ndash Potential Autosampler Issues
ndash More customers use autosamplers with ICP for automation
ndash Issues to consider
bull Long transfer tube between sampler and ICP-MS
ndash May need to program a longer sample uptake delay
ndash May exacerbate problems with memory effects
ndash Use ldquoFast Pumprdquo during sample uptake delay
bull Caution ndash not always possible
Not recommended with high TDS samples and organics
bull Ensure probe diameter is appropriate for sample matrix
ndash Use wider bore for high TDS or viscous samples
bull Sample stability - potential for sample changes while uncovered in racks ndash impacts accuracy
ndash Dust ingress can introduce contamination
ndash Sample evaporation may occur during long unattended runs
ndash Sediment in the sample may settle out esp with wear metals or suspensions
bull Ensure transfer line to ICP-MS is in good condition
ndash Kinks in the line may cause poor uptake or pulsing in the sample
ndash Impacts on precision and accuracy
33
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sample Throughput ndash What to Check
ndash Samples fully digested
bull No excess particulates in the sample that may cause blockage
ndash Sample Introduction System optimized
ndash Capable of handling the TDS levels in the sample
ndash TorchNebulizer cleaned and ready for analysis
ndash Method parameters optimized
bull Sample uptake delay and stabilization times are appropriate ndash optimized
bull Integration time is appropriate for the expected concentration
ndash Use a longer integration time at low concentrations
bull Rinse time is appropriate
bull Use ldquoISISrdquo discrete sampling for faster measurement and faster washout
34
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Handles tough sample matrices better
than any other ICP-MS
ndash Highest plasma temperature (lowest
CeOCe) as standard
ndash HMI (high matrix introduction) allows direct
analysis of difficult samples
eg sea water
bull ORS3 operates in He collision mode to
remove ALL polyatomic interferences
ndash Enables reliable removal of all polyatomic
interferences using a single set of
conditions
ndash Gives lower levels of interference and
better long-term stability HMI gives lower suppression and
better long-term stability
Relative signal (suppression) in undiluted seawater
Long-term stability in undiluted seawater
35
Agilent ICP-MS Performance - Benefits
Best matrix tolerance amp less interferences
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS ndash Recommended Maintenance Schedule
ICP-MS Maintenance amp Trouble Shooting
May 2012 37
These functions
(and more) are
completed as part
of a Preventative
Maintenance
program by an
Agilent Field
Service Engineer
Summary ndash Key Consumables for ICP-MS
Sample preparationpresentation
ndash Peristaltic pump tubing
ndash Transfer and drain tubing
ndash ICP-MS standard solutions
ndash Internal Standard solutions
ndash Torches
ndash Spray chambers
ndash Nebulizers
Ion Extraction
ndash Sampler and skimmer cones
Autosampling
ndash Sample tubes racks probes and transfer tubing
ISIS
ndash Peristaltic pump tubing ferrules amp fittings
38
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sample Introduction
Key consumables requiring frequent replacement
bull Pump tubing
bull Torches and quartz transfer tube
bull Nebulizers
bull Spray chambers
bull Interface cones (skimmer amp sampler)
bull Transfer amp connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalogue
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24406(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 39
Autosampler Supplies
Key consumables requiring frequent replacement
ndash Peristaltic pump tubing
ndash Sample racks
ndash Sample tubes
ndash Spare probes
ndash Standard racks
ndash Connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24407(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 40
ISIS Supplies
Key consumables requiring frequent replacement
bull Peristaltic pump tubing
bull Ferrules and fittings
bull Valving
For ISIS Hydride Generation Accessory
bull Membrane filter
bull Concentric nebulizer
bull Gas-liquid separator
bull Other tubing and connectors
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceProductListingaspxcat=SubCat2ECS_24437(Agilent)amppcat=SubCat1ECS_24407(Agilent)amprcat=ClassECS_22674(Agilent)
41
ICP-MS Maintenance amp Trouble Shooting
May 2012
Where to Find the Right Consumable Analytical Consumables Agilent Assist
Consumables amp Supplies Instrument Sales ampServices 1-800-227-9770 (Option 11) 1-800-227-9770 (Option 13) wwwagilentcomchemcontactus wwwagilentcomchemcontactus
On-Line resources
ICP-MS Supplies
2nd Edition Speciation Handbook
ICP-MS Journal Archives
Recorded Agilent e-Seminars
ICP-OES Supplies
Atomic Absorption Supplies
Instrument Parts amp Supplies
Atomic Spec Application Notes
Agilent Quick Reference Guide for 77008800 ICP-MS (pub 5990-8182EN)
Agilent Atomic Spec Supplies Catalogue (pub 5990-8767EN)
Agilent Consumables Catalogue (pub 5990-6674EN)
Instrument User Manuals
42
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
Detector
③Ion Transmission
Efficiency
②Plasma Ionization
Efficiency
①Nebulizer
Efficiency
7
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sensitivity ndash Itrsquos Determined Byhellip
Low ICP-MS Sensitivity
What to Check
ndash Standards prepared correctly and fresh
ndash Check the pump tubing (see tips on later slide)
and confirm pumping liquid smoothly
ndash Check for nebulizer blockage (use ldquonebulizer testrdquo in SW)
bull If required remove nebulizer and check liquid flowaerosol formation
ndash Check for blockage in the injector of the torch
bull Aspirate a Y solution
bull Check the position of ldquobulletrdquo in the plasma
bull Should be stable
ndash Check the interface cones (see tips on later slide)
ndash Check the ion lens (use ldquoion lens testrdquo in SW)
ndash Check torch positioning and tuning
ndash Check sensitivity in ldquono gas moderdquo ndash if OK suspect reaction gas purity
8
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sensitivity - Peristaltic Pump Tubing
bull Selection of tubing used for an application based on 2 key factors
ndash Resistance to the solvent in use
ndash ID of the tubing required (indicated by the coloured tabs)
bull Usersrsquo usually know what size they need
ndash Sample ndash 102 mm ID or whitewhite tabs
ndash Drain ndash 152 mm ID or yellowblue tabs
bull Smaller sizes used when application demands it
ndash Internal standard ndash 019 mm ID with orangered tabs
or 025 mm ID with orangeblue tabs
9
ICP-MS Maintenance amp Trouble Shooting
May 2012
Trim to 5-10mm to
reduce washout
and contamination
Potential Pump Tube Problems
10
ICP-MS Maintenance amp Trouble Shooting
May 2012
What to Check
ndash Tubing diameters
bull Want tubing used for waste to be larger ID than sample ID
ndash Chemical compatibility
bull Ensure tubing is resistant to the solvent being used
ndash Tube lifetime
bull Typical lifetime is ~1 week based on normal 8 hour working day
ndash Detach from tube holder after use ndash allows tube to ldquorelaxrdquo
bull Check 2 key things on pump tubing
ndash Roundness of tube ndash should not be any ldquoflatrdquo spots
ndash Tubing should still be elastic ndash replace if obviously stretched
bull Using ldquooldrdquo tubing can lead to problems with precision and stability
bull Installation and tensioning critical
ndash Donrsquot overtighten ndash just need smooth and even sample flow
ndash Remember to check other tubing for wear leaks and crimps
Normal wear amp tear
(~5 days) needs
replacing
ICP-MS Sensitivity ndash Method Parameters
What to Check
ndash Isotope selection
bull Using the most sensitive isotope
ndash Pump speed
bull Use the default speed as guide
bull Change pump tubing to give resistance to the solvent
ndash Interferences
bull Check for polyatomic interferences ndash try an alternate isotope first (if required)
ndash Otherwise use ORS3 to remove
bull Physical interferences can affect aerosol formation
ndash Use internal standard matched standards or standard additions
bull Chemical interferences can reduce atom formation and ionization
ndash Use higher RF power optimize neb flow + appropriate matrix modifiers
11
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sensitivity ndash Automated ldquoExpertrdquo Tuning
bull Startup provides a simple
user-configured schedule of
system optimization and
performance checks
bull One-click expert autotuning for
simple plasma optimization
bull Ensures consistent
performance from day to day
bull Independent of operator
experience
bull Automatically generate a
Performance Report
bull Provides a continuing record of
system performance
12
ICP-MS Maintenance amp Trouble Shooting
May 2012
13
Hardware Performance Report
is run under ldquostandardrdquo (factory
check-out) conditions
Gives record of performance
history under consistent default
tuning conditions
Note this is different to the ldquoTune
Reportrdquo which is generated
using Batch tune conditions
Sensitivity ndash Performance Report
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS specific contamination concerns -This is a topic of its own often leads to the clean room
conversation
But remember its not just where your instrument
is located ndash itrsquos everything the sample encounters
on its way to the instrument
ICP-MS Maintenance amp Trouble Shooting
May 2012 14
Sensitivity ndash Cleanliness amp Contamination
Sensitivity ndash Contamination Sources
bull Use high purity or ICP-MS grade reagents
bull Acid purity
ndash Buy only what you need to do the job
ndash Check the certificate of analysis
ndash Donrsquot insert pipette tips into your acids
ndash Use contaminated acid for cleaning
bull Sample containers
ndash Borosilicate glass introduces boron
ndash FEP containers preferred
bull Pipette tips
ndash Colors add interest ndash but increase contamination (Cu Fe Zn Cd)
bull Gloves
ndash Powder free unless you like Zn
Anything that touches sample during prep dilution
transfer analysis and storage
ICP-MS Maintenance amp Trouble Shooting
May 2012 15
PFA spray
chamber
PFA
endcap
PFA
nebulizer
PFA
connector
tube
Quartz torch with sapphire
or platinum injector
Complete sample introduction can be
changed to a system specifically
designed to reduce contamination
bull Usually used for semi-con applications
Clean integrated Auto-Sampler ndash I-AS
Clean sample introduction system - PFA
16
Cleanliness ndash The Ultimate for Contamination Free
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sensitivity ndash System Cleanliness
What to Check
ndash Sample Introduction System
bull Deposits in nebulizer can reduce
sample uptake rate
ndash Soak in aqua regia or use a nebulizer
cleaning tool to back flush
bull Solid material in torch injector
affects aerosol introduction into
plasma and increases noise
bull Contamination in spray chamber
impacts on aerosol formation ndash
increases noise
bull If seeing poor precision may be
due to beading in spray chamber
ndash Soak in 25 detergent solution
overnight (preferably for 24 hours)
17
ICP-MS Maintenance amp Trouble Shooting
May 2012
Nebulizer cleaner
Agilent PN G3266-80020
ICP-MS Sensitivity ndash System Cleanliness
What to Check
ndash Interface cones
bull Deposits or discoloration indicates
cleaning is required
bull Other indicators that cone cleaning
is required
ndash Poor sensitivity
ndash High background
ndash Distorted peak shapes
ndash Changes in interface vacuum reading
(deposition or build-up)
18
ICP-MS Maintenance amp Trouble Shooting
May 2012
Close up
Sample cone after measuring 75 undiluted sea water
samples using HMI Some deposition on outer edges
away from the orifice ndash no blockage of the sampling
orifice ndash but cleaning still recommended
System Cleanliness - Sampling Cone
1 mm Orifice Nickel or Platinum Centres
bull Nickel
bull Physically stronger
bull Tip runs hotter ndash less sample deposition
bull Platinum
bull Chemically stronger
bull Used for higher acid conc (incl HF)
bull 2 centre sizes 10-18 mm
bull Higher cost
Potential Problems
bull Biggest risk is physical damage to the orifice due to excessively aggressive cleaning
bull Cones also affected by sample matrix (acid strength amp type) and number of samples analyzed each day
bull Nickel - Typically replace 3 or 5 each year (assumes measuring 250-350 environmental samples each day)
bull Platinum - Typically replace 1 or 2 each year (assumes measuring 20-50 semiconductor samples each day)
bull If not clean then can result in analytical problems eg poor signal stability elemental contamination
ICP-MS Maintenance amp Trouble Shooting
May 2012 19
System Cleanliness - Skimmer Cone
04 mm Orifice Nickel or Platinum
bull The Nickel skimmer cone is the standard interface
bull The skimmer cone is relatively robust to samples containing high concentrations of matrix and salts and is suitable for a wide variety of samples It is usually used with the Nickel sampling cone
bull The Platinum skimmer cone is usually used for introduction of hydrofluoric acid and other reagents It is usually used with the Platinum sampling cone
Potential Problems
bull Biggest risk is from physical damage to the orifice due to excessively aggressive cleaning
bull Cones also affected by sample matrix (acid strength amp type) and number of samples analyzed each day
bull Nickel ndash Typically replace 3 or 5 each year (assumes measuring 250-350 environmental samples each day)
bull Platinum ndash Typically replace 1 or 2 each year (assumes measuring 20-50 semiconductor samples each day)
bull If not clean then can result in analytical problems eg poor signal stability elemental contamination
20
ICP-MS Maintenance amp Trouble Shooting
May 2012
System Cleanliness - Cone Cleaning Procedure
Caution - Take care to avoid damage to the cone tip when removing ndash and place base down - Check the graphite gasket and replace if creased or damaged - Sonicate in a 2 Citranox or 2 Nitric Acid solution for a few minutes - Rinse well with de-ionized water - If still dirty or memory problems remain polish using an alumina powder slurry on a Q-tip then sonicate in 2 Citranox solution and rinse well with de-ionized water - Dry with nitrogen before installing
22
ICP-MS Maintenance amp Trouble Shooting
May 2012
Precision - Why is This Important
What does ldquoPrecisionrdquo mean
ndash Ability to get the same result for the same
sample when measured multiple times
ndash Usually measured as RSD or sometimes SD
RSD = (SD Mean Result) 100
ndash Low values indicate good precision
bull For ICP-MS expect 1-2 RSD
Why is this important
ndash User loses confidence in the system
What impacts on precision
ndash Nebulizerplasma stability
ndash Sample introduction system
ndash Method parameters
23
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash System stabilized
bull Allow 10 mins for plasma warm-up before
analysis
ndash Plasma status
bull ldquoBulletrdquo in the plasma should be stable
bull Check for deposits in the injector of the torch
ndash Check condition of interface cones and
clean if necessary
ndash Clean the Extraction Lens - Omega Lens
assembly
ndash Method parameters
bull Appropriate times set for sample uptake
delay and stabilization times
24
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash Sample Intro
What to Check ndash Nebulizer
bull Nebulizer type used can impact on sensitivity and precision
ndash MicroMist (glass concentric type) is the standard nebulizer ndash handles most sample
types
ndash PFA MicroFlow nebulizer best for low volume samples aggressive samples (HF
digests) and when low contamination required (semi-con)
ndash Babington gives poorer precision - best for high TDS samples
bull Check nebulizer condition regularly
ndash Chips in the nebulizer tip impact on aerosol formation ndash poor precision
(use a magnifying glass if necessary)
ndash Check for deposits or blockage in the tip
bull Sample uptake or flow rate
ndash Lower pump speed or using narrow bore pump tubing will reduce uptake rate
- better for high TDS samples
25
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Sample Introduction bull Contamination in the spray chamber
ndash When was the spray chamber cleaned
bull Any blockages in the nebulizer injector
ndash Check for stable aerosol formation
bull Air leaks in spray chamber end cap or connecting tubes
ndash Are they in good condition with tight connections
bull Damaged pump tubes
ndash When did you check the pump tubes
bull Is the pump speed too slow
ndash Low pump speeds may cause signal pulsation
ndash If required use narrower bore pump tube and increase pump speed
bull Samples have a high TDS content
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
26
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Memory effects
bull If possible avoid running high concentrations of these analytes
(Ag Au B Hg Mo Si Sn W Zn Zr)
ndash Maybe necessary to pre-dilute samples (if known to be high in concentration)
bull Ensure an adequate rinse time
ndash Should be at least equal to the sample uptake delay
(30-40 seconds typical)
bull May require an acidified rinse solution between samples
(2 HNO3)
bull Other strategies to minimize memory effects
ndash Use an inert spray chamber
ndash Use the ISIS to introduce discrete amounts of sample This means
bull Cones are exposed to less sample matrix = improved stability
bull Less memorycarry-over
bull Reduced uptake amp rinse times = faster measurement
27
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy - Why is This Important
What does ldquoAccuracyrdquo mean
ndash Ability to get the ldquorightrdquo answer for the sample
ndash Heavily dependent on operatorrsquos skill
Why is this important
ndash User loses confidence in the system
ndash Your reputationhellip
bull Customerrsquos question the results
bull Poor performance in ldquoround robinrdquo comparisons
How do You Confirm Accuracy
ndash Check the result for a prepared standard
ndash Measure a certified reference material
ndash Use other quality control checks to check analysis
28
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Calibration standards properly prepared
bull See earlier recommendations ndash important to match to samples prepare
accurately and use them ldquofreshrdquo
ndash Any interferences impacting on results
ndash Use matched standards or standard additions
ndash Ensure isotope selected has no polyatomic interferences
ndash If necessary use ORS3
ndash Precision optimized
bull Optimum signal to noise performance improves accuracy
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
29
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Reprocess data post
run using an
alternate internal
standard
bull Ensure Internal
Standard used is
similar in mass
bull Check whether the
Internal Standard is
present in the
sample
ndash If necessary do a Semi-
Quant measurement
bull Dilute with cal blk
matrix
30
Accuracy ndash Suspect Internal Standard Recovery
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Sample preparation
bull Is the most appropriate digestion being used
bull Are all of the analytes being quantitatively (and reproducibly) extracted and
dissolved
ndash Many digestions are only partial extracts ndash efficiency will vary with the
sample matrix
ndash Some volatile analytes may be ldquolostrdquo during digestion
bull Confirm by taking a solid certified reference material
through your preparation and analysis procedure
bull Is the digest stable ndash or are you seeing any precipitates or a suspension
bull Do you see any potential contamination from either reagents or the digestion
equipment eg especially with Si B or Ca
bull Include a ldquoReagent Blankrdquo with every sample batch to
monitor
31
ICP-MS Maintenance amp Trouble Shooting
May 2012
Laboratory environment can have
direct impact on quality of results
bull Clean uncluttered work area
bull Proper ventilation
bull Safety considerations
bull Instrument lifetime consideration
ICP-MS Maintenance amp Trouble Shooting
May 2012 32
Laboratory Environment
ICP-MS ndash Potential Autosampler Issues
ndash More customers use autosamplers with ICP for automation
ndash Issues to consider
bull Long transfer tube between sampler and ICP-MS
ndash May need to program a longer sample uptake delay
ndash May exacerbate problems with memory effects
ndash Use ldquoFast Pumprdquo during sample uptake delay
bull Caution ndash not always possible
Not recommended with high TDS samples and organics
bull Ensure probe diameter is appropriate for sample matrix
ndash Use wider bore for high TDS or viscous samples
bull Sample stability - potential for sample changes while uncovered in racks ndash impacts accuracy
ndash Dust ingress can introduce contamination
ndash Sample evaporation may occur during long unattended runs
ndash Sediment in the sample may settle out esp with wear metals or suspensions
bull Ensure transfer line to ICP-MS is in good condition
ndash Kinks in the line may cause poor uptake or pulsing in the sample
ndash Impacts on precision and accuracy
33
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sample Throughput ndash What to Check
ndash Samples fully digested
bull No excess particulates in the sample that may cause blockage
ndash Sample Introduction System optimized
ndash Capable of handling the TDS levels in the sample
ndash TorchNebulizer cleaned and ready for analysis
ndash Method parameters optimized
bull Sample uptake delay and stabilization times are appropriate ndash optimized
bull Integration time is appropriate for the expected concentration
ndash Use a longer integration time at low concentrations
bull Rinse time is appropriate
bull Use ldquoISISrdquo discrete sampling for faster measurement and faster washout
34
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Handles tough sample matrices better
than any other ICP-MS
ndash Highest plasma temperature (lowest
CeOCe) as standard
ndash HMI (high matrix introduction) allows direct
analysis of difficult samples
eg sea water
bull ORS3 operates in He collision mode to
remove ALL polyatomic interferences
ndash Enables reliable removal of all polyatomic
interferences using a single set of
conditions
ndash Gives lower levels of interference and
better long-term stability HMI gives lower suppression and
better long-term stability
Relative signal (suppression) in undiluted seawater
Long-term stability in undiluted seawater
35
Agilent ICP-MS Performance - Benefits
Best matrix tolerance amp less interferences
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS ndash Recommended Maintenance Schedule
ICP-MS Maintenance amp Trouble Shooting
May 2012 37
These functions
(and more) are
completed as part
of a Preventative
Maintenance
program by an
Agilent Field
Service Engineer
Summary ndash Key Consumables for ICP-MS
Sample preparationpresentation
ndash Peristaltic pump tubing
ndash Transfer and drain tubing
ndash ICP-MS standard solutions
ndash Internal Standard solutions
ndash Torches
ndash Spray chambers
ndash Nebulizers
Ion Extraction
ndash Sampler and skimmer cones
Autosampling
ndash Sample tubes racks probes and transfer tubing
ISIS
ndash Peristaltic pump tubing ferrules amp fittings
38
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sample Introduction
Key consumables requiring frequent replacement
bull Pump tubing
bull Torches and quartz transfer tube
bull Nebulizers
bull Spray chambers
bull Interface cones (skimmer amp sampler)
bull Transfer amp connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalogue
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24406(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 39
Autosampler Supplies
Key consumables requiring frequent replacement
ndash Peristaltic pump tubing
ndash Sample racks
ndash Sample tubes
ndash Spare probes
ndash Standard racks
ndash Connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24407(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 40
ISIS Supplies
Key consumables requiring frequent replacement
bull Peristaltic pump tubing
bull Ferrules and fittings
bull Valving
For ISIS Hydride Generation Accessory
bull Membrane filter
bull Concentric nebulizer
bull Gas-liquid separator
bull Other tubing and connectors
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceProductListingaspxcat=SubCat2ECS_24437(Agilent)amppcat=SubCat1ECS_24407(Agilent)amprcat=ClassECS_22674(Agilent)
41
ICP-MS Maintenance amp Trouble Shooting
May 2012
Where to Find the Right Consumable Analytical Consumables Agilent Assist
Consumables amp Supplies Instrument Sales ampServices 1-800-227-9770 (Option 11) 1-800-227-9770 (Option 13) wwwagilentcomchemcontactus wwwagilentcomchemcontactus
On-Line resources
ICP-MS Supplies
2nd Edition Speciation Handbook
ICP-MS Journal Archives
Recorded Agilent e-Seminars
ICP-OES Supplies
Atomic Absorption Supplies
Instrument Parts amp Supplies
Atomic Spec Application Notes
Agilent Quick Reference Guide for 77008800 ICP-MS (pub 5990-8182EN)
Agilent Atomic Spec Supplies Catalogue (pub 5990-8767EN)
Agilent Consumables Catalogue (pub 5990-6674EN)
Instrument User Manuals
42
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
Low ICP-MS Sensitivity
What to Check
ndash Standards prepared correctly and fresh
ndash Check the pump tubing (see tips on later slide)
and confirm pumping liquid smoothly
ndash Check for nebulizer blockage (use ldquonebulizer testrdquo in SW)
bull If required remove nebulizer and check liquid flowaerosol formation
ndash Check for blockage in the injector of the torch
bull Aspirate a Y solution
bull Check the position of ldquobulletrdquo in the plasma
bull Should be stable
ndash Check the interface cones (see tips on later slide)
ndash Check the ion lens (use ldquoion lens testrdquo in SW)
ndash Check torch positioning and tuning
ndash Check sensitivity in ldquono gas moderdquo ndash if OK suspect reaction gas purity
8
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sensitivity - Peristaltic Pump Tubing
bull Selection of tubing used for an application based on 2 key factors
ndash Resistance to the solvent in use
ndash ID of the tubing required (indicated by the coloured tabs)
bull Usersrsquo usually know what size they need
ndash Sample ndash 102 mm ID or whitewhite tabs
ndash Drain ndash 152 mm ID or yellowblue tabs
bull Smaller sizes used when application demands it
ndash Internal standard ndash 019 mm ID with orangered tabs
or 025 mm ID with orangeblue tabs
9
ICP-MS Maintenance amp Trouble Shooting
May 2012
Trim to 5-10mm to
reduce washout
and contamination
Potential Pump Tube Problems
10
ICP-MS Maintenance amp Trouble Shooting
May 2012
What to Check
ndash Tubing diameters
bull Want tubing used for waste to be larger ID than sample ID
ndash Chemical compatibility
bull Ensure tubing is resistant to the solvent being used
ndash Tube lifetime
bull Typical lifetime is ~1 week based on normal 8 hour working day
ndash Detach from tube holder after use ndash allows tube to ldquorelaxrdquo
bull Check 2 key things on pump tubing
ndash Roundness of tube ndash should not be any ldquoflatrdquo spots
ndash Tubing should still be elastic ndash replace if obviously stretched
bull Using ldquooldrdquo tubing can lead to problems with precision and stability
bull Installation and tensioning critical
ndash Donrsquot overtighten ndash just need smooth and even sample flow
ndash Remember to check other tubing for wear leaks and crimps
Normal wear amp tear
(~5 days) needs
replacing
ICP-MS Sensitivity ndash Method Parameters
What to Check
ndash Isotope selection
bull Using the most sensitive isotope
ndash Pump speed
bull Use the default speed as guide
bull Change pump tubing to give resistance to the solvent
ndash Interferences
bull Check for polyatomic interferences ndash try an alternate isotope first (if required)
ndash Otherwise use ORS3 to remove
bull Physical interferences can affect aerosol formation
ndash Use internal standard matched standards or standard additions
bull Chemical interferences can reduce atom formation and ionization
ndash Use higher RF power optimize neb flow + appropriate matrix modifiers
11
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sensitivity ndash Automated ldquoExpertrdquo Tuning
bull Startup provides a simple
user-configured schedule of
system optimization and
performance checks
bull One-click expert autotuning for
simple plasma optimization
bull Ensures consistent
performance from day to day
bull Independent of operator
experience
bull Automatically generate a
Performance Report
bull Provides a continuing record of
system performance
12
ICP-MS Maintenance amp Trouble Shooting
May 2012
13
Hardware Performance Report
is run under ldquostandardrdquo (factory
check-out) conditions
Gives record of performance
history under consistent default
tuning conditions
Note this is different to the ldquoTune
Reportrdquo which is generated
using Batch tune conditions
Sensitivity ndash Performance Report
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS specific contamination concerns -This is a topic of its own often leads to the clean room
conversation
But remember its not just where your instrument
is located ndash itrsquos everything the sample encounters
on its way to the instrument
ICP-MS Maintenance amp Trouble Shooting
May 2012 14
Sensitivity ndash Cleanliness amp Contamination
Sensitivity ndash Contamination Sources
bull Use high purity or ICP-MS grade reagents
bull Acid purity
ndash Buy only what you need to do the job
ndash Check the certificate of analysis
ndash Donrsquot insert pipette tips into your acids
ndash Use contaminated acid for cleaning
bull Sample containers
ndash Borosilicate glass introduces boron
ndash FEP containers preferred
bull Pipette tips
ndash Colors add interest ndash but increase contamination (Cu Fe Zn Cd)
bull Gloves
ndash Powder free unless you like Zn
Anything that touches sample during prep dilution
transfer analysis and storage
ICP-MS Maintenance amp Trouble Shooting
May 2012 15
PFA spray
chamber
PFA
endcap
PFA
nebulizer
PFA
connector
tube
Quartz torch with sapphire
or platinum injector
Complete sample introduction can be
changed to a system specifically
designed to reduce contamination
bull Usually used for semi-con applications
Clean integrated Auto-Sampler ndash I-AS
Clean sample introduction system - PFA
16
Cleanliness ndash The Ultimate for Contamination Free
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sensitivity ndash System Cleanliness
What to Check
ndash Sample Introduction System
bull Deposits in nebulizer can reduce
sample uptake rate
ndash Soak in aqua regia or use a nebulizer
cleaning tool to back flush
bull Solid material in torch injector
affects aerosol introduction into
plasma and increases noise
bull Contamination in spray chamber
impacts on aerosol formation ndash
increases noise
bull If seeing poor precision may be
due to beading in spray chamber
ndash Soak in 25 detergent solution
overnight (preferably for 24 hours)
17
ICP-MS Maintenance amp Trouble Shooting
May 2012
Nebulizer cleaner
Agilent PN G3266-80020
ICP-MS Sensitivity ndash System Cleanliness
What to Check
ndash Interface cones
bull Deposits or discoloration indicates
cleaning is required
bull Other indicators that cone cleaning
is required
ndash Poor sensitivity
ndash High background
ndash Distorted peak shapes
ndash Changes in interface vacuum reading
(deposition or build-up)
18
ICP-MS Maintenance amp Trouble Shooting
May 2012
Close up
Sample cone after measuring 75 undiluted sea water
samples using HMI Some deposition on outer edges
away from the orifice ndash no blockage of the sampling
orifice ndash but cleaning still recommended
System Cleanliness - Sampling Cone
1 mm Orifice Nickel or Platinum Centres
bull Nickel
bull Physically stronger
bull Tip runs hotter ndash less sample deposition
bull Platinum
bull Chemically stronger
bull Used for higher acid conc (incl HF)
bull 2 centre sizes 10-18 mm
bull Higher cost
Potential Problems
bull Biggest risk is physical damage to the orifice due to excessively aggressive cleaning
bull Cones also affected by sample matrix (acid strength amp type) and number of samples analyzed each day
bull Nickel - Typically replace 3 or 5 each year (assumes measuring 250-350 environmental samples each day)
bull Platinum - Typically replace 1 or 2 each year (assumes measuring 20-50 semiconductor samples each day)
bull If not clean then can result in analytical problems eg poor signal stability elemental contamination
ICP-MS Maintenance amp Trouble Shooting
May 2012 19
System Cleanliness - Skimmer Cone
04 mm Orifice Nickel or Platinum
bull The Nickel skimmer cone is the standard interface
bull The skimmer cone is relatively robust to samples containing high concentrations of matrix and salts and is suitable for a wide variety of samples It is usually used with the Nickel sampling cone
bull The Platinum skimmer cone is usually used for introduction of hydrofluoric acid and other reagents It is usually used with the Platinum sampling cone
Potential Problems
bull Biggest risk is from physical damage to the orifice due to excessively aggressive cleaning
bull Cones also affected by sample matrix (acid strength amp type) and number of samples analyzed each day
bull Nickel ndash Typically replace 3 or 5 each year (assumes measuring 250-350 environmental samples each day)
bull Platinum ndash Typically replace 1 or 2 each year (assumes measuring 20-50 semiconductor samples each day)
bull If not clean then can result in analytical problems eg poor signal stability elemental contamination
20
ICP-MS Maintenance amp Trouble Shooting
May 2012
System Cleanliness - Cone Cleaning Procedure
Caution - Take care to avoid damage to the cone tip when removing ndash and place base down - Check the graphite gasket and replace if creased or damaged - Sonicate in a 2 Citranox or 2 Nitric Acid solution for a few minutes - Rinse well with de-ionized water - If still dirty or memory problems remain polish using an alumina powder slurry on a Q-tip then sonicate in 2 Citranox solution and rinse well with de-ionized water - Dry with nitrogen before installing
22
ICP-MS Maintenance amp Trouble Shooting
May 2012
Precision - Why is This Important
What does ldquoPrecisionrdquo mean
ndash Ability to get the same result for the same
sample when measured multiple times
ndash Usually measured as RSD or sometimes SD
RSD = (SD Mean Result) 100
ndash Low values indicate good precision
bull For ICP-MS expect 1-2 RSD
Why is this important
ndash User loses confidence in the system
What impacts on precision
ndash Nebulizerplasma stability
ndash Sample introduction system
ndash Method parameters
23
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash System stabilized
bull Allow 10 mins for plasma warm-up before
analysis
ndash Plasma status
bull ldquoBulletrdquo in the plasma should be stable
bull Check for deposits in the injector of the torch
ndash Check condition of interface cones and
clean if necessary
ndash Clean the Extraction Lens - Omega Lens
assembly
ndash Method parameters
bull Appropriate times set for sample uptake
delay and stabilization times
24
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash Sample Intro
What to Check ndash Nebulizer
bull Nebulizer type used can impact on sensitivity and precision
ndash MicroMist (glass concentric type) is the standard nebulizer ndash handles most sample
types
ndash PFA MicroFlow nebulizer best for low volume samples aggressive samples (HF
digests) and when low contamination required (semi-con)
ndash Babington gives poorer precision - best for high TDS samples
bull Check nebulizer condition regularly
ndash Chips in the nebulizer tip impact on aerosol formation ndash poor precision
(use a magnifying glass if necessary)
ndash Check for deposits or blockage in the tip
bull Sample uptake or flow rate
ndash Lower pump speed or using narrow bore pump tubing will reduce uptake rate
- better for high TDS samples
25
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Sample Introduction bull Contamination in the spray chamber
ndash When was the spray chamber cleaned
bull Any blockages in the nebulizer injector
ndash Check for stable aerosol formation
bull Air leaks in spray chamber end cap or connecting tubes
ndash Are they in good condition with tight connections
bull Damaged pump tubes
ndash When did you check the pump tubes
bull Is the pump speed too slow
ndash Low pump speeds may cause signal pulsation
ndash If required use narrower bore pump tube and increase pump speed
bull Samples have a high TDS content
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
26
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Memory effects
bull If possible avoid running high concentrations of these analytes
(Ag Au B Hg Mo Si Sn W Zn Zr)
ndash Maybe necessary to pre-dilute samples (if known to be high in concentration)
bull Ensure an adequate rinse time
ndash Should be at least equal to the sample uptake delay
(30-40 seconds typical)
bull May require an acidified rinse solution between samples
(2 HNO3)
bull Other strategies to minimize memory effects
ndash Use an inert spray chamber
ndash Use the ISIS to introduce discrete amounts of sample This means
bull Cones are exposed to less sample matrix = improved stability
bull Less memorycarry-over
bull Reduced uptake amp rinse times = faster measurement
27
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy - Why is This Important
What does ldquoAccuracyrdquo mean
ndash Ability to get the ldquorightrdquo answer for the sample
ndash Heavily dependent on operatorrsquos skill
Why is this important
ndash User loses confidence in the system
ndash Your reputationhellip
bull Customerrsquos question the results
bull Poor performance in ldquoround robinrdquo comparisons
How do You Confirm Accuracy
ndash Check the result for a prepared standard
ndash Measure a certified reference material
ndash Use other quality control checks to check analysis
28
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Calibration standards properly prepared
bull See earlier recommendations ndash important to match to samples prepare
accurately and use them ldquofreshrdquo
ndash Any interferences impacting on results
ndash Use matched standards or standard additions
ndash Ensure isotope selected has no polyatomic interferences
ndash If necessary use ORS3
ndash Precision optimized
bull Optimum signal to noise performance improves accuracy
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
29
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Reprocess data post
run using an
alternate internal
standard
bull Ensure Internal
Standard used is
similar in mass
bull Check whether the
Internal Standard is
present in the
sample
ndash If necessary do a Semi-
Quant measurement
bull Dilute with cal blk
matrix
30
Accuracy ndash Suspect Internal Standard Recovery
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Sample preparation
bull Is the most appropriate digestion being used
bull Are all of the analytes being quantitatively (and reproducibly) extracted and
dissolved
ndash Many digestions are only partial extracts ndash efficiency will vary with the
sample matrix
ndash Some volatile analytes may be ldquolostrdquo during digestion
bull Confirm by taking a solid certified reference material
through your preparation and analysis procedure
bull Is the digest stable ndash or are you seeing any precipitates or a suspension
bull Do you see any potential contamination from either reagents or the digestion
equipment eg especially with Si B or Ca
bull Include a ldquoReagent Blankrdquo with every sample batch to
monitor
31
ICP-MS Maintenance amp Trouble Shooting
May 2012
Laboratory environment can have
direct impact on quality of results
bull Clean uncluttered work area
bull Proper ventilation
bull Safety considerations
bull Instrument lifetime consideration
ICP-MS Maintenance amp Trouble Shooting
May 2012 32
Laboratory Environment
ICP-MS ndash Potential Autosampler Issues
ndash More customers use autosamplers with ICP for automation
ndash Issues to consider
bull Long transfer tube between sampler and ICP-MS
ndash May need to program a longer sample uptake delay
ndash May exacerbate problems with memory effects
ndash Use ldquoFast Pumprdquo during sample uptake delay
bull Caution ndash not always possible
Not recommended with high TDS samples and organics
bull Ensure probe diameter is appropriate for sample matrix
ndash Use wider bore for high TDS or viscous samples
bull Sample stability - potential for sample changes while uncovered in racks ndash impacts accuracy
ndash Dust ingress can introduce contamination
ndash Sample evaporation may occur during long unattended runs
ndash Sediment in the sample may settle out esp with wear metals or suspensions
bull Ensure transfer line to ICP-MS is in good condition
ndash Kinks in the line may cause poor uptake or pulsing in the sample
ndash Impacts on precision and accuracy
33
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sample Throughput ndash What to Check
ndash Samples fully digested
bull No excess particulates in the sample that may cause blockage
ndash Sample Introduction System optimized
ndash Capable of handling the TDS levels in the sample
ndash TorchNebulizer cleaned and ready for analysis
ndash Method parameters optimized
bull Sample uptake delay and stabilization times are appropriate ndash optimized
bull Integration time is appropriate for the expected concentration
ndash Use a longer integration time at low concentrations
bull Rinse time is appropriate
bull Use ldquoISISrdquo discrete sampling for faster measurement and faster washout
34
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Handles tough sample matrices better
than any other ICP-MS
ndash Highest plasma temperature (lowest
CeOCe) as standard
ndash HMI (high matrix introduction) allows direct
analysis of difficult samples
eg sea water
bull ORS3 operates in He collision mode to
remove ALL polyatomic interferences
ndash Enables reliable removal of all polyatomic
interferences using a single set of
conditions
ndash Gives lower levels of interference and
better long-term stability HMI gives lower suppression and
better long-term stability
Relative signal (suppression) in undiluted seawater
Long-term stability in undiluted seawater
35
Agilent ICP-MS Performance - Benefits
Best matrix tolerance amp less interferences
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS ndash Recommended Maintenance Schedule
ICP-MS Maintenance amp Trouble Shooting
May 2012 37
These functions
(and more) are
completed as part
of a Preventative
Maintenance
program by an
Agilent Field
Service Engineer
Summary ndash Key Consumables for ICP-MS
Sample preparationpresentation
ndash Peristaltic pump tubing
ndash Transfer and drain tubing
ndash ICP-MS standard solutions
ndash Internal Standard solutions
ndash Torches
ndash Spray chambers
ndash Nebulizers
Ion Extraction
ndash Sampler and skimmer cones
Autosampling
ndash Sample tubes racks probes and transfer tubing
ISIS
ndash Peristaltic pump tubing ferrules amp fittings
38
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sample Introduction
Key consumables requiring frequent replacement
bull Pump tubing
bull Torches and quartz transfer tube
bull Nebulizers
bull Spray chambers
bull Interface cones (skimmer amp sampler)
bull Transfer amp connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalogue
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24406(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 39
Autosampler Supplies
Key consumables requiring frequent replacement
ndash Peristaltic pump tubing
ndash Sample racks
ndash Sample tubes
ndash Spare probes
ndash Standard racks
ndash Connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24407(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 40
ISIS Supplies
Key consumables requiring frequent replacement
bull Peristaltic pump tubing
bull Ferrules and fittings
bull Valving
For ISIS Hydride Generation Accessory
bull Membrane filter
bull Concentric nebulizer
bull Gas-liquid separator
bull Other tubing and connectors
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceProductListingaspxcat=SubCat2ECS_24437(Agilent)amppcat=SubCat1ECS_24407(Agilent)amprcat=ClassECS_22674(Agilent)
41
ICP-MS Maintenance amp Trouble Shooting
May 2012
Where to Find the Right Consumable Analytical Consumables Agilent Assist
Consumables amp Supplies Instrument Sales ampServices 1-800-227-9770 (Option 11) 1-800-227-9770 (Option 13) wwwagilentcomchemcontactus wwwagilentcomchemcontactus
On-Line resources
ICP-MS Supplies
2nd Edition Speciation Handbook
ICP-MS Journal Archives
Recorded Agilent e-Seminars
ICP-OES Supplies
Atomic Absorption Supplies
Instrument Parts amp Supplies
Atomic Spec Application Notes
Agilent Quick Reference Guide for 77008800 ICP-MS (pub 5990-8182EN)
Agilent Atomic Spec Supplies Catalogue (pub 5990-8767EN)
Agilent Consumables Catalogue (pub 5990-6674EN)
Instrument User Manuals
42
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sensitivity - Peristaltic Pump Tubing
bull Selection of tubing used for an application based on 2 key factors
ndash Resistance to the solvent in use
ndash ID of the tubing required (indicated by the coloured tabs)
bull Usersrsquo usually know what size they need
ndash Sample ndash 102 mm ID or whitewhite tabs
ndash Drain ndash 152 mm ID or yellowblue tabs
bull Smaller sizes used when application demands it
ndash Internal standard ndash 019 mm ID with orangered tabs
or 025 mm ID with orangeblue tabs
9
ICP-MS Maintenance amp Trouble Shooting
May 2012
Trim to 5-10mm to
reduce washout
and contamination
Potential Pump Tube Problems
10
ICP-MS Maintenance amp Trouble Shooting
May 2012
What to Check
ndash Tubing diameters
bull Want tubing used for waste to be larger ID than sample ID
ndash Chemical compatibility
bull Ensure tubing is resistant to the solvent being used
ndash Tube lifetime
bull Typical lifetime is ~1 week based on normal 8 hour working day
ndash Detach from tube holder after use ndash allows tube to ldquorelaxrdquo
bull Check 2 key things on pump tubing
ndash Roundness of tube ndash should not be any ldquoflatrdquo spots
ndash Tubing should still be elastic ndash replace if obviously stretched
bull Using ldquooldrdquo tubing can lead to problems with precision and stability
bull Installation and tensioning critical
ndash Donrsquot overtighten ndash just need smooth and even sample flow
ndash Remember to check other tubing for wear leaks and crimps
Normal wear amp tear
(~5 days) needs
replacing
ICP-MS Sensitivity ndash Method Parameters
What to Check
ndash Isotope selection
bull Using the most sensitive isotope
ndash Pump speed
bull Use the default speed as guide
bull Change pump tubing to give resistance to the solvent
ndash Interferences
bull Check for polyatomic interferences ndash try an alternate isotope first (if required)
ndash Otherwise use ORS3 to remove
bull Physical interferences can affect aerosol formation
ndash Use internal standard matched standards or standard additions
bull Chemical interferences can reduce atom formation and ionization
ndash Use higher RF power optimize neb flow + appropriate matrix modifiers
11
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sensitivity ndash Automated ldquoExpertrdquo Tuning
bull Startup provides a simple
user-configured schedule of
system optimization and
performance checks
bull One-click expert autotuning for
simple plasma optimization
bull Ensures consistent
performance from day to day
bull Independent of operator
experience
bull Automatically generate a
Performance Report
bull Provides a continuing record of
system performance
12
ICP-MS Maintenance amp Trouble Shooting
May 2012
13
Hardware Performance Report
is run under ldquostandardrdquo (factory
check-out) conditions
Gives record of performance
history under consistent default
tuning conditions
Note this is different to the ldquoTune
Reportrdquo which is generated
using Batch tune conditions
Sensitivity ndash Performance Report
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS specific contamination concerns -This is a topic of its own often leads to the clean room
conversation
But remember its not just where your instrument
is located ndash itrsquos everything the sample encounters
on its way to the instrument
ICP-MS Maintenance amp Trouble Shooting
May 2012 14
Sensitivity ndash Cleanliness amp Contamination
Sensitivity ndash Contamination Sources
bull Use high purity or ICP-MS grade reagents
bull Acid purity
ndash Buy only what you need to do the job
ndash Check the certificate of analysis
ndash Donrsquot insert pipette tips into your acids
ndash Use contaminated acid for cleaning
bull Sample containers
ndash Borosilicate glass introduces boron
ndash FEP containers preferred
bull Pipette tips
ndash Colors add interest ndash but increase contamination (Cu Fe Zn Cd)
bull Gloves
ndash Powder free unless you like Zn
Anything that touches sample during prep dilution
transfer analysis and storage
ICP-MS Maintenance amp Trouble Shooting
May 2012 15
PFA spray
chamber
PFA
endcap
PFA
nebulizer
PFA
connector
tube
Quartz torch with sapphire
or platinum injector
Complete sample introduction can be
changed to a system specifically
designed to reduce contamination
bull Usually used for semi-con applications
Clean integrated Auto-Sampler ndash I-AS
Clean sample introduction system - PFA
16
Cleanliness ndash The Ultimate for Contamination Free
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sensitivity ndash System Cleanliness
What to Check
ndash Sample Introduction System
bull Deposits in nebulizer can reduce
sample uptake rate
ndash Soak in aqua regia or use a nebulizer
cleaning tool to back flush
bull Solid material in torch injector
affects aerosol introduction into
plasma and increases noise
bull Contamination in spray chamber
impacts on aerosol formation ndash
increases noise
bull If seeing poor precision may be
due to beading in spray chamber
ndash Soak in 25 detergent solution
overnight (preferably for 24 hours)
17
ICP-MS Maintenance amp Trouble Shooting
May 2012
Nebulizer cleaner
Agilent PN G3266-80020
ICP-MS Sensitivity ndash System Cleanliness
What to Check
ndash Interface cones
bull Deposits or discoloration indicates
cleaning is required
bull Other indicators that cone cleaning
is required
ndash Poor sensitivity
ndash High background
ndash Distorted peak shapes
ndash Changes in interface vacuum reading
(deposition or build-up)
18
ICP-MS Maintenance amp Trouble Shooting
May 2012
Close up
Sample cone after measuring 75 undiluted sea water
samples using HMI Some deposition on outer edges
away from the orifice ndash no blockage of the sampling
orifice ndash but cleaning still recommended
System Cleanliness - Sampling Cone
1 mm Orifice Nickel or Platinum Centres
bull Nickel
bull Physically stronger
bull Tip runs hotter ndash less sample deposition
bull Platinum
bull Chemically stronger
bull Used for higher acid conc (incl HF)
bull 2 centre sizes 10-18 mm
bull Higher cost
Potential Problems
bull Biggest risk is physical damage to the orifice due to excessively aggressive cleaning
bull Cones also affected by sample matrix (acid strength amp type) and number of samples analyzed each day
bull Nickel - Typically replace 3 or 5 each year (assumes measuring 250-350 environmental samples each day)
bull Platinum - Typically replace 1 or 2 each year (assumes measuring 20-50 semiconductor samples each day)
bull If not clean then can result in analytical problems eg poor signal stability elemental contamination
ICP-MS Maintenance amp Trouble Shooting
May 2012 19
System Cleanliness - Skimmer Cone
04 mm Orifice Nickel or Platinum
bull The Nickel skimmer cone is the standard interface
bull The skimmer cone is relatively robust to samples containing high concentrations of matrix and salts and is suitable for a wide variety of samples It is usually used with the Nickel sampling cone
bull The Platinum skimmer cone is usually used for introduction of hydrofluoric acid and other reagents It is usually used with the Platinum sampling cone
Potential Problems
bull Biggest risk is from physical damage to the orifice due to excessively aggressive cleaning
bull Cones also affected by sample matrix (acid strength amp type) and number of samples analyzed each day
bull Nickel ndash Typically replace 3 or 5 each year (assumes measuring 250-350 environmental samples each day)
bull Platinum ndash Typically replace 1 or 2 each year (assumes measuring 20-50 semiconductor samples each day)
bull If not clean then can result in analytical problems eg poor signal stability elemental contamination
20
ICP-MS Maintenance amp Trouble Shooting
May 2012
System Cleanliness - Cone Cleaning Procedure
Caution - Take care to avoid damage to the cone tip when removing ndash and place base down - Check the graphite gasket and replace if creased or damaged - Sonicate in a 2 Citranox or 2 Nitric Acid solution for a few minutes - Rinse well with de-ionized water - If still dirty or memory problems remain polish using an alumina powder slurry on a Q-tip then sonicate in 2 Citranox solution and rinse well with de-ionized water - Dry with nitrogen before installing
22
ICP-MS Maintenance amp Trouble Shooting
May 2012
Precision - Why is This Important
What does ldquoPrecisionrdquo mean
ndash Ability to get the same result for the same
sample when measured multiple times
ndash Usually measured as RSD or sometimes SD
RSD = (SD Mean Result) 100
ndash Low values indicate good precision
bull For ICP-MS expect 1-2 RSD
Why is this important
ndash User loses confidence in the system
What impacts on precision
ndash Nebulizerplasma stability
ndash Sample introduction system
ndash Method parameters
23
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash System stabilized
bull Allow 10 mins for plasma warm-up before
analysis
ndash Plasma status
bull ldquoBulletrdquo in the plasma should be stable
bull Check for deposits in the injector of the torch
ndash Check condition of interface cones and
clean if necessary
ndash Clean the Extraction Lens - Omega Lens
assembly
ndash Method parameters
bull Appropriate times set for sample uptake
delay and stabilization times
24
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash Sample Intro
What to Check ndash Nebulizer
bull Nebulizer type used can impact on sensitivity and precision
ndash MicroMist (glass concentric type) is the standard nebulizer ndash handles most sample
types
ndash PFA MicroFlow nebulizer best for low volume samples aggressive samples (HF
digests) and when low contamination required (semi-con)
ndash Babington gives poorer precision - best for high TDS samples
bull Check nebulizer condition regularly
ndash Chips in the nebulizer tip impact on aerosol formation ndash poor precision
(use a magnifying glass if necessary)
ndash Check for deposits or blockage in the tip
bull Sample uptake or flow rate
ndash Lower pump speed or using narrow bore pump tubing will reduce uptake rate
- better for high TDS samples
25
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Sample Introduction bull Contamination in the spray chamber
ndash When was the spray chamber cleaned
bull Any blockages in the nebulizer injector
ndash Check for stable aerosol formation
bull Air leaks in spray chamber end cap or connecting tubes
ndash Are they in good condition with tight connections
bull Damaged pump tubes
ndash When did you check the pump tubes
bull Is the pump speed too slow
ndash Low pump speeds may cause signal pulsation
ndash If required use narrower bore pump tube and increase pump speed
bull Samples have a high TDS content
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
26
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Memory effects
bull If possible avoid running high concentrations of these analytes
(Ag Au B Hg Mo Si Sn W Zn Zr)
ndash Maybe necessary to pre-dilute samples (if known to be high in concentration)
bull Ensure an adequate rinse time
ndash Should be at least equal to the sample uptake delay
(30-40 seconds typical)
bull May require an acidified rinse solution between samples
(2 HNO3)
bull Other strategies to minimize memory effects
ndash Use an inert spray chamber
ndash Use the ISIS to introduce discrete amounts of sample This means
bull Cones are exposed to less sample matrix = improved stability
bull Less memorycarry-over
bull Reduced uptake amp rinse times = faster measurement
27
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy - Why is This Important
What does ldquoAccuracyrdquo mean
ndash Ability to get the ldquorightrdquo answer for the sample
ndash Heavily dependent on operatorrsquos skill
Why is this important
ndash User loses confidence in the system
ndash Your reputationhellip
bull Customerrsquos question the results
bull Poor performance in ldquoround robinrdquo comparisons
How do You Confirm Accuracy
ndash Check the result for a prepared standard
ndash Measure a certified reference material
ndash Use other quality control checks to check analysis
28
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Calibration standards properly prepared
bull See earlier recommendations ndash important to match to samples prepare
accurately and use them ldquofreshrdquo
ndash Any interferences impacting on results
ndash Use matched standards or standard additions
ndash Ensure isotope selected has no polyatomic interferences
ndash If necessary use ORS3
ndash Precision optimized
bull Optimum signal to noise performance improves accuracy
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
29
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Reprocess data post
run using an
alternate internal
standard
bull Ensure Internal
Standard used is
similar in mass
bull Check whether the
Internal Standard is
present in the
sample
ndash If necessary do a Semi-
Quant measurement
bull Dilute with cal blk
matrix
30
Accuracy ndash Suspect Internal Standard Recovery
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Sample preparation
bull Is the most appropriate digestion being used
bull Are all of the analytes being quantitatively (and reproducibly) extracted and
dissolved
ndash Many digestions are only partial extracts ndash efficiency will vary with the
sample matrix
ndash Some volatile analytes may be ldquolostrdquo during digestion
bull Confirm by taking a solid certified reference material
through your preparation and analysis procedure
bull Is the digest stable ndash or are you seeing any precipitates or a suspension
bull Do you see any potential contamination from either reagents or the digestion
equipment eg especially with Si B or Ca
bull Include a ldquoReagent Blankrdquo with every sample batch to
monitor
31
ICP-MS Maintenance amp Trouble Shooting
May 2012
Laboratory environment can have
direct impact on quality of results
bull Clean uncluttered work area
bull Proper ventilation
bull Safety considerations
bull Instrument lifetime consideration
ICP-MS Maintenance amp Trouble Shooting
May 2012 32
Laboratory Environment
ICP-MS ndash Potential Autosampler Issues
ndash More customers use autosamplers with ICP for automation
ndash Issues to consider
bull Long transfer tube between sampler and ICP-MS
ndash May need to program a longer sample uptake delay
ndash May exacerbate problems with memory effects
ndash Use ldquoFast Pumprdquo during sample uptake delay
bull Caution ndash not always possible
Not recommended with high TDS samples and organics
bull Ensure probe diameter is appropriate for sample matrix
ndash Use wider bore for high TDS or viscous samples
bull Sample stability - potential for sample changes while uncovered in racks ndash impacts accuracy
ndash Dust ingress can introduce contamination
ndash Sample evaporation may occur during long unattended runs
ndash Sediment in the sample may settle out esp with wear metals or suspensions
bull Ensure transfer line to ICP-MS is in good condition
ndash Kinks in the line may cause poor uptake or pulsing in the sample
ndash Impacts on precision and accuracy
33
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sample Throughput ndash What to Check
ndash Samples fully digested
bull No excess particulates in the sample that may cause blockage
ndash Sample Introduction System optimized
ndash Capable of handling the TDS levels in the sample
ndash TorchNebulizer cleaned and ready for analysis
ndash Method parameters optimized
bull Sample uptake delay and stabilization times are appropriate ndash optimized
bull Integration time is appropriate for the expected concentration
ndash Use a longer integration time at low concentrations
bull Rinse time is appropriate
bull Use ldquoISISrdquo discrete sampling for faster measurement and faster washout
34
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Handles tough sample matrices better
than any other ICP-MS
ndash Highest plasma temperature (lowest
CeOCe) as standard
ndash HMI (high matrix introduction) allows direct
analysis of difficult samples
eg sea water
bull ORS3 operates in He collision mode to
remove ALL polyatomic interferences
ndash Enables reliable removal of all polyatomic
interferences using a single set of
conditions
ndash Gives lower levels of interference and
better long-term stability HMI gives lower suppression and
better long-term stability
Relative signal (suppression) in undiluted seawater
Long-term stability in undiluted seawater
35
Agilent ICP-MS Performance - Benefits
Best matrix tolerance amp less interferences
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS ndash Recommended Maintenance Schedule
ICP-MS Maintenance amp Trouble Shooting
May 2012 37
These functions
(and more) are
completed as part
of a Preventative
Maintenance
program by an
Agilent Field
Service Engineer
Summary ndash Key Consumables for ICP-MS
Sample preparationpresentation
ndash Peristaltic pump tubing
ndash Transfer and drain tubing
ndash ICP-MS standard solutions
ndash Internal Standard solutions
ndash Torches
ndash Spray chambers
ndash Nebulizers
Ion Extraction
ndash Sampler and skimmer cones
Autosampling
ndash Sample tubes racks probes and transfer tubing
ISIS
ndash Peristaltic pump tubing ferrules amp fittings
38
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sample Introduction
Key consumables requiring frequent replacement
bull Pump tubing
bull Torches and quartz transfer tube
bull Nebulizers
bull Spray chambers
bull Interface cones (skimmer amp sampler)
bull Transfer amp connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalogue
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24406(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 39
Autosampler Supplies
Key consumables requiring frequent replacement
ndash Peristaltic pump tubing
ndash Sample racks
ndash Sample tubes
ndash Spare probes
ndash Standard racks
ndash Connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24407(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 40
ISIS Supplies
Key consumables requiring frequent replacement
bull Peristaltic pump tubing
bull Ferrules and fittings
bull Valving
For ISIS Hydride Generation Accessory
bull Membrane filter
bull Concentric nebulizer
bull Gas-liquid separator
bull Other tubing and connectors
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceProductListingaspxcat=SubCat2ECS_24437(Agilent)amppcat=SubCat1ECS_24407(Agilent)amprcat=ClassECS_22674(Agilent)
41
ICP-MS Maintenance amp Trouble Shooting
May 2012
Where to Find the Right Consumable Analytical Consumables Agilent Assist
Consumables amp Supplies Instrument Sales ampServices 1-800-227-9770 (Option 11) 1-800-227-9770 (Option 13) wwwagilentcomchemcontactus wwwagilentcomchemcontactus
On-Line resources
ICP-MS Supplies
2nd Edition Speciation Handbook
ICP-MS Journal Archives
Recorded Agilent e-Seminars
ICP-OES Supplies
Atomic Absorption Supplies
Instrument Parts amp Supplies
Atomic Spec Application Notes
Agilent Quick Reference Guide for 77008800 ICP-MS (pub 5990-8182EN)
Agilent Atomic Spec Supplies Catalogue (pub 5990-8767EN)
Agilent Consumables Catalogue (pub 5990-6674EN)
Instrument User Manuals
42
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
Potential Pump Tube Problems
10
ICP-MS Maintenance amp Trouble Shooting
May 2012
What to Check
ndash Tubing diameters
bull Want tubing used for waste to be larger ID than sample ID
ndash Chemical compatibility
bull Ensure tubing is resistant to the solvent being used
ndash Tube lifetime
bull Typical lifetime is ~1 week based on normal 8 hour working day
ndash Detach from tube holder after use ndash allows tube to ldquorelaxrdquo
bull Check 2 key things on pump tubing
ndash Roundness of tube ndash should not be any ldquoflatrdquo spots
ndash Tubing should still be elastic ndash replace if obviously stretched
bull Using ldquooldrdquo tubing can lead to problems with precision and stability
bull Installation and tensioning critical
ndash Donrsquot overtighten ndash just need smooth and even sample flow
ndash Remember to check other tubing for wear leaks and crimps
Normal wear amp tear
(~5 days) needs
replacing
ICP-MS Sensitivity ndash Method Parameters
What to Check
ndash Isotope selection
bull Using the most sensitive isotope
ndash Pump speed
bull Use the default speed as guide
bull Change pump tubing to give resistance to the solvent
ndash Interferences
bull Check for polyatomic interferences ndash try an alternate isotope first (if required)
ndash Otherwise use ORS3 to remove
bull Physical interferences can affect aerosol formation
ndash Use internal standard matched standards or standard additions
bull Chemical interferences can reduce atom formation and ionization
ndash Use higher RF power optimize neb flow + appropriate matrix modifiers
11
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sensitivity ndash Automated ldquoExpertrdquo Tuning
bull Startup provides a simple
user-configured schedule of
system optimization and
performance checks
bull One-click expert autotuning for
simple plasma optimization
bull Ensures consistent
performance from day to day
bull Independent of operator
experience
bull Automatically generate a
Performance Report
bull Provides a continuing record of
system performance
12
ICP-MS Maintenance amp Trouble Shooting
May 2012
13
Hardware Performance Report
is run under ldquostandardrdquo (factory
check-out) conditions
Gives record of performance
history under consistent default
tuning conditions
Note this is different to the ldquoTune
Reportrdquo which is generated
using Batch tune conditions
Sensitivity ndash Performance Report
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS specific contamination concerns -This is a topic of its own often leads to the clean room
conversation
But remember its not just where your instrument
is located ndash itrsquos everything the sample encounters
on its way to the instrument
ICP-MS Maintenance amp Trouble Shooting
May 2012 14
Sensitivity ndash Cleanliness amp Contamination
Sensitivity ndash Contamination Sources
bull Use high purity or ICP-MS grade reagents
bull Acid purity
ndash Buy only what you need to do the job
ndash Check the certificate of analysis
ndash Donrsquot insert pipette tips into your acids
ndash Use contaminated acid for cleaning
bull Sample containers
ndash Borosilicate glass introduces boron
ndash FEP containers preferred
bull Pipette tips
ndash Colors add interest ndash but increase contamination (Cu Fe Zn Cd)
bull Gloves
ndash Powder free unless you like Zn
Anything that touches sample during prep dilution
transfer analysis and storage
ICP-MS Maintenance amp Trouble Shooting
May 2012 15
PFA spray
chamber
PFA
endcap
PFA
nebulizer
PFA
connector
tube
Quartz torch with sapphire
or platinum injector
Complete sample introduction can be
changed to a system specifically
designed to reduce contamination
bull Usually used for semi-con applications
Clean integrated Auto-Sampler ndash I-AS
Clean sample introduction system - PFA
16
Cleanliness ndash The Ultimate for Contamination Free
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sensitivity ndash System Cleanliness
What to Check
ndash Sample Introduction System
bull Deposits in nebulizer can reduce
sample uptake rate
ndash Soak in aqua regia or use a nebulizer
cleaning tool to back flush
bull Solid material in torch injector
affects aerosol introduction into
plasma and increases noise
bull Contamination in spray chamber
impacts on aerosol formation ndash
increases noise
bull If seeing poor precision may be
due to beading in spray chamber
ndash Soak in 25 detergent solution
overnight (preferably for 24 hours)
17
ICP-MS Maintenance amp Trouble Shooting
May 2012
Nebulizer cleaner
Agilent PN G3266-80020
ICP-MS Sensitivity ndash System Cleanliness
What to Check
ndash Interface cones
bull Deposits or discoloration indicates
cleaning is required
bull Other indicators that cone cleaning
is required
ndash Poor sensitivity
ndash High background
ndash Distorted peak shapes
ndash Changes in interface vacuum reading
(deposition or build-up)
18
ICP-MS Maintenance amp Trouble Shooting
May 2012
Close up
Sample cone after measuring 75 undiluted sea water
samples using HMI Some deposition on outer edges
away from the orifice ndash no blockage of the sampling
orifice ndash but cleaning still recommended
System Cleanliness - Sampling Cone
1 mm Orifice Nickel or Platinum Centres
bull Nickel
bull Physically stronger
bull Tip runs hotter ndash less sample deposition
bull Platinum
bull Chemically stronger
bull Used for higher acid conc (incl HF)
bull 2 centre sizes 10-18 mm
bull Higher cost
Potential Problems
bull Biggest risk is physical damage to the orifice due to excessively aggressive cleaning
bull Cones also affected by sample matrix (acid strength amp type) and number of samples analyzed each day
bull Nickel - Typically replace 3 or 5 each year (assumes measuring 250-350 environmental samples each day)
bull Platinum - Typically replace 1 or 2 each year (assumes measuring 20-50 semiconductor samples each day)
bull If not clean then can result in analytical problems eg poor signal stability elemental contamination
ICP-MS Maintenance amp Trouble Shooting
May 2012 19
System Cleanliness - Skimmer Cone
04 mm Orifice Nickel or Platinum
bull The Nickel skimmer cone is the standard interface
bull The skimmer cone is relatively robust to samples containing high concentrations of matrix and salts and is suitable for a wide variety of samples It is usually used with the Nickel sampling cone
bull The Platinum skimmer cone is usually used for introduction of hydrofluoric acid and other reagents It is usually used with the Platinum sampling cone
Potential Problems
bull Biggest risk is from physical damage to the orifice due to excessively aggressive cleaning
bull Cones also affected by sample matrix (acid strength amp type) and number of samples analyzed each day
bull Nickel ndash Typically replace 3 or 5 each year (assumes measuring 250-350 environmental samples each day)
bull Platinum ndash Typically replace 1 or 2 each year (assumes measuring 20-50 semiconductor samples each day)
bull If not clean then can result in analytical problems eg poor signal stability elemental contamination
20
ICP-MS Maintenance amp Trouble Shooting
May 2012
System Cleanliness - Cone Cleaning Procedure
Caution - Take care to avoid damage to the cone tip when removing ndash and place base down - Check the graphite gasket and replace if creased or damaged - Sonicate in a 2 Citranox or 2 Nitric Acid solution for a few minutes - Rinse well with de-ionized water - If still dirty or memory problems remain polish using an alumina powder slurry on a Q-tip then sonicate in 2 Citranox solution and rinse well with de-ionized water - Dry with nitrogen before installing
22
ICP-MS Maintenance amp Trouble Shooting
May 2012
Precision - Why is This Important
What does ldquoPrecisionrdquo mean
ndash Ability to get the same result for the same
sample when measured multiple times
ndash Usually measured as RSD or sometimes SD
RSD = (SD Mean Result) 100
ndash Low values indicate good precision
bull For ICP-MS expect 1-2 RSD
Why is this important
ndash User loses confidence in the system
What impacts on precision
ndash Nebulizerplasma stability
ndash Sample introduction system
ndash Method parameters
23
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash System stabilized
bull Allow 10 mins for plasma warm-up before
analysis
ndash Plasma status
bull ldquoBulletrdquo in the plasma should be stable
bull Check for deposits in the injector of the torch
ndash Check condition of interface cones and
clean if necessary
ndash Clean the Extraction Lens - Omega Lens
assembly
ndash Method parameters
bull Appropriate times set for sample uptake
delay and stabilization times
24
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash Sample Intro
What to Check ndash Nebulizer
bull Nebulizer type used can impact on sensitivity and precision
ndash MicroMist (glass concentric type) is the standard nebulizer ndash handles most sample
types
ndash PFA MicroFlow nebulizer best for low volume samples aggressive samples (HF
digests) and when low contamination required (semi-con)
ndash Babington gives poorer precision - best for high TDS samples
bull Check nebulizer condition regularly
ndash Chips in the nebulizer tip impact on aerosol formation ndash poor precision
(use a magnifying glass if necessary)
ndash Check for deposits or blockage in the tip
bull Sample uptake or flow rate
ndash Lower pump speed or using narrow bore pump tubing will reduce uptake rate
- better for high TDS samples
25
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Sample Introduction bull Contamination in the spray chamber
ndash When was the spray chamber cleaned
bull Any blockages in the nebulizer injector
ndash Check for stable aerosol formation
bull Air leaks in spray chamber end cap or connecting tubes
ndash Are they in good condition with tight connections
bull Damaged pump tubes
ndash When did you check the pump tubes
bull Is the pump speed too slow
ndash Low pump speeds may cause signal pulsation
ndash If required use narrower bore pump tube and increase pump speed
bull Samples have a high TDS content
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
26
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Memory effects
bull If possible avoid running high concentrations of these analytes
(Ag Au B Hg Mo Si Sn W Zn Zr)
ndash Maybe necessary to pre-dilute samples (if known to be high in concentration)
bull Ensure an adequate rinse time
ndash Should be at least equal to the sample uptake delay
(30-40 seconds typical)
bull May require an acidified rinse solution between samples
(2 HNO3)
bull Other strategies to minimize memory effects
ndash Use an inert spray chamber
ndash Use the ISIS to introduce discrete amounts of sample This means
bull Cones are exposed to less sample matrix = improved stability
bull Less memorycarry-over
bull Reduced uptake amp rinse times = faster measurement
27
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy - Why is This Important
What does ldquoAccuracyrdquo mean
ndash Ability to get the ldquorightrdquo answer for the sample
ndash Heavily dependent on operatorrsquos skill
Why is this important
ndash User loses confidence in the system
ndash Your reputationhellip
bull Customerrsquos question the results
bull Poor performance in ldquoround robinrdquo comparisons
How do You Confirm Accuracy
ndash Check the result for a prepared standard
ndash Measure a certified reference material
ndash Use other quality control checks to check analysis
28
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Calibration standards properly prepared
bull See earlier recommendations ndash important to match to samples prepare
accurately and use them ldquofreshrdquo
ndash Any interferences impacting on results
ndash Use matched standards or standard additions
ndash Ensure isotope selected has no polyatomic interferences
ndash If necessary use ORS3
ndash Precision optimized
bull Optimum signal to noise performance improves accuracy
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
29
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Reprocess data post
run using an
alternate internal
standard
bull Ensure Internal
Standard used is
similar in mass
bull Check whether the
Internal Standard is
present in the
sample
ndash If necessary do a Semi-
Quant measurement
bull Dilute with cal blk
matrix
30
Accuracy ndash Suspect Internal Standard Recovery
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Sample preparation
bull Is the most appropriate digestion being used
bull Are all of the analytes being quantitatively (and reproducibly) extracted and
dissolved
ndash Many digestions are only partial extracts ndash efficiency will vary with the
sample matrix
ndash Some volatile analytes may be ldquolostrdquo during digestion
bull Confirm by taking a solid certified reference material
through your preparation and analysis procedure
bull Is the digest stable ndash or are you seeing any precipitates or a suspension
bull Do you see any potential contamination from either reagents or the digestion
equipment eg especially with Si B or Ca
bull Include a ldquoReagent Blankrdquo with every sample batch to
monitor
31
ICP-MS Maintenance amp Trouble Shooting
May 2012
Laboratory environment can have
direct impact on quality of results
bull Clean uncluttered work area
bull Proper ventilation
bull Safety considerations
bull Instrument lifetime consideration
ICP-MS Maintenance amp Trouble Shooting
May 2012 32
Laboratory Environment
ICP-MS ndash Potential Autosampler Issues
ndash More customers use autosamplers with ICP for automation
ndash Issues to consider
bull Long transfer tube between sampler and ICP-MS
ndash May need to program a longer sample uptake delay
ndash May exacerbate problems with memory effects
ndash Use ldquoFast Pumprdquo during sample uptake delay
bull Caution ndash not always possible
Not recommended with high TDS samples and organics
bull Ensure probe diameter is appropriate for sample matrix
ndash Use wider bore for high TDS or viscous samples
bull Sample stability - potential for sample changes while uncovered in racks ndash impacts accuracy
ndash Dust ingress can introduce contamination
ndash Sample evaporation may occur during long unattended runs
ndash Sediment in the sample may settle out esp with wear metals or suspensions
bull Ensure transfer line to ICP-MS is in good condition
ndash Kinks in the line may cause poor uptake or pulsing in the sample
ndash Impacts on precision and accuracy
33
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sample Throughput ndash What to Check
ndash Samples fully digested
bull No excess particulates in the sample that may cause blockage
ndash Sample Introduction System optimized
ndash Capable of handling the TDS levels in the sample
ndash TorchNebulizer cleaned and ready for analysis
ndash Method parameters optimized
bull Sample uptake delay and stabilization times are appropriate ndash optimized
bull Integration time is appropriate for the expected concentration
ndash Use a longer integration time at low concentrations
bull Rinse time is appropriate
bull Use ldquoISISrdquo discrete sampling for faster measurement and faster washout
34
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Handles tough sample matrices better
than any other ICP-MS
ndash Highest plasma temperature (lowest
CeOCe) as standard
ndash HMI (high matrix introduction) allows direct
analysis of difficult samples
eg sea water
bull ORS3 operates in He collision mode to
remove ALL polyatomic interferences
ndash Enables reliable removal of all polyatomic
interferences using a single set of
conditions
ndash Gives lower levels of interference and
better long-term stability HMI gives lower suppression and
better long-term stability
Relative signal (suppression) in undiluted seawater
Long-term stability in undiluted seawater
35
Agilent ICP-MS Performance - Benefits
Best matrix tolerance amp less interferences
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS ndash Recommended Maintenance Schedule
ICP-MS Maintenance amp Trouble Shooting
May 2012 37
These functions
(and more) are
completed as part
of a Preventative
Maintenance
program by an
Agilent Field
Service Engineer
Summary ndash Key Consumables for ICP-MS
Sample preparationpresentation
ndash Peristaltic pump tubing
ndash Transfer and drain tubing
ndash ICP-MS standard solutions
ndash Internal Standard solutions
ndash Torches
ndash Spray chambers
ndash Nebulizers
Ion Extraction
ndash Sampler and skimmer cones
Autosampling
ndash Sample tubes racks probes and transfer tubing
ISIS
ndash Peristaltic pump tubing ferrules amp fittings
38
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sample Introduction
Key consumables requiring frequent replacement
bull Pump tubing
bull Torches and quartz transfer tube
bull Nebulizers
bull Spray chambers
bull Interface cones (skimmer amp sampler)
bull Transfer amp connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalogue
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24406(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 39
Autosampler Supplies
Key consumables requiring frequent replacement
ndash Peristaltic pump tubing
ndash Sample racks
ndash Sample tubes
ndash Spare probes
ndash Standard racks
ndash Connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24407(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 40
ISIS Supplies
Key consumables requiring frequent replacement
bull Peristaltic pump tubing
bull Ferrules and fittings
bull Valving
For ISIS Hydride Generation Accessory
bull Membrane filter
bull Concentric nebulizer
bull Gas-liquid separator
bull Other tubing and connectors
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceProductListingaspxcat=SubCat2ECS_24437(Agilent)amppcat=SubCat1ECS_24407(Agilent)amprcat=ClassECS_22674(Agilent)
41
ICP-MS Maintenance amp Trouble Shooting
May 2012
Where to Find the Right Consumable Analytical Consumables Agilent Assist
Consumables amp Supplies Instrument Sales ampServices 1-800-227-9770 (Option 11) 1-800-227-9770 (Option 13) wwwagilentcomchemcontactus wwwagilentcomchemcontactus
On-Line resources
ICP-MS Supplies
2nd Edition Speciation Handbook
ICP-MS Journal Archives
Recorded Agilent e-Seminars
ICP-OES Supplies
Atomic Absorption Supplies
Instrument Parts amp Supplies
Atomic Spec Application Notes
Agilent Quick Reference Guide for 77008800 ICP-MS (pub 5990-8182EN)
Agilent Atomic Spec Supplies Catalogue (pub 5990-8767EN)
Agilent Consumables Catalogue (pub 5990-6674EN)
Instrument User Manuals
42
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sensitivity ndash Method Parameters
What to Check
ndash Isotope selection
bull Using the most sensitive isotope
ndash Pump speed
bull Use the default speed as guide
bull Change pump tubing to give resistance to the solvent
ndash Interferences
bull Check for polyatomic interferences ndash try an alternate isotope first (if required)
ndash Otherwise use ORS3 to remove
bull Physical interferences can affect aerosol formation
ndash Use internal standard matched standards or standard additions
bull Chemical interferences can reduce atom formation and ionization
ndash Use higher RF power optimize neb flow + appropriate matrix modifiers
11
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sensitivity ndash Automated ldquoExpertrdquo Tuning
bull Startup provides a simple
user-configured schedule of
system optimization and
performance checks
bull One-click expert autotuning for
simple plasma optimization
bull Ensures consistent
performance from day to day
bull Independent of operator
experience
bull Automatically generate a
Performance Report
bull Provides a continuing record of
system performance
12
ICP-MS Maintenance amp Trouble Shooting
May 2012
13
Hardware Performance Report
is run under ldquostandardrdquo (factory
check-out) conditions
Gives record of performance
history under consistent default
tuning conditions
Note this is different to the ldquoTune
Reportrdquo which is generated
using Batch tune conditions
Sensitivity ndash Performance Report
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS specific contamination concerns -This is a topic of its own often leads to the clean room
conversation
But remember its not just where your instrument
is located ndash itrsquos everything the sample encounters
on its way to the instrument
ICP-MS Maintenance amp Trouble Shooting
May 2012 14
Sensitivity ndash Cleanliness amp Contamination
Sensitivity ndash Contamination Sources
bull Use high purity or ICP-MS grade reagents
bull Acid purity
ndash Buy only what you need to do the job
ndash Check the certificate of analysis
ndash Donrsquot insert pipette tips into your acids
ndash Use contaminated acid for cleaning
bull Sample containers
ndash Borosilicate glass introduces boron
ndash FEP containers preferred
bull Pipette tips
ndash Colors add interest ndash but increase contamination (Cu Fe Zn Cd)
bull Gloves
ndash Powder free unless you like Zn
Anything that touches sample during prep dilution
transfer analysis and storage
ICP-MS Maintenance amp Trouble Shooting
May 2012 15
PFA spray
chamber
PFA
endcap
PFA
nebulizer
PFA
connector
tube
Quartz torch with sapphire
or platinum injector
Complete sample introduction can be
changed to a system specifically
designed to reduce contamination
bull Usually used for semi-con applications
Clean integrated Auto-Sampler ndash I-AS
Clean sample introduction system - PFA
16
Cleanliness ndash The Ultimate for Contamination Free
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sensitivity ndash System Cleanliness
What to Check
ndash Sample Introduction System
bull Deposits in nebulizer can reduce
sample uptake rate
ndash Soak in aqua regia or use a nebulizer
cleaning tool to back flush
bull Solid material in torch injector
affects aerosol introduction into
plasma and increases noise
bull Contamination in spray chamber
impacts on aerosol formation ndash
increases noise
bull If seeing poor precision may be
due to beading in spray chamber
ndash Soak in 25 detergent solution
overnight (preferably for 24 hours)
17
ICP-MS Maintenance amp Trouble Shooting
May 2012
Nebulizer cleaner
Agilent PN G3266-80020
ICP-MS Sensitivity ndash System Cleanliness
What to Check
ndash Interface cones
bull Deposits or discoloration indicates
cleaning is required
bull Other indicators that cone cleaning
is required
ndash Poor sensitivity
ndash High background
ndash Distorted peak shapes
ndash Changes in interface vacuum reading
(deposition or build-up)
18
ICP-MS Maintenance amp Trouble Shooting
May 2012
Close up
Sample cone after measuring 75 undiluted sea water
samples using HMI Some deposition on outer edges
away from the orifice ndash no blockage of the sampling
orifice ndash but cleaning still recommended
System Cleanliness - Sampling Cone
1 mm Orifice Nickel or Platinum Centres
bull Nickel
bull Physically stronger
bull Tip runs hotter ndash less sample deposition
bull Platinum
bull Chemically stronger
bull Used for higher acid conc (incl HF)
bull 2 centre sizes 10-18 mm
bull Higher cost
Potential Problems
bull Biggest risk is physical damage to the orifice due to excessively aggressive cleaning
bull Cones also affected by sample matrix (acid strength amp type) and number of samples analyzed each day
bull Nickel - Typically replace 3 or 5 each year (assumes measuring 250-350 environmental samples each day)
bull Platinum - Typically replace 1 or 2 each year (assumes measuring 20-50 semiconductor samples each day)
bull If not clean then can result in analytical problems eg poor signal stability elemental contamination
ICP-MS Maintenance amp Trouble Shooting
May 2012 19
System Cleanliness - Skimmer Cone
04 mm Orifice Nickel or Platinum
bull The Nickel skimmer cone is the standard interface
bull The skimmer cone is relatively robust to samples containing high concentrations of matrix and salts and is suitable for a wide variety of samples It is usually used with the Nickel sampling cone
bull The Platinum skimmer cone is usually used for introduction of hydrofluoric acid and other reagents It is usually used with the Platinum sampling cone
Potential Problems
bull Biggest risk is from physical damage to the orifice due to excessively aggressive cleaning
bull Cones also affected by sample matrix (acid strength amp type) and number of samples analyzed each day
bull Nickel ndash Typically replace 3 or 5 each year (assumes measuring 250-350 environmental samples each day)
bull Platinum ndash Typically replace 1 or 2 each year (assumes measuring 20-50 semiconductor samples each day)
bull If not clean then can result in analytical problems eg poor signal stability elemental contamination
20
ICP-MS Maintenance amp Trouble Shooting
May 2012
System Cleanliness - Cone Cleaning Procedure
Caution - Take care to avoid damage to the cone tip when removing ndash and place base down - Check the graphite gasket and replace if creased or damaged - Sonicate in a 2 Citranox or 2 Nitric Acid solution for a few minutes - Rinse well with de-ionized water - If still dirty or memory problems remain polish using an alumina powder slurry on a Q-tip then sonicate in 2 Citranox solution and rinse well with de-ionized water - Dry with nitrogen before installing
22
ICP-MS Maintenance amp Trouble Shooting
May 2012
Precision - Why is This Important
What does ldquoPrecisionrdquo mean
ndash Ability to get the same result for the same
sample when measured multiple times
ndash Usually measured as RSD or sometimes SD
RSD = (SD Mean Result) 100
ndash Low values indicate good precision
bull For ICP-MS expect 1-2 RSD
Why is this important
ndash User loses confidence in the system
What impacts on precision
ndash Nebulizerplasma stability
ndash Sample introduction system
ndash Method parameters
23
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash System stabilized
bull Allow 10 mins for plasma warm-up before
analysis
ndash Plasma status
bull ldquoBulletrdquo in the plasma should be stable
bull Check for deposits in the injector of the torch
ndash Check condition of interface cones and
clean if necessary
ndash Clean the Extraction Lens - Omega Lens
assembly
ndash Method parameters
bull Appropriate times set for sample uptake
delay and stabilization times
24
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash Sample Intro
What to Check ndash Nebulizer
bull Nebulizer type used can impact on sensitivity and precision
ndash MicroMist (glass concentric type) is the standard nebulizer ndash handles most sample
types
ndash PFA MicroFlow nebulizer best for low volume samples aggressive samples (HF
digests) and when low contamination required (semi-con)
ndash Babington gives poorer precision - best for high TDS samples
bull Check nebulizer condition regularly
ndash Chips in the nebulizer tip impact on aerosol formation ndash poor precision
(use a magnifying glass if necessary)
ndash Check for deposits or blockage in the tip
bull Sample uptake or flow rate
ndash Lower pump speed or using narrow bore pump tubing will reduce uptake rate
- better for high TDS samples
25
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Sample Introduction bull Contamination in the spray chamber
ndash When was the spray chamber cleaned
bull Any blockages in the nebulizer injector
ndash Check for stable aerosol formation
bull Air leaks in spray chamber end cap or connecting tubes
ndash Are they in good condition with tight connections
bull Damaged pump tubes
ndash When did you check the pump tubes
bull Is the pump speed too slow
ndash Low pump speeds may cause signal pulsation
ndash If required use narrower bore pump tube and increase pump speed
bull Samples have a high TDS content
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
26
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Memory effects
bull If possible avoid running high concentrations of these analytes
(Ag Au B Hg Mo Si Sn W Zn Zr)
ndash Maybe necessary to pre-dilute samples (if known to be high in concentration)
bull Ensure an adequate rinse time
ndash Should be at least equal to the sample uptake delay
(30-40 seconds typical)
bull May require an acidified rinse solution between samples
(2 HNO3)
bull Other strategies to minimize memory effects
ndash Use an inert spray chamber
ndash Use the ISIS to introduce discrete amounts of sample This means
bull Cones are exposed to less sample matrix = improved stability
bull Less memorycarry-over
bull Reduced uptake amp rinse times = faster measurement
27
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy - Why is This Important
What does ldquoAccuracyrdquo mean
ndash Ability to get the ldquorightrdquo answer for the sample
ndash Heavily dependent on operatorrsquos skill
Why is this important
ndash User loses confidence in the system
ndash Your reputationhellip
bull Customerrsquos question the results
bull Poor performance in ldquoround robinrdquo comparisons
How do You Confirm Accuracy
ndash Check the result for a prepared standard
ndash Measure a certified reference material
ndash Use other quality control checks to check analysis
28
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Calibration standards properly prepared
bull See earlier recommendations ndash important to match to samples prepare
accurately and use them ldquofreshrdquo
ndash Any interferences impacting on results
ndash Use matched standards or standard additions
ndash Ensure isotope selected has no polyatomic interferences
ndash If necessary use ORS3
ndash Precision optimized
bull Optimum signal to noise performance improves accuracy
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
29
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Reprocess data post
run using an
alternate internal
standard
bull Ensure Internal
Standard used is
similar in mass
bull Check whether the
Internal Standard is
present in the
sample
ndash If necessary do a Semi-
Quant measurement
bull Dilute with cal blk
matrix
30
Accuracy ndash Suspect Internal Standard Recovery
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Sample preparation
bull Is the most appropriate digestion being used
bull Are all of the analytes being quantitatively (and reproducibly) extracted and
dissolved
ndash Many digestions are only partial extracts ndash efficiency will vary with the
sample matrix
ndash Some volatile analytes may be ldquolostrdquo during digestion
bull Confirm by taking a solid certified reference material
through your preparation and analysis procedure
bull Is the digest stable ndash or are you seeing any precipitates or a suspension
bull Do you see any potential contamination from either reagents or the digestion
equipment eg especially with Si B or Ca
bull Include a ldquoReagent Blankrdquo with every sample batch to
monitor
31
ICP-MS Maintenance amp Trouble Shooting
May 2012
Laboratory environment can have
direct impact on quality of results
bull Clean uncluttered work area
bull Proper ventilation
bull Safety considerations
bull Instrument lifetime consideration
ICP-MS Maintenance amp Trouble Shooting
May 2012 32
Laboratory Environment
ICP-MS ndash Potential Autosampler Issues
ndash More customers use autosamplers with ICP for automation
ndash Issues to consider
bull Long transfer tube between sampler and ICP-MS
ndash May need to program a longer sample uptake delay
ndash May exacerbate problems with memory effects
ndash Use ldquoFast Pumprdquo during sample uptake delay
bull Caution ndash not always possible
Not recommended with high TDS samples and organics
bull Ensure probe diameter is appropriate for sample matrix
ndash Use wider bore for high TDS or viscous samples
bull Sample stability - potential for sample changes while uncovered in racks ndash impacts accuracy
ndash Dust ingress can introduce contamination
ndash Sample evaporation may occur during long unattended runs
ndash Sediment in the sample may settle out esp with wear metals or suspensions
bull Ensure transfer line to ICP-MS is in good condition
ndash Kinks in the line may cause poor uptake or pulsing in the sample
ndash Impacts on precision and accuracy
33
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sample Throughput ndash What to Check
ndash Samples fully digested
bull No excess particulates in the sample that may cause blockage
ndash Sample Introduction System optimized
ndash Capable of handling the TDS levels in the sample
ndash TorchNebulizer cleaned and ready for analysis
ndash Method parameters optimized
bull Sample uptake delay and stabilization times are appropriate ndash optimized
bull Integration time is appropriate for the expected concentration
ndash Use a longer integration time at low concentrations
bull Rinse time is appropriate
bull Use ldquoISISrdquo discrete sampling for faster measurement and faster washout
34
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Handles tough sample matrices better
than any other ICP-MS
ndash Highest plasma temperature (lowest
CeOCe) as standard
ndash HMI (high matrix introduction) allows direct
analysis of difficult samples
eg sea water
bull ORS3 operates in He collision mode to
remove ALL polyatomic interferences
ndash Enables reliable removal of all polyatomic
interferences using a single set of
conditions
ndash Gives lower levels of interference and
better long-term stability HMI gives lower suppression and
better long-term stability
Relative signal (suppression) in undiluted seawater
Long-term stability in undiluted seawater
35
Agilent ICP-MS Performance - Benefits
Best matrix tolerance amp less interferences
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS ndash Recommended Maintenance Schedule
ICP-MS Maintenance amp Trouble Shooting
May 2012 37
These functions
(and more) are
completed as part
of a Preventative
Maintenance
program by an
Agilent Field
Service Engineer
Summary ndash Key Consumables for ICP-MS
Sample preparationpresentation
ndash Peristaltic pump tubing
ndash Transfer and drain tubing
ndash ICP-MS standard solutions
ndash Internal Standard solutions
ndash Torches
ndash Spray chambers
ndash Nebulizers
Ion Extraction
ndash Sampler and skimmer cones
Autosampling
ndash Sample tubes racks probes and transfer tubing
ISIS
ndash Peristaltic pump tubing ferrules amp fittings
38
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sample Introduction
Key consumables requiring frequent replacement
bull Pump tubing
bull Torches and quartz transfer tube
bull Nebulizers
bull Spray chambers
bull Interface cones (skimmer amp sampler)
bull Transfer amp connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalogue
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24406(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 39
Autosampler Supplies
Key consumables requiring frequent replacement
ndash Peristaltic pump tubing
ndash Sample racks
ndash Sample tubes
ndash Spare probes
ndash Standard racks
ndash Connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24407(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 40
ISIS Supplies
Key consumables requiring frequent replacement
bull Peristaltic pump tubing
bull Ferrules and fittings
bull Valving
For ISIS Hydride Generation Accessory
bull Membrane filter
bull Concentric nebulizer
bull Gas-liquid separator
bull Other tubing and connectors
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceProductListingaspxcat=SubCat2ECS_24437(Agilent)amppcat=SubCat1ECS_24407(Agilent)amprcat=ClassECS_22674(Agilent)
41
ICP-MS Maintenance amp Trouble Shooting
May 2012
Where to Find the Right Consumable Analytical Consumables Agilent Assist
Consumables amp Supplies Instrument Sales ampServices 1-800-227-9770 (Option 11) 1-800-227-9770 (Option 13) wwwagilentcomchemcontactus wwwagilentcomchemcontactus
On-Line resources
ICP-MS Supplies
2nd Edition Speciation Handbook
ICP-MS Journal Archives
Recorded Agilent e-Seminars
ICP-OES Supplies
Atomic Absorption Supplies
Instrument Parts amp Supplies
Atomic Spec Application Notes
Agilent Quick Reference Guide for 77008800 ICP-MS (pub 5990-8182EN)
Agilent Atomic Spec Supplies Catalogue (pub 5990-8767EN)
Agilent Consumables Catalogue (pub 5990-6674EN)
Instrument User Manuals
42
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sensitivity ndash Automated ldquoExpertrdquo Tuning
bull Startup provides a simple
user-configured schedule of
system optimization and
performance checks
bull One-click expert autotuning for
simple plasma optimization
bull Ensures consistent
performance from day to day
bull Independent of operator
experience
bull Automatically generate a
Performance Report
bull Provides a continuing record of
system performance
12
ICP-MS Maintenance amp Trouble Shooting
May 2012
13
Hardware Performance Report
is run under ldquostandardrdquo (factory
check-out) conditions
Gives record of performance
history under consistent default
tuning conditions
Note this is different to the ldquoTune
Reportrdquo which is generated
using Batch tune conditions
Sensitivity ndash Performance Report
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS specific contamination concerns -This is a topic of its own often leads to the clean room
conversation
But remember its not just where your instrument
is located ndash itrsquos everything the sample encounters
on its way to the instrument
ICP-MS Maintenance amp Trouble Shooting
May 2012 14
Sensitivity ndash Cleanliness amp Contamination
Sensitivity ndash Contamination Sources
bull Use high purity or ICP-MS grade reagents
bull Acid purity
ndash Buy only what you need to do the job
ndash Check the certificate of analysis
ndash Donrsquot insert pipette tips into your acids
ndash Use contaminated acid for cleaning
bull Sample containers
ndash Borosilicate glass introduces boron
ndash FEP containers preferred
bull Pipette tips
ndash Colors add interest ndash but increase contamination (Cu Fe Zn Cd)
bull Gloves
ndash Powder free unless you like Zn
Anything that touches sample during prep dilution
transfer analysis and storage
ICP-MS Maintenance amp Trouble Shooting
May 2012 15
PFA spray
chamber
PFA
endcap
PFA
nebulizer
PFA
connector
tube
Quartz torch with sapphire
or platinum injector
Complete sample introduction can be
changed to a system specifically
designed to reduce contamination
bull Usually used for semi-con applications
Clean integrated Auto-Sampler ndash I-AS
Clean sample introduction system - PFA
16
Cleanliness ndash The Ultimate for Contamination Free
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sensitivity ndash System Cleanliness
What to Check
ndash Sample Introduction System
bull Deposits in nebulizer can reduce
sample uptake rate
ndash Soak in aqua regia or use a nebulizer
cleaning tool to back flush
bull Solid material in torch injector
affects aerosol introduction into
plasma and increases noise
bull Contamination in spray chamber
impacts on aerosol formation ndash
increases noise
bull If seeing poor precision may be
due to beading in spray chamber
ndash Soak in 25 detergent solution
overnight (preferably for 24 hours)
17
ICP-MS Maintenance amp Trouble Shooting
May 2012
Nebulizer cleaner
Agilent PN G3266-80020
ICP-MS Sensitivity ndash System Cleanliness
What to Check
ndash Interface cones
bull Deposits or discoloration indicates
cleaning is required
bull Other indicators that cone cleaning
is required
ndash Poor sensitivity
ndash High background
ndash Distorted peak shapes
ndash Changes in interface vacuum reading
(deposition or build-up)
18
ICP-MS Maintenance amp Trouble Shooting
May 2012
Close up
Sample cone after measuring 75 undiluted sea water
samples using HMI Some deposition on outer edges
away from the orifice ndash no blockage of the sampling
orifice ndash but cleaning still recommended
System Cleanliness - Sampling Cone
1 mm Orifice Nickel or Platinum Centres
bull Nickel
bull Physically stronger
bull Tip runs hotter ndash less sample deposition
bull Platinum
bull Chemically stronger
bull Used for higher acid conc (incl HF)
bull 2 centre sizes 10-18 mm
bull Higher cost
Potential Problems
bull Biggest risk is physical damage to the orifice due to excessively aggressive cleaning
bull Cones also affected by sample matrix (acid strength amp type) and number of samples analyzed each day
bull Nickel - Typically replace 3 or 5 each year (assumes measuring 250-350 environmental samples each day)
bull Platinum - Typically replace 1 or 2 each year (assumes measuring 20-50 semiconductor samples each day)
bull If not clean then can result in analytical problems eg poor signal stability elemental contamination
ICP-MS Maintenance amp Trouble Shooting
May 2012 19
System Cleanliness - Skimmer Cone
04 mm Orifice Nickel or Platinum
bull The Nickel skimmer cone is the standard interface
bull The skimmer cone is relatively robust to samples containing high concentrations of matrix and salts and is suitable for a wide variety of samples It is usually used with the Nickel sampling cone
bull The Platinum skimmer cone is usually used for introduction of hydrofluoric acid and other reagents It is usually used with the Platinum sampling cone
Potential Problems
bull Biggest risk is from physical damage to the orifice due to excessively aggressive cleaning
bull Cones also affected by sample matrix (acid strength amp type) and number of samples analyzed each day
bull Nickel ndash Typically replace 3 or 5 each year (assumes measuring 250-350 environmental samples each day)
bull Platinum ndash Typically replace 1 or 2 each year (assumes measuring 20-50 semiconductor samples each day)
bull If not clean then can result in analytical problems eg poor signal stability elemental contamination
20
ICP-MS Maintenance amp Trouble Shooting
May 2012
System Cleanliness - Cone Cleaning Procedure
Caution - Take care to avoid damage to the cone tip when removing ndash and place base down - Check the graphite gasket and replace if creased or damaged - Sonicate in a 2 Citranox or 2 Nitric Acid solution for a few minutes - Rinse well with de-ionized water - If still dirty or memory problems remain polish using an alumina powder slurry on a Q-tip then sonicate in 2 Citranox solution and rinse well with de-ionized water - Dry with nitrogen before installing
22
ICP-MS Maintenance amp Trouble Shooting
May 2012
Precision - Why is This Important
What does ldquoPrecisionrdquo mean
ndash Ability to get the same result for the same
sample when measured multiple times
ndash Usually measured as RSD or sometimes SD
RSD = (SD Mean Result) 100
ndash Low values indicate good precision
bull For ICP-MS expect 1-2 RSD
Why is this important
ndash User loses confidence in the system
What impacts on precision
ndash Nebulizerplasma stability
ndash Sample introduction system
ndash Method parameters
23
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash System stabilized
bull Allow 10 mins for plasma warm-up before
analysis
ndash Plasma status
bull ldquoBulletrdquo in the plasma should be stable
bull Check for deposits in the injector of the torch
ndash Check condition of interface cones and
clean if necessary
ndash Clean the Extraction Lens - Omega Lens
assembly
ndash Method parameters
bull Appropriate times set for sample uptake
delay and stabilization times
24
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash Sample Intro
What to Check ndash Nebulizer
bull Nebulizer type used can impact on sensitivity and precision
ndash MicroMist (glass concentric type) is the standard nebulizer ndash handles most sample
types
ndash PFA MicroFlow nebulizer best for low volume samples aggressive samples (HF
digests) and when low contamination required (semi-con)
ndash Babington gives poorer precision - best for high TDS samples
bull Check nebulizer condition regularly
ndash Chips in the nebulizer tip impact on aerosol formation ndash poor precision
(use a magnifying glass if necessary)
ndash Check for deposits or blockage in the tip
bull Sample uptake or flow rate
ndash Lower pump speed or using narrow bore pump tubing will reduce uptake rate
- better for high TDS samples
25
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Sample Introduction bull Contamination in the spray chamber
ndash When was the spray chamber cleaned
bull Any blockages in the nebulizer injector
ndash Check for stable aerosol formation
bull Air leaks in spray chamber end cap or connecting tubes
ndash Are they in good condition with tight connections
bull Damaged pump tubes
ndash When did you check the pump tubes
bull Is the pump speed too slow
ndash Low pump speeds may cause signal pulsation
ndash If required use narrower bore pump tube and increase pump speed
bull Samples have a high TDS content
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
26
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Memory effects
bull If possible avoid running high concentrations of these analytes
(Ag Au B Hg Mo Si Sn W Zn Zr)
ndash Maybe necessary to pre-dilute samples (if known to be high in concentration)
bull Ensure an adequate rinse time
ndash Should be at least equal to the sample uptake delay
(30-40 seconds typical)
bull May require an acidified rinse solution between samples
(2 HNO3)
bull Other strategies to minimize memory effects
ndash Use an inert spray chamber
ndash Use the ISIS to introduce discrete amounts of sample This means
bull Cones are exposed to less sample matrix = improved stability
bull Less memorycarry-over
bull Reduced uptake amp rinse times = faster measurement
27
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy - Why is This Important
What does ldquoAccuracyrdquo mean
ndash Ability to get the ldquorightrdquo answer for the sample
ndash Heavily dependent on operatorrsquos skill
Why is this important
ndash User loses confidence in the system
ndash Your reputationhellip
bull Customerrsquos question the results
bull Poor performance in ldquoround robinrdquo comparisons
How do You Confirm Accuracy
ndash Check the result for a prepared standard
ndash Measure a certified reference material
ndash Use other quality control checks to check analysis
28
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Calibration standards properly prepared
bull See earlier recommendations ndash important to match to samples prepare
accurately and use them ldquofreshrdquo
ndash Any interferences impacting on results
ndash Use matched standards or standard additions
ndash Ensure isotope selected has no polyatomic interferences
ndash If necessary use ORS3
ndash Precision optimized
bull Optimum signal to noise performance improves accuracy
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
29
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Reprocess data post
run using an
alternate internal
standard
bull Ensure Internal
Standard used is
similar in mass
bull Check whether the
Internal Standard is
present in the
sample
ndash If necessary do a Semi-
Quant measurement
bull Dilute with cal blk
matrix
30
Accuracy ndash Suspect Internal Standard Recovery
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Sample preparation
bull Is the most appropriate digestion being used
bull Are all of the analytes being quantitatively (and reproducibly) extracted and
dissolved
ndash Many digestions are only partial extracts ndash efficiency will vary with the
sample matrix
ndash Some volatile analytes may be ldquolostrdquo during digestion
bull Confirm by taking a solid certified reference material
through your preparation and analysis procedure
bull Is the digest stable ndash or are you seeing any precipitates or a suspension
bull Do you see any potential contamination from either reagents or the digestion
equipment eg especially with Si B or Ca
bull Include a ldquoReagent Blankrdquo with every sample batch to
monitor
31
ICP-MS Maintenance amp Trouble Shooting
May 2012
Laboratory environment can have
direct impact on quality of results
bull Clean uncluttered work area
bull Proper ventilation
bull Safety considerations
bull Instrument lifetime consideration
ICP-MS Maintenance amp Trouble Shooting
May 2012 32
Laboratory Environment
ICP-MS ndash Potential Autosampler Issues
ndash More customers use autosamplers with ICP for automation
ndash Issues to consider
bull Long transfer tube between sampler and ICP-MS
ndash May need to program a longer sample uptake delay
ndash May exacerbate problems with memory effects
ndash Use ldquoFast Pumprdquo during sample uptake delay
bull Caution ndash not always possible
Not recommended with high TDS samples and organics
bull Ensure probe diameter is appropriate for sample matrix
ndash Use wider bore for high TDS or viscous samples
bull Sample stability - potential for sample changes while uncovered in racks ndash impacts accuracy
ndash Dust ingress can introduce contamination
ndash Sample evaporation may occur during long unattended runs
ndash Sediment in the sample may settle out esp with wear metals or suspensions
bull Ensure transfer line to ICP-MS is in good condition
ndash Kinks in the line may cause poor uptake or pulsing in the sample
ndash Impacts on precision and accuracy
33
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sample Throughput ndash What to Check
ndash Samples fully digested
bull No excess particulates in the sample that may cause blockage
ndash Sample Introduction System optimized
ndash Capable of handling the TDS levels in the sample
ndash TorchNebulizer cleaned and ready for analysis
ndash Method parameters optimized
bull Sample uptake delay and stabilization times are appropriate ndash optimized
bull Integration time is appropriate for the expected concentration
ndash Use a longer integration time at low concentrations
bull Rinse time is appropriate
bull Use ldquoISISrdquo discrete sampling for faster measurement and faster washout
34
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Handles tough sample matrices better
than any other ICP-MS
ndash Highest plasma temperature (lowest
CeOCe) as standard
ndash HMI (high matrix introduction) allows direct
analysis of difficult samples
eg sea water
bull ORS3 operates in He collision mode to
remove ALL polyatomic interferences
ndash Enables reliable removal of all polyatomic
interferences using a single set of
conditions
ndash Gives lower levels of interference and
better long-term stability HMI gives lower suppression and
better long-term stability
Relative signal (suppression) in undiluted seawater
Long-term stability in undiluted seawater
35
Agilent ICP-MS Performance - Benefits
Best matrix tolerance amp less interferences
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS ndash Recommended Maintenance Schedule
ICP-MS Maintenance amp Trouble Shooting
May 2012 37
These functions
(and more) are
completed as part
of a Preventative
Maintenance
program by an
Agilent Field
Service Engineer
Summary ndash Key Consumables for ICP-MS
Sample preparationpresentation
ndash Peristaltic pump tubing
ndash Transfer and drain tubing
ndash ICP-MS standard solutions
ndash Internal Standard solutions
ndash Torches
ndash Spray chambers
ndash Nebulizers
Ion Extraction
ndash Sampler and skimmer cones
Autosampling
ndash Sample tubes racks probes and transfer tubing
ISIS
ndash Peristaltic pump tubing ferrules amp fittings
38
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sample Introduction
Key consumables requiring frequent replacement
bull Pump tubing
bull Torches and quartz transfer tube
bull Nebulizers
bull Spray chambers
bull Interface cones (skimmer amp sampler)
bull Transfer amp connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalogue
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24406(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 39
Autosampler Supplies
Key consumables requiring frequent replacement
ndash Peristaltic pump tubing
ndash Sample racks
ndash Sample tubes
ndash Spare probes
ndash Standard racks
ndash Connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24407(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 40
ISIS Supplies
Key consumables requiring frequent replacement
bull Peristaltic pump tubing
bull Ferrules and fittings
bull Valving
For ISIS Hydride Generation Accessory
bull Membrane filter
bull Concentric nebulizer
bull Gas-liquid separator
bull Other tubing and connectors
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceProductListingaspxcat=SubCat2ECS_24437(Agilent)amppcat=SubCat1ECS_24407(Agilent)amprcat=ClassECS_22674(Agilent)
41
ICP-MS Maintenance amp Trouble Shooting
May 2012
Where to Find the Right Consumable Analytical Consumables Agilent Assist
Consumables amp Supplies Instrument Sales ampServices 1-800-227-9770 (Option 11) 1-800-227-9770 (Option 13) wwwagilentcomchemcontactus wwwagilentcomchemcontactus
On-Line resources
ICP-MS Supplies
2nd Edition Speciation Handbook
ICP-MS Journal Archives
Recorded Agilent e-Seminars
ICP-OES Supplies
Atomic Absorption Supplies
Instrument Parts amp Supplies
Atomic Spec Application Notes
Agilent Quick Reference Guide for 77008800 ICP-MS (pub 5990-8182EN)
Agilent Atomic Spec Supplies Catalogue (pub 5990-8767EN)
Agilent Consumables Catalogue (pub 5990-6674EN)
Instrument User Manuals
42
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
13
Hardware Performance Report
is run under ldquostandardrdquo (factory
check-out) conditions
Gives record of performance
history under consistent default
tuning conditions
Note this is different to the ldquoTune
Reportrdquo which is generated
using Batch tune conditions
Sensitivity ndash Performance Report
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS specific contamination concerns -This is a topic of its own often leads to the clean room
conversation
But remember its not just where your instrument
is located ndash itrsquos everything the sample encounters
on its way to the instrument
ICP-MS Maintenance amp Trouble Shooting
May 2012 14
Sensitivity ndash Cleanliness amp Contamination
Sensitivity ndash Contamination Sources
bull Use high purity or ICP-MS grade reagents
bull Acid purity
ndash Buy only what you need to do the job
ndash Check the certificate of analysis
ndash Donrsquot insert pipette tips into your acids
ndash Use contaminated acid for cleaning
bull Sample containers
ndash Borosilicate glass introduces boron
ndash FEP containers preferred
bull Pipette tips
ndash Colors add interest ndash but increase contamination (Cu Fe Zn Cd)
bull Gloves
ndash Powder free unless you like Zn
Anything that touches sample during prep dilution
transfer analysis and storage
ICP-MS Maintenance amp Trouble Shooting
May 2012 15
PFA spray
chamber
PFA
endcap
PFA
nebulizer
PFA
connector
tube
Quartz torch with sapphire
or platinum injector
Complete sample introduction can be
changed to a system specifically
designed to reduce contamination
bull Usually used for semi-con applications
Clean integrated Auto-Sampler ndash I-AS
Clean sample introduction system - PFA
16
Cleanliness ndash The Ultimate for Contamination Free
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sensitivity ndash System Cleanliness
What to Check
ndash Sample Introduction System
bull Deposits in nebulizer can reduce
sample uptake rate
ndash Soak in aqua regia or use a nebulizer
cleaning tool to back flush
bull Solid material in torch injector
affects aerosol introduction into
plasma and increases noise
bull Contamination in spray chamber
impacts on aerosol formation ndash
increases noise
bull If seeing poor precision may be
due to beading in spray chamber
ndash Soak in 25 detergent solution
overnight (preferably for 24 hours)
17
ICP-MS Maintenance amp Trouble Shooting
May 2012
Nebulizer cleaner
Agilent PN G3266-80020
ICP-MS Sensitivity ndash System Cleanliness
What to Check
ndash Interface cones
bull Deposits or discoloration indicates
cleaning is required
bull Other indicators that cone cleaning
is required
ndash Poor sensitivity
ndash High background
ndash Distorted peak shapes
ndash Changes in interface vacuum reading
(deposition or build-up)
18
ICP-MS Maintenance amp Trouble Shooting
May 2012
Close up
Sample cone after measuring 75 undiluted sea water
samples using HMI Some deposition on outer edges
away from the orifice ndash no blockage of the sampling
orifice ndash but cleaning still recommended
System Cleanliness - Sampling Cone
1 mm Orifice Nickel or Platinum Centres
bull Nickel
bull Physically stronger
bull Tip runs hotter ndash less sample deposition
bull Platinum
bull Chemically stronger
bull Used for higher acid conc (incl HF)
bull 2 centre sizes 10-18 mm
bull Higher cost
Potential Problems
bull Biggest risk is physical damage to the orifice due to excessively aggressive cleaning
bull Cones also affected by sample matrix (acid strength amp type) and number of samples analyzed each day
bull Nickel - Typically replace 3 or 5 each year (assumes measuring 250-350 environmental samples each day)
bull Platinum - Typically replace 1 or 2 each year (assumes measuring 20-50 semiconductor samples each day)
bull If not clean then can result in analytical problems eg poor signal stability elemental contamination
ICP-MS Maintenance amp Trouble Shooting
May 2012 19
System Cleanliness - Skimmer Cone
04 mm Orifice Nickel or Platinum
bull The Nickel skimmer cone is the standard interface
bull The skimmer cone is relatively robust to samples containing high concentrations of matrix and salts and is suitable for a wide variety of samples It is usually used with the Nickel sampling cone
bull The Platinum skimmer cone is usually used for introduction of hydrofluoric acid and other reagents It is usually used with the Platinum sampling cone
Potential Problems
bull Biggest risk is from physical damage to the orifice due to excessively aggressive cleaning
bull Cones also affected by sample matrix (acid strength amp type) and number of samples analyzed each day
bull Nickel ndash Typically replace 3 or 5 each year (assumes measuring 250-350 environmental samples each day)
bull Platinum ndash Typically replace 1 or 2 each year (assumes measuring 20-50 semiconductor samples each day)
bull If not clean then can result in analytical problems eg poor signal stability elemental contamination
20
ICP-MS Maintenance amp Trouble Shooting
May 2012
System Cleanliness - Cone Cleaning Procedure
Caution - Take care to avoid damage to the cone tip when removing ndash and place base down - Check the graphite gasket and replace if creased or damaged - Sonicate in a 2 Citranox or 2 Nitric Acid solution for a few minutes - Rinse well with de-ionized water - If still dirty or memory problems remain polish using an alumina powder slurry on a Q-tip then sonicate in 2 Citranox solution and rinse well with de-ionized water - Dry with nitrogen before installing
22
ICP-MS Maintenance amp Trouble Shooting
May 2012
Precision - Why is This Important
What does ldquoPrecisionrdquo mean
ndash Ability to get the same result for the same
sample when measured multiple times
ndash Usually measured as RSD or sometimes SD
RSD = (SD Mean Result) 100
ndash Low values indicate good precision
bull For ICP-MS expect 1-2 RSD
Why is this important
ndash User loses confidence in the system
What impacts on precision
ndash Nebulizerplasma stability
ndash Sample introduction system
ndash Method parameters
23
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash System stabilized
bull Allow 10 mins for plasma warm-up before
analysis
ndash Plasma status
bull ldquoBulletrdquo in the plasma should be stable
bull Check for deposits in the injector of the torch
ndash Check condition of interface cones and
clean if necessary
ndash Clean the Extraction Lens - Omega Lens
assembly
ndash Method parameters
bull Appropriate times set for sample uptake
delay and stabilization times
24
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash Sample Intro
What to Check ndash Nebulizer
bull Nebulizer type used can impact on sensitivity and precision
ndash MicroMist (glass concentric type) is the standard nebulizer ndash handles most sample
types
ndash PFA MicroFlow nebulizer best for low volume samples aggressive samples (HF
digests) and when low contamination required (semi-con)
ndash Babington gives poorer precision - best for high TDS samples
bull Check nebulizer condition regularly
ndash Chips in the nebulizer tip impact on aerosol formation ndash poor precision
(use a magnifying glass if necessary)
ndash Check for deposits or blockage in the tip
bull Sample uptake or flow rate
ndash Lower pump speed or using narrow bore pump tubing will reduce uptake rate
- better for high TDS samples
25
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Sample Introduction bull Contamination in the spray chamber
ndash When was the spray chamber cleaned
bull Any blockages in the nebulizer injector
ndash Check for stable aerosol formation
bull Air leaks in spray chamber end cap or connecting tubes
ndash Are they in good condition with tight connections
bull Damaged pump tubes
ndash When did you check the pump tubes
bull Is the pump speed too slow
ndash Low pump speeds may cause signal pulsation
ndash If required use narrower bore pump tube and increase pump speed
bull Samples have a high TDS content
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
26
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Memory effects
bull If possible avoid running high concentrations of these analytes
(Ag Au B Hg Mo Si Sn W Zn Zr)
ndash Maybe necessary to pre-dilute samples (if known to be high in concentration)
bull Ensure an adequate rinse time
ndash Should be at least equal to the sample uptake delay
(30-40 seconds typical)
bull May require an acidified rinse solution between samples
(2 HNO3)
bull Other strategies to minimize memory effects
ndash Use an inert spray chamber
ndash Use the ISIS to introduce discrete amounts of sample This means
bull Cones are exposed to less sample matrix = improved stability
bull Less memorycarry-over
bull Reduced uptake amp rinse times = faster measurement
27
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy - Why is This Important
What does ldquoAccuracyrdquo mean
ndash Ability to get the ldquorightrdquo answer for the sample
ndash Heavily dependent on operatorrsquos skill
Why is this important
ndash User loses confidence in the system
ndash Your reputationhellip
bull Customerrsquos question the results
bull Poor performance in ldquoround robinrdquo comparisons
How do You Confirm Accuracy
ndash Check the result for a prepared standard
ndash Measure a certified reference material
ndash Use other quality control checks to check analysis
28
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Calibration standards properly prepared
bull See earlier recommendations ndash important to match to samples prepare
accurately and use them ldquofreshrdquo
ndash Any interferences impacting on results
ndash Use matched standards or standard additions
ndash Ensure isotope selected has no polyatomic interferences
ndash If necessary use ORS3
ndash Precision optimized
bull Optimum signal to noise performance improves accuracy
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
29
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Reprocess data post
run using an
alternate internal
standard
bull Ensure Internal
Standard used is
similar in mass
bull Check whether the
Internal Standard is
present in the
sample
ndash If necessary do a Semi-
Quant measurement
bull Dilute with cal blk
matrix
30
Accuracy ndash Suspect Internal Standard Recovery
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Sample preparation
bull Is the most appropriate digestion being used
bull Are all of the analytes being quantitatively (and reproducibly) extracted and
dissolved
ndash Many digestions are only partial extracts ndash efficiency will vary with the
sample matrix
ndash Some volatile analytes may be ldquolostrdquo during digestion
bull Confirm by taking a solid certified reference material
through your preparation and analysis procedure
bull Is the digest stable ndash or are you seeing any precipitates or a suspension
bull Do you see any potential contamination from either reagents or the digestion
equipment eg especially with Si B or Ca
bull Include a ldquoReagent Blankrdquo with every sample batch to
monitor
31
ICP-MS Maintenance amp Trouble Shooting
May 2012
Laboratory environment can have
direct impact on quality of results
bull Clean uncluttered work area
bull Proper ventilation
bull Safety considerations
bull Instrument lifetime consideration
ICP-MS Maintenance amp Trouble Shooting
May 2012 32
Laboratory Environment
ICP-MS ndash Potential Autosampler Issues
ndash More customers use autosamplers with ICP for automation
ndash Issues to consider
bull Long transfer tube between sampler and ICP-MS
ndash May need to program a longer sample uptake delay
ndash May exacerbate problems with memory effects
ndash Use ldquoFast Pumprdquo during sample uptake delay
bull Caution ndash not always possible
Not recommended with high TDS samples and organics
bull Ensure probe diameter is appropriate for sample matrix
ndash Use wider bore for high TDS or viscous samples
bull Sample stability - potential for sample changes while uncovered in racks ndash impacts accuracy
ndash Dust ingress can introduce contamination
ndash Sample evaporation may occur during long unattended runs
ndash Sediment in the sample may settle out esp with wear metals or suspensions
bull Ensure transfer line to ICP-MS is in good condition
ndash Kinks in the line may cause poor uptake or pulsing in the sample
ndash Impacts on precision and accuracy
33
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sample Throughput ndash What to Check
ndash Samples fully digested
bull No excess particulates in the sample that may cause blockage
ndash Sample Introduction System optimized
ndash Capable of handling the TDS levels in the sample
ndash TorchNebulizer cleaned and ready for analysis
ndash Method parameters optimized
bull Sample uptake delay and stabilization times are appropriate ndash optimized
bull Integration time is appropriate for the expected concentration
ndash Use a longer integration time at low concentrations
bull Rinse time is appropriate
bull Use ldquoISISrdquo discrete sampling for faster measurement and faster washout
34
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Handles tough sample matrices better
than any other ICP-MS
ndash Highest plasma temperature (lowest
CeOCe) as standard
ndash HMI (high matrix introduction) allows direct
analysis of difficult samples
eg sea water
bull ORS3 operates in He collision mode to
remove ALL polyatomic interferences
ndash Enables reliable removal of all polyatomic
interferences using a single set of
conditions
ndash Gives lower levels of interference and
better long-term stability HMI gives lower suppression and
better long-term stability
Relative signal (suppression) in undiluted seawater
Long-term stability in undiluted seawater
35
Agilent ICP-MS Performance - Benefits
Best matrix tolerance amp less interferences
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS ndash Recommended Maintenance Schedule
ICP-MS Maintenance amp Trouble Shooting
May 2012 37
These functions
(and more) are
completed as part
of a Preventative
Maintenance
program by an
Agilent Field
Service Engineer
Summary ndash Key Consumables for ICP-MS
Sample preparationpresentation
ndash Peristaltic pump tubing
ndash Transfer and drain tubing
ndash ICP-MS standard solutions
ndash Internal Standard solutions
ndash Torches
ndash Spray chambers
ndash Nebulizers
Ion Extraction
ndash Sampler and skimmer cones
Autosampling
ndash Sample tubes racks probes and transfer tubing
ISIS
ndash Peristaltic pump tubing ferrules amp fittings
38
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sample Introduction
Key consumables requiring frequent replacement
bull Pump tubing
bull Torches and quartz transfer tube
bull Nebulizers
bull Spray chambers
bull Interface cones (skimmer amp sampler)
bull Transfer amp connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalogue
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24406(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 39
Autosampler Supplies
Key consumables requiring frequent replacement
ndash Peristaltic pump tubing
ndash Sample racks
ndash Sample tubes
ndash Spare probes
ndash Standard racks
ndash Connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24407(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 40
ISIS Supplies
Key consumables requiring frequent replacement
bull Peristaltic pump tubing
bull Ferrules and fittings
bull Valving
For ISIS Hydride Generation Accessory
bull Membrane filter
bull Concentric nebulizer
bull Gas-liquid separator
bull Other tubing and connectors
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceProductListingaspxcat=SubCat2ECS_24437(Agilent)amppcat=SubCat1ECS_24407(Agilent)amprcat=ClassECS_22674(Agilent)
41
ICP-MS Maintenance amp Trouble Shooting
May 2012
Where to Find the Right Consumable Analytical Consumables Agilent Assist
Consumables amp Supplies Instrument Sales ampServices 1-800-227-9770 (Option 11) 1-800-227-9770 (Option 13) wwwagilentcomchemcontactus wwwagilentcomchemcontactus
On-Line resources
ICP-MS Supplies
2nd Edition Speciation Handbook
ICP-MS Journal Archives
Recorded Agilent e-Seminars
ICP-OES Supplies
Atomic Absorption Supplies
Instrument Parts amp Supplies
Atomic Spec Application Notes
Agilent Quick Reference Guide for 77008800 ICP-MS (pub 5990-8182EN)
Agilent Atomic Spec Supplies Catalogue (pub 5990-8767EN)
Agilent Consumables Catalogue (pub 5990-6674EN)
Instrument User Manuals
42
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS specific contamination concerns -This is a topic of its own often leads to the clean room
conversation
But remember its not just where your instrument
is located ndash itrsquos everything the sample encounters
on its way to the instrument
ICP-MS Maintenance amp Trouble Shooting
May 2012 14
Sensitivity ndash Cleanliness amp Contamination
Sensitivity ndash Contamination Sources
bull Use high purity or ICP-MS grade reagents
bull Acid purity
ndash Buy only what you need to do the job
ndash Check the certificate of analysis
ndash Donrsquot insert pipette tips into your acids
ndash Use contaminated acid for cleaning
bull Sample containers
ndash Borosilicate glass introduces boron
ndash FEP containers preferred
bull Pipette tips
ndash Colors add interest ndash but increase contamination (Cu Fe Zn Cd)
bull Gloves
ndash Powder free unless you like Zn
Anything that touches sample during prep dilution
transfer analysis and storage
ICP-MS Maintenance amp Trouble Shooting
May 2012 15
PFA spray
chamber
PFA
endcap
PFA
nebulizer
PFA
connector
tube
Quartz torch with sapphire
or platinum injector
Complete sample introduction can be
changed to a system specifically
designed to reduce contamination
bull Usually used for semi-con applications
Clean integrated Auto-Sampler ndash I-AS
Clean sample introduction system - PFA
16
Cleanliness ndash The Ultimate for Contamination Free
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sensitivity ndash System Cleanliness
What to Check
ndash Sample Introduction System
bull Deposits in nebulizer can reduce
sample uptake rate
ndash Soak in aqua regia or use a nebulizer
cleaning tool to back flush
bull Solid material in torch injector
affects aerosol introduction into
plasma and increases noise
bull Contamination in spray chamber
impacts on aerosol formation ndash
increases noise
bull If seeing poor precision may be
due to beading in spray chamber
ndash Soak in 25 detergent solution
overnight (preferably for 24 hours)
17
ICP-MS Maintenance amp Trouble Shooting
May 2012
Nebulizer cleaner
Agilent PN G3266-80020
ICP-MS Sensitivity ndash System Cleanliness
What to Check
ndash Interface cones
bull Deposits or discoloration indicates
cleaning is required
bull Other indicators that cone cleaning
is required
ndash Poor sensitivity
ndash High background
ndash Distorted peak shapes
ndash Changes in interface vacuum reading
(deposition or build-up)
18
ICP-MS Maintenance amp Trouble Shooting
May 2012
Close up
Sample cone after measuring 75 undiluted sea water
samples using HMI Some deposition on outer edges
away from the orifice ndash no blockage of the sampling
orifice ndash but cleaning still recommended
System Cleanliness - Sampling Cone
1 mm Orifice Nickel or Platinum Centres
bull Nickel
bull Physically stronger
bull Tip runs hotter ndash less sample deposition
bull Platinum
bull Chemically stronger
bull Used for higher acid conc (incl HF)
bull 2 centre sizes 10-18 mm
bull Higher cost
Potential Problems
bull Biggest risk is physical damage to the orifice due to excessively aggressive cleaning
bull Cones also affected by sample matrix (acid strength amp type) and number of samples analyzed each day
bull Nickel - Typically replace 3 or 5 each year (assumes measuring 250-350 environmental samples each day)
bull Platinum - Typically replace 1 or 2 each year (assumes measuring 20-50 semiconductor samples each day)
bull If not clean then can result in analytical problems eg poor signal stability elemental contamination
ICP-MS Maintenance amp Trouble Shooting
May 2012 19
System Cleanliness - Skimmer Cone
04 mm Orifice Nickel or Platinum
bull The Nickel skimmer cone is the standard interface
bull The skimmer cone is relatively robust to samples containing high concentrations of matrix and salts and is suitable for a wide variety of samples It is usually used with the Nickel sampling cone
bull The Platinum skimmer cone is usually used for introduction of hydrofluoric acid and other reagents It is usually used with the Platinum sampling cone
Potential Problems
bull Biggest risk is from physical damage to the orifice due to excessively aggressive cleaning
bull Cones also affected by sample matrix (acid strength amp type) and number of samples analyzed each day
bull Nickel ndash Typically replace 3 or 5 each year (assumes measuring 250-350 environmental samples each day)
bull Platinum ndash Typically replace 1 or 2 each year (assumes measuring 20-50 semiconductor samples each day)
bull If not clean then can result in analytical problems eg poor signal stability elemental contamination
20
ICP-MS Maintenance amp Trouble Shooting
May 2012
System Cleanliness - Cone Cleaning Procedure
Caution - Take care to avoid damage to the cone tip when removing ndash and place base down - Check the graphite gasket and replace if creased or damaged - Sonicate in a 2 Citranox or 2 Nitric Acid solution for a few minutes - Rinse well with de-ionized water - If still dirty or memory problems remain polish using an alumina powder slurry on a Q-tip then sonicate in 2 Citranox solution and rinse well with de-ionized water - Dry with nitrogen before installing
22
ICP-MS Maintenance amp Trouble Shooting
May 2012
Precision - Why is This Important
What does ldquoPrecisionrdquo mean
ndash Ability to get the same result for the same
sample when measured multiple times
ndash Usually measured as RSD or sometimes SD
RSD = (SD Mean Result) 100
ndash Low values indicate good precision
bull For ICP-MS expect 1-2 RSD
Why is this important
ndash User loses confidence in the system
What impacts on precision
ndash Nebulizerplasma stability
ndash Sample introduction system
ndash Method parameters
23
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash System stabilized
bull Allow 10 mins for plasma warm-up before
analysis
ndash Plasma status
bull ldquoBulletrdquo in the plasma should be stable
bull Check for deposits in the injector of the torch
ndash Check condition of interface cones and
clean if necessary
ndash Clean the Extraction Lens - Omega Lens
assembly
ndash Method parameters
bull Appropriate times set for sample uptake
delay and stabilization times
24
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash Sample Intro
What to Check ndash Nebulizer
bull Nebulizer type used can impact on sensitivity and precision
ndash MicroMist (glass concentric type) is the standard nebulizer ndash handles most sample
types
ndash PFA MicroFlow nebulizer best for low volume samples aggressive samples (HF
digests) and when low contamination required (semi-con)
ndash Babington gives poorer precision - best for high TDS samples
bull Check nebulizer condition regularly
ndash Chips in the nebulizer tip impact on aerosol formation ndash poor precision
(use a magnifying glass if necessary)
ndash Check for deposits or blockage in the tip
bull Sample uptake or flow rate
ndash Lower pump speed or using narrow bore pump tubing will reduce uptake rate
- better for high TDS samples
25
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Sample Introduction bull Contamination in the spray chamber
ndash When was the spray chamber cleaned
bull Any blockages in the nebulizer injector
ndash Check for stable aerosol formation
bull Air leaks in spray chamber end cap or connecting tubes
ndash Are they in good condition with tight connections
bull Damaged pump tubes
ndash When did you check the pump tubes
bull Is the pump speed too slow
ndash Low pump speeds may cause signal pulsation
ndash If required use narrower bore pump tube and increase pump speed
bull Samples have a high TDS content
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
26
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Memory effects
bull If possible avoid running high concentrations of these analytes
(Ag Au B Hg Mo Si Sn W Zn Zr)
ndash Maybe necessary to pre-dilute samples (if known to be high in concentration)
bull Ensure an adequate rinse time
ndash Should be at least equal to the sample uptake delay
(30-40 seconds typical)
bull May require an acidified rinse solution between samples
(2 HNO3)
bull Other strategies to minimize memory effects
ndash Use an inert spray chamber
ndash Use the ISIS to introduce discrete amounts of sample This means
bull Cones are exposed to less sample matrix = improved stability
bull Less memorycarry-over
bull Reduced uptake amp rinse times = faster measurement
27
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy - Why is This Important
What does ldquoAccuracyrdquo mean
ndash Ability to get the ldquorightrdquo answer for the sample
ndash Heavily dependent on operatorrsquos skill
Why is this important
ndash User loses confidence in the system
ndash Your reputationhellip
bull Customerrsquos question the results
bull Poor performance in ldquoround robinrdquo comparisons
How do You Confirm Accuracy
ndash Check the result for a prepared standard
ndash Measure a certified reference material
ndash Use other quality control checks to check analysis
28
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Calibration standards properly prepared
bull See earlier recommendations ndash important to match to samples prepare
accurately and use them ldquofreshrdquo
ndash Any interferences impacting on results
ndash Use matched standards or standard additions
ndash Ensure isotope selected has no polyatomic interferences
ndash If necessary use ORS3
ndash Precision optimized
bull Optimum signal to noise performance improves accuracy
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
29
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Reprocess data post
run using an
alternate internal
standard
bull Ensure Internal
Standard used is
similar in mass
bull Check whether the
Internal Standard is
present in the
sample
ndash If necessary do a Semi-
Quant measurement
bull Dilute with cal blk
matrix
30
Accuracy ndash Suspect Internal Standard Recovery
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Sample preparation
bull Is the most appropriate digestion being used
bull Are all of the analytes being quantitatively (and reproducibly) extracted and
dissolved
ndash Many digestions are only partial extracts ndash efficiency will vary with the
sample matrix
ndash Some volatile analytes may be ldquolostrdquo during digestion
bull Confirm by taking a solid certified reference material
through your preparation and analysis procedure
bull Is the digest stable ndash or are you seeing any precipitates or a suspension
bull Do you see any potential contamination from either reagents or the digestion
equipment eg especially with Si B or Ca
bull Include a ldquoReagent Blankrdquo with every sample batch to
monitor
31
ICP-MS Maintenance amp Trouble Shooting
May 2012
Laboratory environment can have
direct impact on quality of results
bull Clean uncluttered work area
bull Proper ventilation
bull Safety considerations
bull Instrument lifetime consideration
ICP-MS Maintenance amp Trouble Shooting
May 2012 32
Laboratory Environment
ICP-MS ndash Potential Autosampler Issues
ndash More customers use autosamplers with ICP for automation
ndash Issues to consider
bull Long transfer tube between sampler and ICP-MS
ndash May need to program a longer sample uptake delay
ndash May exacerbate problems with memory effects
ndash Use ldquoFast Pumprdquo during sample uptake delay
bull Caution ndash not always possible
Not recommended with high TDS samples and organics
bull Ensure probe diameter is appropriate for sample matrix
ndash Use wider bore for high TDS or viscous samples
bull Sample stability - potential for sample changes while uncovered in racks ndash impacts accuracy
ndash Dust ingress can introduce contamination
ndash Sample evaporation may occur during long unattended runs
ndash Sediment in the sample may settle out esp with wear metals or suspensions
bull Ensure transfer line to ICP-MS is in good condition
ndash Kinks in the line may cause poor uptake or pulsing in the sample
ndash Impacts on precision and accuracy
33
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sample Throughput ndash What to Check
ndash Samples fully digested
bull No excess particulates in the sample that may cause blockage
ndash Sample Introduction System optimized
ndash Capable of handling the TDS levels in the sample
ndash TorchNebulizer cleaned and ready for analysis
ndash Method parameters optimized
bull Sample uptake delay and stabilization times are appropriate ndash optimized
bull Integration time is appropriate for the expected concentration
ndash Use a longer integration time at low concentrations
bull Rinse time is appropriate
bull Use ldquoISISrdquo discrete sampling for faster measurement and faster washout
34
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Handles tough sample matrices better
than any other ICP-MS
ndash Highest plasma temperature (lowest
CeOCe) as standard
ndash HMI (high matrix introduction) allows direct
analysis of difficult samples
eg sea water
bull ORS3 operates in He collision mode to
remove ALL polyatomic interferences
ndash Enables reliable removal of all polyatomic
interferences using a single set of
conditions
ndash Gives lower levels of interference and
better long-term stability HMI gives lower suppression and
better long-term stability
Relative signal (suppression) in undiluted seawater
Long-term stability in undiluted seawater
35
Agilent ICP-MS Performance - Benefits
Best matrix tolerance amp less interferences
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS ndash Recommended Maintenance Schedule
ICP-MS Maintenance amp Trouble Shooting
May 2012 37
These functions
(and more) are
completed as part
of a Preventative
Maintenance
program by an
Agilent Field
Service Engineer
Summary ndash Key Consumables for ICP-MS
Sample preparationpresentation
ndash Peristaltic pump tubing
ndash Transfer and drain tubing
ndash ICP-MS standard solutions
ndash Internal Standard solutions
ndash Torches
ndash Spray chambers
ndash Nebulizers
Ion Extraction
ndash Sampler and skimmer cones
Autosampling
ndash Sample tubes racks probes and transfer tubing
ISIS
ndash Peristaltic pump tubing ferrules amp fittings
38
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sample Introduction
Key consumables requiring frequent replacement
bull Pump tubing
bull Torches and quartz transfer tube
bull Nebulizers
bull Spray chambers
bull Interface cones (skimmer amp sampler)
bull Transfer amp connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalogue
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24406(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 39
Autosampler Supplies
Key consumables requiring frequent replacement
ndash Peristaltic pump tubing
ndash Sample racks
ndash Sample tubes
ndash Spare probes
ndash Standard racks
ndash Connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24407(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 40
ISIS Supplies
Key consumables requiring frequent replacement
bull Peristaltic pump tubing
bull Ferrules and fittings
bull Valving
For ISIS Hydride Generation Accessory
bull Membrane filter
bull Concentric nebulizer
bull Gas-liquid separator
bull Other tubing and connectors
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceProductListingaspxcat=SubCat2ECS_24437(Agilent)amppcat=SubCat1ECS_24407(Agilent)amprcat=ClassECS_22674(Agilent)
41
ICP-MS Maintenance amp Trouble Shooting
May 2012
Where to Find the Right Consumable Analytical Consumables Agilent Assist
Consumables amp Supplies Instrument Sales ampServices 1-800-227-9770 (Option 11) 1-800-227-9770 (Option 13) wwwagilentcomchemcontactus wwwagilentcomchemcontactus
On-Line resources
ICP-MS Supplies
2nd Edition Speciation Handbook
ICP-MS Journal Archives
Recorded Agilent e-Seminars
ICP-OES Supplies
Atomic Absorption Supplies
Instrument Parts amp Supplies
Atomic Spec Application Notes
Agilent Quick Reference Guide for 77008800 ICP-MS (pub 5990-8182EN)
Agilent Atomic Spec Supplies Catalogue (pub 5990-8767EN)
Agilent Consumables Catalogue (pub 5990-6674EN)
Instrument User Manuals
42
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sensitivity ndash Contamination Sources
bull Use high purity or ICP-MS grade reagents
bull Acid purity
ndash Buy only what you need to do the job
ndash Check the certificate of analysis
ndash Donrsquot insert pipette tips into your acids
ndash Use contaminated acid for cleaning
bull Sample containers
ndash Borosilicate glass introduces boron
ndash FEP containers preferred
bull Pipette tips
ndash Colors add interest ndash but increase contamination (Cu Fe Zn Cd)
bull Gloves
ndash Powder free unless you like Zn
Anything that touches sample during prep dilution
transfer analysis and storage
ICP-MS Maintenance amp Trouble Shooting
May 2012 15
PFA spray
chamber
PFA
endcap
PFA
nebulizer
PFA
connector
tube
Quartz torch with sapphire
or platinum injector
Complete sample introduction can be
changed to a system specifically
designed to reduce contamination
bull Usually used for semi-con applications
Clean integrated Auto-Sampler ndash I-AS
Clean sample introduction system - PFA
16
Cleanliness ndash The Ultimate for Contamination Free
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sensitivity ndash System Cleanliness
What to Check
ndash Sample Introduction System
bull Deposits in nebulizer can reduce
sample uptake rate
ndash Soak in aqua regia or use a nebulizer
cleaning tool to back flush
bull Solid material in torch injector
affects aerosol introduction into
plasma and increases noise
bull Contamination in spray chamber
impacts on aerosol formation ndash
increases noise
bull If seeing poor precision may be
due to beading in spray chamber
ndash Soak in 25 detergent solution
overnight (preferably for 24 hours)
17
ICP-MS Maintenance amp Trouble Shooting
May 2012
Nebulizer cleaner
Agilent PN G3266-80020
ICP-MS Sensitivity ndash System Cleanliness
What to Check
ndash Interface cones
bull Deposits or discoloration indicates
cleaning is required
bull Other indicators that cone cleaning
is required
ndash Poor sensitivity
ndash High background
ndash Distorted peak shapes
ndash Changes in interface vacuum reading
(deposition or build-up)
18
ICP-MS Maintenance amp Trouble Shooting
May 2012
Close up
Sample cone after measuring 75 undiluted sea water
samples using HMI Some deposition on outer edges
away from the orifice ndash no blockage of the sampling
orifice ndash but cleaning still recommended
System Cleanliness - Sampling Cone
1 mm Orifice Nickel or Platinum Centres
bull Nickel
bull Physically stronger
bull Tip runs hotter ndash less sample deposition
bull Platinum
bull Chemically stronger
bull Used for higher acid conc (incl HF)
bull 2 centre sizes 10-18 mm
bull Higher cost
Potential Problems
bull Biggest risk is physical damage to the orifice due to excessively aggressive cleaning
bull Cones also affected by sample matrix (acid strength amp type) and number of samples analyzed each day
bull Nickel - Typically replace 3 or 5 each year (assumes measuring 250-350 environmental samples each day)
bull Platinum - Typically replace 1 or 2 each year (assumes measuring 20-50 semiconductor samples each day)
bull If not clean then can result in analytical problems eg poor signal stability elemental contamination
ICP-MS Maintenance amp Trouble Shooting
May 2012 19
System Cleanliness - Skimmer Cone
04 mm Orifice Nickel or Platinum
bull The Nickel skimmer cone is the standard interface
bull The skimmer cone is relatively robust to samples containing high concentrations of matrix and salts and is suitable for a wide variety of samples It is usually used with the Nickel sampling cone
bull The Platinum skimmer cone is usually used for introduction of hydrofluoric acid and other reagents It is usually used with the Platinum sampling cone
Potential Problems
bull Biggest risk is from physical damage to the orifice due to excessively aggressive cleaning
bull Cones also affected by sample matrix (acid strength amp type) and number of samples analyzed each day
bull Nickel ndash Typically replace 3 or 5 each year (assumes measuring 250-350 environmental samples each day)
bull Platinum ndash Typically replace 1 or 2 each year (assumes measuring 20-50 semiconductor samples each day)
bull If not clean then can result in analytical problems eg poor signal stability elemental contamination
20
ICP-MS Maintenance amp Trouble Shooting
May 2012
System Cleanliness - Cone Cleaning Procedure
Caution - Take care to avoid damage to the cone tip when removing ndash and place base down - Check the graphite gasket and replace if creased or damaged - Sonicate in a 2 Citranox or 2 Nitric Acid solution for a few minutes - Rinse well with de-ionized water - If still dirty or memory problems remain polish using an alumina powder slurry on a Q-tip then sonicate in 2 Citranox solution and rinse well with de-ionized water - Dry with nitrogen before installing
22
ICP-MS Maintenance amp Trouble Shooting
May 2012
Precision - Why is This Important
What does ldquoPrecisionrdquo mean
ndash Ability to get the same result for the same
sample when measured multiple times
ndash Usually measured as RSD or sometimes SD
RSD = (SD Mean Result) 100
ndash Low values indicate good precision
bull For ICP-MS expect 1-2 RSD
Why is this important
ndash User loses confidence in the system
What impacts on precision
ndash Nebulizerplasma stability
ndash Sample introduction system
ndash Method parameters
23
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash System stabilized
bull Allow 10 mins for plasma warm-up before
analysis
ndash Plasma status
bull ldquoBulletrdquo in the plasma should be stable
bull Check for deposits in the injector of the torch
ndash Check condition of interface cones and
clean if necessary
ndash Clean the Extraction Lens - Omega Lens
assembly
ndash Method parameters
bull Appropriate times set for sample uptake
delay and stabilization times
24
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash Sample Intro
What to Check ndash Nebulizer
bull Nebulizer type used can impact on sensitivity and precision
ndash MicroMist (glass concentric type) is the standard nebulizer ndash handles most sample
types
ndash PFA MicroFlow nebulizer best for low volume samples aggressive samples (HF
digests) and when low contamination required (semi-con)
ndash Babington gives poorer precision - best for high TDS samples
bull Check nebulizer condition regularly
ndash Chips in the nebulizer tip impact on aerosol formation ndash poor precision
(use a magnifying glass if necessary)
ndash Check for deposits or blockage in the tip
bull Sample uptake or flow rate
ndash Lower pump speed or using narrow bore pump tubing will reduce uptake rate
- better for high TDS samples
25
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Sample Introduction bull Contamination in the spray chamber
ndash When was the spray chamber cleaned
bull Any blockages in the nebulizer injector
ndash Check for stable aerosol formation
bull Air leaks in spray chamber end cap or connecting tubes
ndash Are they in good condition with tight connections
bull Damaged pump tubes
ndash When did you check the pump tubes
bull Is the pump speed too slow
ndash Low pump speeds may cause signal pulsation
ndash If required use narrower bore pump tube and increase pump speed
bull Samples have a high TDS content
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
26
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Memory effects
bull If possible avoid running high concentrations of these analytes
(Ag Au B Hg Mo Si Sn W Zn Zr)
ndash Maybe necessary to pre-dilute samples (if known to be high in concentration)
bull Ensure an adequate rinse time
ndash Should be at least equal to the sample uptake delay
(30-40 seconds typical)
bull May require an acidified rinse solution between samples
(2 HNO3)
bull Other strategies to minimize memory effects
ndash Use an inert spray chamber
ndash Use the ISIS to introduce discrete amounts of sample This means
bull Cones are exposed to less sample matrix = improved stability
bull Less memorycarry-over
bull Reduced uptake amp rinse times = faster measurement
27
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy - Why is This Important
What does ldquoAccuracyrdquo mean
ndash Ability to get the ldquorightrdquo answer for the sample
ndash Heavily dependent on operatorrsquos skill
Why is this important
ndash User loses confidence in the system
ndash Your reputationhellip
bull Customerrsquos question the results
bull Poor performance in ldquoround robinrdquo comparisons
How do You Confirm Accuracy
ndash Check the result for a prepared standard
ndash Measure a certified reference material
ndash Use other quality control checks to check analysis
28
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Calibration standards properly prepared
bull See earlier recommendations ndash important to match to samples prepare
accurately and use them ldquofreshrdquo
ndash Any interferences impacting on results
ndash Use matched standards or standard additions
ndash Ensure isotope selected has no polyatomic interferences
ndash If necessary use ORS3
ndash Precision optimized
bull Optimum signal to noise performance improves accuracy
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
29
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Reprocess data post
run using an
alternate internal
standard
bull Ensure Internal
Standard used is
similar in mass
bull Check whether the
Internal Standard is
present in the
sample
ndash If necessary do a Semi-
Quant measurement
bull Dilute with cal blk
matrix
30
Accuracy ndash Suspect Internal Standard Recovery
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Sample preparation
bull Is the most appropriate digestion being used
bull Are all of the analytes being quantitatively (and reproducibly) extracted and
dissolved
ndash Many digestions are only partial extracts ndash efficiency will vary with the
sample matrix
ndash Some volatile analytes may be ldquolostrdquo during digestion
bull Confirm by taking a solid certified reference material
through your preparation and analysis procedure
bull Is the digest stable ndash or are you seeing any precipitates or a suspension
bull Do you see any potential contamination from either reagents or the digestion
equipment eg especially with Si B or Ca
bull Include a ldquoReagent Blankrdquo with every sample batch to
monitor
31
ICP-MS Maintenance amp Trouble Shooting
May 2012
Laboratory environment can have
direct impact on quality of results
bull Clean uncluttered work area
bull Proper ventilation
bull Safety considerations
bull Instrument lifetime consideration
ICP-MS Maintenance amp Trouble Shooting
May 2012 32
Laboratory Environment
ICP-MS ndash Potential Autosampler Issues
ndash More customers use autosamplers with ICP for automation
ndash Issues to consider
bull Long transfer tube between sampler and ICP-MS
ndash May need to program a longer sample uptake delay
ndash May exacerbate problems with memory effects
ndash Use ldquoFast Pumprdquo during sample uptake delay
bull Caution ndash not always possible
Not recommended with high TDS samples and organics
bull Ensure probe diameter is appropriate for sample matrix
ndash Use wider bore for high TDS or viscous samples
bull Sample stability - potential for sample changes while uncovered in racks ndash impacts accuracy
ndash Dust ingress can introduce contamination
ndash Sample evaporation may occur during long unattended runs
ndash Sediment in the sample may settle out esp with wear metals or suspensions
bull Ensure transfer line to ICP-MS is in good condition
ndash Kinks in the line may cause poor uptake or pulsing in the sample
ndash Impacts on precision and accuracy
33
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sample Throughput ndash What to Check
ndash Samples fully digested
bull No excess particulates in the sample that may cause blockage
ndash Sample Introduction System optimized
ndash Capable of handling the TDS levels in the sample
ndash TorchNebulizer cleaned and ready for analysis
ndash Method parameters optimized
bull Sample uptake delay and stabilization times are appropriate ndash optimized
bull Integration time is appropriate for the expected concentration
ndash Use a longer integration time at low concentrations
bull Rinse time is appropriate
bull Use ldquoISISrdquo discrete sampling for faster measurement and faster washout
34
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Handles tough sample matrices better
than any other ICP-MS
ndash Highest plasma temperature (lowest
CeOCe) as standard
ndash HMI (high matrix introduction) allows direct
analysis of difficult samples
eg sea water
bull ORS3 operates in He collision mode to
remove ALL polyatomic interferences
ndash Enables reliable removal of all polyatomic
interferences using a single set of
conditions
ndash Gives lower levels of interference and
better long-term stability HMI gives lower suppression and
better long-term stability
Relative signal (suppression) in undiluted seawater
Long-term stability in undiluted seawater
35
Agilent ICP-MS Performance - Benefits
Best matrix tolerance amp less interferences
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS ndash Recommended Maintenance Schedule
ICP-MS Maintenance amp Trouble Shooting
May 2012 37
These functions
(and more) are
completed as part
of a Preventative
Maintenance
program by an
Agilent Field
Service Engineer
Summary ndash Key Consumables for ICP-MS
Sample preparationpresentation
ndash Peristaltic pump tubing
ndash Transfer and drain tubing
ndash ICP-MS standard solutions
ndash Internal Standard solutions
ndash Torches
ndash Spray chambers
ndash Nebulizers
Ion Extraction
ndash Sampler and skimmer cones
Autosampling
ndash Sample tubes racks probes and transfer tubing
ISIS
ndash Peristaltic pump tubing ferrules amp fittings
38
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sample Introduction
Key consumables requiring frequent replacement
bull Pump tubing
bull Torches and quartz transfer tube
bull Nebulizers
bull Spray chambers
bull Interface cones (skimmer amp sampler)
bull Transfer amp connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalogue
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24406(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 39
Autosampler Supplies
Key consumables requiring frequent replacement
ndash Peristaltic pump tubing
ndash Sample racks
ndash Sample tubes
ndash Spare probes
ndash Standard racks
ndash Connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24407(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 40
ISIS Supplies
Key consumables requiring frequent replacement
bull Peristaltic pump tubing
bull Ferrules and fittings
bull Valving
For ISIS Hydride Generation Accessory
bull Membrane filter
bull Concentric nebulizer
bull Gas-liquid separator
bull Other tubing and connectors
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceProductListingaspxcat=SubCat2ECS_24437(Agilent)amppcat=SubCat1ECS_24407(Agilent)amprcat=ClassECS_22674(Agilent)
41
ICP-MS Maintenance amp Trouble Shooting
May 2012
Where to Find the Right Consumable Analytical Consumables Agilent Assist
Consumables amp Supplies Instrument Sales ampServices 1-800-227-9770 (Option 11) 1-800-227-9770 (Option 13) wwwagilentcomchemcontactus wwwagilentcomchemcontactus
On-Line resources
ICP-MS Supplies
2nd Edition Speciation Handbook
ICP-MS Journal Archives
Recorded Agilent e-Seminars
ICP-OES Supplies
Atomic Absorption Supplies
Instrument Parts amp Supplies
Atomic Spec Application Notes
Agilent Quick Reference Guide for 77008800 ICP-MS (pub 5990-8182EN)
Agilent Atomic Spec Supplies Catalogue (pub 5990-8767EN)
Agilent Consumables Catalogue (pub 5990-6674EN)
Instrument User Manuals
42
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
PFA spray
chamber
PFA
endcap
PFA
nebulizer
PFA
connector
tube
Quartz torch with sapphire
or platinum injector
Complete sample introduction can be
changed to a system specifically
designed to reduce contamination
bull Usually used for semi-con applications
Clean integrated Auto-Sampler ndash I-AS
Clean sample introduction system - PFA
16
Cleanliness ndash The Ultimate for Contamination Free
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sensitivity ndash System Cleanliness
What to Check
ndash Sample Introduction System
bull Deposits in nebulizer can reduce
sample uptake rate
ndash Soak in aqua regia or use a nebulizer
cleaning tool to back flush
bull Solid material in torch injector
affects aerosol introduction into
plasma and increases noise
bull Contamination in spray chamber
impacts on aerosol formation ndash
increases noise
bull If seeing poor precision may be
due to beading in spray chamber
ndash Soak in 25 detergent solution
overnight (preferably for 24 hours)
17
ICP-MS Maintenance amp Trouble Shooting
May 2012
Nebulizer cleaner
Agilent PN G3266-80020
ICP-MS Sensitivity ndash System Cleanliness
What to Check
ndash Interface cones
bull Deposits or discoloration indicates
cleaning is required
bull Other indicators that cone cleaning
is required
ndash Poor sensitivity
ndash High background
ndash Distorted peak shapes
ndash Changes in interface vacuum reading
(deposition or build-up)
18
ICP-MS Maintenance amp Trouble Shooting
May 2012
Close up
Sample cone after measuring 75 undiluted sea water
samples using HMI Some deposition on outer edges
away from the orifice ndash no blockage of the sampling
orifice ndash but cleaning still recommended
System Cleanliness - Sampling Cone
1 mm Orifice Nickel or Platinum Centres
bull Nickel
bull Physically stronger
bull Tip runs hotter ndash less sample deposition
bull Platinum
bull Chemically stronger
bull Used for higher acid conc (incl HF)
bull 2 centre sizes 10-18 mm
bull Higher cost
Potential Problems
bull Biggest risk is physical damage to the orifice due to excessively aggressive cleaning
bull Cones also affected by sample matrix (acid strength amp type) and number of samples analyzed each day
bull Nickel - Typically replace 3 or 5 each year (assumes measuring 250-350 environmental samples each day)
bull Platinum - Typically replace 1 or 2 each year (assumes measuring 20-50 semiconductor samples each day)
bull If not clean then can result in analytical problems eg poor signal stability elemental contamination
ICP-MS Maintenance amp Trouble Shooting
May 2012 19
System Cleanliness - Skimmer Cone
04 mm Orifice Nickel or Platinum
bull The Nickel skimmer cone is the standard interface
bull The skimmer cone is relatively robust to samples containing high concentrations of matrix and salts and is suitable for a wide variety of samples It is usually used with the Nickel sampling cone
bull The Platinum skimmer cone is usually used for introduction of hydrofluoric acid and other reagents It is usually used with the Platinum sampling cone
Potential Problems
bull Biggest risk is from physical damage to the orifice due to excessively aggressive cleaning
bull Cones also affected by sample matrix (acid strength amp type) and number of samples analyzed each day
bull Nickel ndash Typically replace 3 or 5 each year (assumes measuring 250-350 environmental samples each day)
bull Platinum ndash Typically replace 1 or 2 each year (assumes measuring 20-50 semiconductor samples each day)
bull If not clean then can result in analytical problems eg poor signal stability elemental contamination
20
ICP-MS Maintenance amp Trouble Shooting
May 2012
System Cleanliness - Cone Cleaning Procedure
Caution - Take care to avoid damage to the cone tip when removing ndash and place base down - Check the graphite gasket and replace if creased or damaged - Sonicate in a 2 Citranox or 2 Nitric Acid solution for a few minutes - Rinse well with de-ionized water - If still dirty or memory problems remain polish using an alumina powder slurry on a Q-tip then sonicate in 2 Citranox solution and rinse well with de-ionized water - Dry with nitrogen before installing
22
ICP-MS Maintenance amp Trouble Shooting
May 2012
Precision - Why is This Important
What does ldquoPrecisionrdquo mean
ndash Ability to get the same result for the same
sample when measured multiple times
ndash Usually measured as RSD or sometimes SD
RSD = (SD Mean Result) 100
ndash Low values indicate good precision
bull For ICP-MS expect 1-2 RSD
Why is this important
ndash User loses confidence in the system
What impacts on precision
ndash Nebulizerplasma stability
ndash Sample introduction system
ndash Method parameters
23
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash System stabilized
bull Allow 10 mins for plasma warm-up before
analysis
ndash Plasma status
bull ldquoBulletrdquo in the plasma should be stable
bull Check for deposits in the injector of the torch
ndash Check condition of interface cones and
clean if necessary
ndash Clean the Extraction Lens - Omega Lens
assembly
ndash Method parameters
bull Appropriate times set for sample uptake
delay and stabilization times
24
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash Sample Intro
What to Check ndash Nebulizer
bull Nebulizer type used can impact on sensitivity and precision
ndash MicroMist (glass concentric type) is the standard nebulizer ndash handles most sample
types
ndash PFA MicroFlow nebulizer best for low volume samples aggressive samples (HF
digests) and when low contamination required (semi-con)
ndash Babington gives poorer precision - best for high TDS samples
bull Check nebulizer condition regularly
ndash Chips in the nebulizer tip impact on aerosol formation ndash poor precision
(use a magnifying glass if necessary)
ndash Check for deposits or blockage in the tip
bull Sample uptake or flow rate
ndash Lower pump speed or using narrow bore pump tubing will reduce uptake rate
- better for high TDS samples
25
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Sample Introduction bull Contamination in the spray chamber
ndash When was the spray chamber cleaned
bull Any blockages in the nebulizer injector
ndash Check for stable aerosol formation
bull Air leaks in spray chamber end cap or connecting tubes
ndash Are they in good condition with tight connections
bull Damaged pump tubes
ndash When did you check the pump tubes
bull Is the pump speed too slow
ndash Low pump speeds may cause signal pulsation
ndash If required use narrower bore pump tube and increase pump speed
bull Samples have a high TDS content
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
26
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Memory effects
bull If possible avoid running high concentrations of these analytes
(Ag Au B Hg Mo Si Sn W Zn Zr)
ndash Maybe necessary to pre-dilute samples (if known to be high in concentration)
bull Ensure an adequate rinse time
ndash Should be at least equal to the sample uptake delay
(30-40 seconds typical)
bull May require an acidified rinse solution between samples
(2 HNO3)
bull Other strategies to minimize memory effects
ndash Use an inert spray chamber
ndash Use the ISIS to introduce discrete amounts of sample This means
bull Cones are exposed to less sample matrix = improved stability
bull Less memorycarry-over
bull Reduced uptake amp rinse times = faster measurement
27
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy - Why is This Important
What does ldquoAccuracyrdquo mean
ndash Ability to get the ldquorightrdquo answer for the sample
ndash Heavily dependent on operatorrsquos skill
Why is this important
ndash User loses confidence in the system
ndash Your reputationhellip
bull Customerrsquos question the results
bull Poor performance in ldquoround robinrdquo comparisons
How do You Confirm Accuracy
ndash Check the result for a prepared standard
ndash Measure a certified reference material
ndash Use other quality control checks to check analysis
28
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Calibration standards properly prepared
bull See earlier recommendations ndash important to match to samples prepare
accurately and use them ldquofreshrdquo
ndash Any interferences impacting on results
ndash Use matched standards or standard additions
ndash Ensure isotope selected has no polyatomic interferences
ndash If necessary use ORS3
ndash Precision optimized
bull Optimum signal to noise performance improves accuracy
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
29
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Reprocess data post
run using an
alternate internal
standard
bull Ensure Internal
Standard used is
similar in mass
bull Check whether the
Internal Standard is
present in the
sample
ndash If necessary do a Semi-
Quant measurement
bull Dilute with cal blk
matrix
30
Accuracy ndash Suspect Internal Standard Recovery
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Sample preparation
bull Is the most appropriate digestion being used
bull Are all of the analytes being quantitatively (and reproducibly) extracted and
dissolved
ndash Many digestions are only partial extracts ndash efficiency will vary with the
sample matrix
ndash Some volatile analytes may be ldquolostrdquo during digestion
bull Confirm by taking a solid certified reference material
through your preparation and analysis procedure
bull Is the digest stable ndash or are you seeing any precipitates or a suspension
bull Do you see any potential contamination from either reagents or the digestion
equipment eg especially with Si B or Ca
bull Include a ldquoReagent Blankrdquo with every sample batch to
monitor
31
ICP-MS Maintenance amp Trouble Shooting
May 2012
Laboratory environment can have
direct impact on quality of results
bull Clean uncluttered work area
bull Proper ventilation
bull Safety considerations
bull Instrument lifetime consideration
ICP-MS Maintenance amp Trouble Shooting
May 2012 32
Laboratory Environment
ICP-MS ndash Potential Autosampler Issues
ndash More customers use autosamplers with ICP for automation
ndash Issues to consider
bull Long transfer tube between sampler and ICP-MS
ndash May need to program a longer sample uptake delay
ndash May exacerbate problems with memory effects
ndash Use ldquoFast Pumprdquo during sample uptake delay
bull Caution ndash not always possible
Not recommended with high TDS samples and organics
bull Ensure probe diameter is appropriate for sample matrix
ndash Use wider bore for high TDS or viscous samples
bull Sample stability - potential for sample changes while uncovered in racks ndash impacts accuracy
ndash Dust ingress can introduce contamination
ndash Sample evaporation may occur during long unattended runs
ndash Sediment in the sample may settle out esp with wear metals or suspensions
bull Ensure transfer line to ICP-MS is in good condition
ndash Kinks in the line may cause poor uptake or pulsing in the sample
ndash Impacts on precision and accuracy
33
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sample Throughput ndash What to Check
ndash Samples fully digested
bull No excess particulates in the sample that may cause blockage
ndash Sample Introduction System optimized
ndash Capable of handling the TDS levels in the sample
ndash TorchNebulizer cleaned and ready for analysis
ndash Method parameters optimized
bull Sample uptake delay and stabilization times are appropriate ndash optimized
bull Integration time is appropriate for the expected concentration
ndash Use a longer integration time at low concentrations
bull Rinse time is appropriate
bull Use ldquoISISrdquo discrete sampling for faster measurement and faster washout
34
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Handles tough sample matrices better
than any other ICP-MS
ndash Highest plasma temperature (lowest
CeOCe) as standard
ndash HMI (high matrix introduction) allows direct
analysis of difficult samples
eg sea water
bull ORS3 operates in He collision mode to
remove ALL polyatomic interferences
ndash Enables reliable removal of all polyatomic
interferences using a single set of
conditions
ndash Gives lower levels of interference and
better long-term stability HMI gives lower suppression and
better long-term stability
Relative signal (suppression) in undiluted seawater
Long-term stability in undiluted seawater
35
Agilent ICP-MS Performance - Benefits
Best matrix tolerance amp less interferences
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS ndash Recommended Maintenance Schedule
ICP-MS Maintenance amp Trouble Shooting
May 2012 37
These functions
(and more) are
completed as part
of a Preventative
Maintenance
program by an
Agilent Field
Service Engineer
Summary ndash Key Consumables for ICP-MS
Sample preparationpresentation
ndash Peristaltic pump tubing
ndash Transfer and drain tubing
ndash ICP-MS standard solutions
ndash Internal Standard solutions
ndash Torches
ndash Spray chambers
ndash Nebulizers
Ion Extraction
ndash Sampler and skimmer cones
Autosampling
ndash Sample tubes racks probes and transfer tubing
ISIS
ndash Peristaltic pump tubing ferrules amp fittings
38
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sample Introduction
Key consumables requiring frequent replacement
bull Pump tubing
bull Torches and quartz transfer tube
bull Nebulizers
bull Spray chambers
bull Interface cones (skimmer amp sampler)
bull Transfer amp connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalogue
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24406(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 39
Autosampler Supplies
Key consumables requiring frequent replacement
ndash Peristaltic pump tubing
ndash Sample racks
ndash Sample tubes
ndash Spare probes
ndash Standard racks
ndash Connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24407(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 40
ISIS Supplies
Key consumables requiring frequent replacement
bull Peristaltic pump tubing
bull Ferrules and fittings
bull Valving
For ISIS Hydride Generation Accessory
bull Membrane filter
bull Concentric nebulizer
bull Gas-liquid separator
bull Other tubing and connectors
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceProductListingaspxcat=SubCat2ECS_24437(Agilent)amppcat=SubCat1ECS_24407(Agilent)amprcat=ClassECS_22674(Agilent)
41
ICP-MS Maintenance amp Trouble Shooting
May 2012
Where to Find the Right Consumable Analytical Consumables Agilent Assist
Consumables amp Supplies Instrument Sales ampServices 1-800-227-9770 (Option 11) 1-800-227-9770 (Option 13) wwwagilentcomchemcontactus wwwagilentcomchemcontactus
On-Line resources
ICP-MS Supplies
2nd Edition Speciation Handbook
ICP-MS Journal Archives
Recorded Agilent e-Seminars
ICP-OES Supplies
Atomic Absorption Supplies
Instrument Parts amp Supplies
Atomic Spec Application Notes
Agilent Quick Reference Guide for 77008800 ICP-MS (pub 5990-8182EN)
Agilent Atomic Spec Supplies Catalogue (pub 5990-8767EN)
Agilent Consumables Catalogue (pub 5990-6674EN)
Instrument User Manuals
42
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sensitivity ndash System Cleanliness
What to Check
ndash Sample Introduction System
bull Deposits in nebulizer can reduce
sample uptake rate
ndash Soak in aqua regia or use a nebulizer
cleaning tool to back flush
bull Solid material in torch injector
affects aerosol introduction into
plasma and increases noise
bull Contamination in spray chamber
impacts on aerosol formation ndash
increases noise
bull If seeing poor precision may be
due to beading in spray chamber
ndash Soak in 25 detergent solution
overnight (preferably for 24 hours)
17
ICP-MS Maintenance amp Trouble Shooting
May 2012
Nebulizer cleaner
Agilent PN G3266-80020
ICP-MS Sensitivity ndash System Cleanliness
What to Check
ndash Interface cones
bull Deposits or discoloration indicates
cleaning is required
bull Other indicators that cone cleaning
is required
ndash Poor sensitivity
ndash High background
ndash Distorted peak shapes
ndash Changes in interface vacuum reading
(deposition or build-up)
18
ICP-MS Maintenance amp Trouble Shooting
May 2012
Close up
Sample cone after measuring 75 undiluted sea water
samples using HMI Some deposition on outer edges
away from the orifice ndash no blockage of the sampling
orifice ndash but cleaning still recommended
System Cleanliness - Sampling Cone
1 mm Orifice Nickel or Platinum Centres
bull Nickel
bull Physically stronger
bull Tip runs hotter ndash less sample deposition
bull Platinum
bull Chemically stronger
bull Used for higher acid conc (incl HF)
bull 2 centre sizes 10-18 mm
bull Higher cost
Potential Problems
bull Biggest risk is physical damage to the orifice due to excessively aggressive cleaning
bull Cones also affected by sample matrix (acid strength amp type) and number of samples analyzed each day
bull Nickel - Typically replace 3 or 5 each year (assumes measuring 250-350 environmental samples each day)
bull Platinum - Typically replace 1 or 2 each year (assumes measuring 20-50 semiconductor samples each day)
bull If not clean then can result in analytical problems eg poor signal stability elemental contamination
ICP-MS Maintenance amp Trouble Shooting
May 2012 19
System Cleanliness - Skimmer Cone
04 mm Orifice Nickel or Platinum
bull The Nickel skimmer cone is the standard interface
bull The skimmer cone is relatively robust to samples containing high concentrations of matrix and salts and is suitable for a wide variety of samples It is usually used with the Nickel sampling cone
bull The Platinum skimmer cone is usually used for introduction of hydrofluoric acid and other reagents It is usually used with the Platinum sampling cone
Potential Problems
bull Biggest risk is from physical damage to the orifice due to excessively aggressive cleaning
bull Cones also affected by sample matrix (acid strength amp type) and number of samples analyzed each day
bull Nickel ndash Typically replace 3 or 5 each year (assumes measuring 250-350 environmental samples each day)
bull Platinum ndash Typically replace 1 or 2 each year (assumes measuring 20-50 semiconductor samples each day)
bull If not clean then can result in analytical problems eg poor signal stability elemental contamination
20
ICP-MS Maintenance amp Trouble Shooting
May 2012
System Cleanliness - Cone Cleaning Procedure
Caution - Take care to avoid damage to the cone tip when removing ndash and place base down - Check the graphite gasket and replace if creased or damaged - Sonicate in a 2 Citranox or 2 Nitric Acid solution for a few minutes - Rinse well with de-ionized water - If still dirty or memory problems remain polish using an alumina powder slurry on a Q-tip then sonicate in 2 Citranox solution and rinse well with de-ionized water - Dry with nitrogen before installing
22
ICP-MS Maintenance amp Trouble Shooting
May 2012
Precision - Why is This Important
What does ldquoPrecisionrdquo mean
ndash Ability to get the same result for the same
sample when measured multiple times
ndash Usually measured as RSD or sometimes SD
RSD = (SD Mean Result) 100
ndash Low values indicate good precision
bull For ICP-MS expect 1-2 RSD
Why is this important
ndash User loses confidence in the system
What impacts on precision
ndash Nebulizerplasma stability
ndash Sample introduction system
ndash Method parameters
23
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash System stabilized
bull Allow 10 mins for plasma warm-up before
analysis
ndash Plasma status
bull ldquoBulletrdquo in the plasma should be stable
bull Check for deposits in the injector of the torch
ndash Check condition of interface cones and
clean if necessary
ndash Clean the Extraction Lens - Omega Lens
assembly
ndash Method parameters
bull Appropriate times set for sample uptake
delay and stabilization times
24
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash Sample Intro
What to Check ndash Nebulizer
bull Nebulizer type used can impact on sensitivity and precision
ndash MicroMist (glass concentric type) is the standard nebulizer ndash handles most sample
types
ndash PFA MicroFlow nebulizer best for low volume samples aggressive samples (HF
digests) and when low contamination required (semi-con)
ndash Babington gives poorer precision - best for high TDS samples
bull Check nebulizer condition regularly
ndash Chips in the nebulizer tip impact on aerosol formation ndash poor precision
(use a magnifying glass if necessary)
ndash Check for deposits or blockage in the tip
bull Sample uptake or flow rate
ndash Lower pump speed or using narrow bore pump tubing will reduce uptake rate
- better for high TDS samples
25
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Sample Introduction bull Contamination in the spray chamber
ndash When was the spray chamber cleaned
bull Any blockages in the nebulizer injector
ndash Check for stable aerosol formation
bull Air leaks in spray chamber end cap or connecting tubes
ndash Are they in good condition with tight connections
bull Damaged pump tubes
ndash When did you check the pump tubes
bull Is the pump speed too slow
ndash Low pump speeds may cause signal pulsation
ndash If required use narrower bore pump tube and increase pump speed
bull Samples have a high TDS content
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
26
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Memory effects
bull If possible avoid running high concentrations of these analytes
(Ag Au B Hg Mo Si Sn W Zn Zr)
ndash Maybe necessary to pre-dilute samples (if known to be high in concentration)
bull Ensure an adequate rinse time
ndash Should be at least equal to the sample uptake delay
(30-40 seconds typical)
bull May require an acidified rinse solution between samples
(2 HNO3)
bull Other strategies to minimize memory effects
ndash Use an inert spray chamber
ndash Use the ISIS to introduce discrete amounts of sample This means
bull Cones are exposed to less sample matrix = improved stability
bull Less memorycarry-over
bull Reduced uptake amp rinse times = faster measurement
27
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy - Why is This Important
What does ldquoAccuracyrdquo mean
ndash Ability to get the ldquorightrdquo answer for the sample
ndash Heavily dependent on operatorrsquos skill
Why is this important
ndash User loses confidence in the system
ndash Your reputationhellip
bull Customerrsquos question the results
bull Poor performance in ldquoround robinrdquo comparisons
How do You Confirm Accuracy
ndash Check the result for a prepared standard
ndash Measure a certified reference material
ndash Use other quality control checks to check analysis
28
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Calibration standards properly prepared
bull See earlier recommendations ndash important to match to samples prepare
accurately and use them ldquofreshrdquo
ndash Any interferences impacting on results
ndash Use matched standards or standard additions
ndash Ensure isotope selected has no polyatomic interferences
ndash If necessary use ORS3
ndash Precision optimized
bull Optimum signal to noise performance improves accuracy
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
29
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Reprocess data post
run using an
alternate internal
standard
bull Ensure Internal
Standard used is
similar in mass
bull Check whether the
Internal Standard is
present in the
sample
ndash If necessary do a Semi-
Quant measurement
bull Dilute with cal blk
matrix
30
Accuracy ndash Suspect Internal Standard Recovery
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Sample preparation
bull Is the most appropriate digestion being used
bull Are all of the analytes being quantitatively (and reproducibly) extracted and
dissolved
ndash Many digestions are only partial extracts ndash efficiency will vary with the
sample matrix
ndash Some volatile analytes may be ldquolostrdquo during digestion
bull Confirm by taking a solid certified reference material
through your preparation and analysis procedure
bull Is the digest stable ndash or are you seeing any precipitates or a suspension
bull Do you see any potential contamination from either reagents or the digestion
equipment eg especially with Si B or Ca
bull Include a ldquoReagent Blankrdquo with every sample batch to
monitor
31
ICP-MS Maintenance amp Trouble Shooting
May 2012
Laboratory environment can have
direct impact on quality of results
bull Clean uncluttered work area
bull Proper ventilation
bull Safety considerations
bull Instrument lifetime consideration
ICP-MS Maintenance amp Trouble Shooting
May 2012 32
Laboratory Environment
ICP-MS ndash Potential Autosampler Issues
ndash More customers use autosamplers with ICP for automation
ndash Issues to consider
bull Long transfer tube between sampler and ICP-MS
ndash May need to program a longer sample uptake delay
ndash May exacerbate problems with memory effects
ndash Use ldquoFast Pumprdquo during sample uptake delay
bull Caution ndash not always possible
Not recommended with high TDS samples and organics
bull Ensure probe diameter is appropriate for sample matrix
ndash Use wider bore for high TDS or viscous samples
bull Sample stability - potential for sample changes while uncovered in racks ndash impacts accuracy
ndash Dust ingress can introduce contamination
ndash Sample evaporation may occur during long unattended runs
ndash Sediment in the sample may settle out esp with wear metals or suspensions
bull Ensure transfer line to ICP-MS is in good condition
ndash Kinks in the line may cause poor uptake or pulsing in the sample
ndash Impacts on precision and accuracy
33
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sample Throughput ndash What to Check
ndash Samples fully digested
bull No excess particulates in the sample that may cause blockage
ndash Sample Introduction System optimized
ndash Capable of handling the TDS levels in the sample
ndash TorchNebulizer cleaned and ready for analysis
ndash Method parameters optimized
bull Sample uptake delay and stabilization times are appropriate ndash optimized
bull Integration time is appropriate for the expected concentration
ndash Use a longer integration time at low concentrations
bull Rinse time is appropriate
bull Use ldquoISISrdquo discrete sampling for faster measurement and faster washout
34
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Handles tough sample matrices better
than any other ICP-MS
ndash Highest plasma temperature (lowest
CeOCe) as standard
ndash HMI (high matrix introduction) allows direct
analysis of difficult samples
eg sea water
bull ORS3 operates in He collision mode to
remove ALL polyatomic interferences
ndash Enables reliable removal of all polyatomic
interferences using a single set of
conditions
ndash Gives lower levels of interference and
better long-term stability HMI gives lower suppression and
better long-term stability
Relative signal (suppression) in undiluted seawater
Long-term stability in undiluted seawater
35
Agilent ICP-MS Performance - Benefits
Best matrix tolerance amp less interferences
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS ndash Recommended Maintenance Schedule
ICP-MS Maintenance amp Trouble Shooting
May 2012 37
These functions
(and more) are
completed as part
of a Preventative
Maintenance
program by an
Agilent Field
Service Engineer
Summary ndash Key Consumables for ICP-MS
Sample preparationpresentation
ndash Peristaltic pump tubing
ndash Transfer and drain tubing
ndash ICP-MS standard solutions
ndash Internal Standard solutions
ndash Torches
ndash Spray chambers
ndash Nebulizers
Ion Extraction
ndash Sampler and skimmer cones
Autosampling
ndash Sample tubes racks probes and transfer tubing
ISIS
ndash Peristaltic pump tubing ferrules amp fittings
38
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sample Introduction
Key consumables requiring frequent replacement
bull Pump tubing
bull Torches and quartz transfer tube
bull Nebulizers
bull Spray chambers
bull Interface cones (skimmer amp sampler)
bull Transfer amp connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalogue
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24406(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 39
Autosampler Supplies
Key consumables requiring frequent replacement
ndash Peristaltic pump tubing
ndash Sample racks
ndash Sample tubes
ndash Spare probes
ndash Standard racks
ndash Connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24407(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 40
ISIS Supplies
Key consumables requiring frequent replacement
bull Peristaltic pump tubing
bull Ferrules and fittings
bull Valving
For ISIS Hydride Generation Accessory
bull Membrane filter
bull Concentric nebulizer
bull Gas-liquid separator
bull Other tubing and connectors
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceProductListingaspxcat=SubCat2ECS_24437(Agilent)amppcat=SubCat1ECS_24407(Agilent)amprcat=ClassECS_22674(Agilent)
41
ICP-MS Maintenance amp Trouble Shooting
May 2012
Where to Find the Right Consumable Analytical Consumables Agilent Assist
Consumables amp Supplies Instrument Sales ampServices 1-800-227-9770 (Option 11) 1-800-227-9770 (Option 13) wwwagilentcomchemcontactus wwwagilentcomchemcontactus
On-Line resources
ICP-MS Supplies
2nd Edition Speciation Handbook
ICP-MS Journal Archives
Recorded Agilent e-Seminars
ICP-OES Supplies
Atomic Absorption Supplies
Instrument Parts amp Supplies
Atomic Spec Application Notes
Agilent Quick Reference Guide for 77008800 ICP-MS (pub 5990-8182EN)
Agilent Atomic Spec Supplies Catalogue (pub 5990-8767EN)
Agilent Consumables Catalogue (pub 5990-6674EN)
Instrument User Manuals
42
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sensitivity ndash System Cleanliness
What to Check
ndash Interface cones
bull Deposits or discoloration indicates
cleaning is required
bull Other indicators that cone cleaning
is required
ndash Poor sensitivity
ndash High background
ndash Distorted peak shapes
ndash Changes in interface vacuum reading
(deposition or build-up)
18
ICP-MS Maintenance amp Trouble Shooting
May 2012
Close up
Sample cone after measuring 75 undiluted sea water
samples using HMI Some deposition on outer edges
away from the orifice ndash no blockage of the sampling
orifice ndash but cleaning still recommended
System Cleanliness - Sampling Cone
1 mm Orifice Nickel or Platinum Centres
bull Nickel
bull Physically stronger
bull Tip runs hotter ndash less sample deposition
bull Platinum
bull Chemically stronger
bull Used for higher acid conc (incl HF)
bull 2 centre sizes 10-18 mm
bull Higher cost
Potential Problems
bull Biggest risk is physical damage to the orifice due to excessively aggressive cleaning
bull Cones also affected by sample matrix (acid strength amp type) and number of samples analyzed each day
bull Nickel - Typically replace 3 or 5 each year (assumes measuring 250-350 environmental samples each day)
bull Platinum - Typically replace 1 or 2 each year (assumes measuring 20-50 semiconductor samples each day)
bull If not clean then can result in analytical problems eg poor signal stability elemental contamination
ICP-MS Maintenance amp Trouble Shooting
May 2012 19
System Cleanliness - Skimmer Cone
04 mm Orifice Nickel or Platinum
bull The Nickel skimmer cone is the standard interface
bull The skimmer cone is relatively robust to samples containing high concentrations of matrix and salts and is suitable for a wide variety of samples It is usually used with the Nickel sampling cone
bull The Platinum skimmer cone is usually used for introduction of hydrofluoric acid and other reagents It is usually used with the Platinum sampling cone
Potential Problems
bull Biggest risk is from physical damage to the orifice due to excessively aggressive cleaning
bull Cones also affected by sample matrix (acid strength amp type) and number of samples analyzed each day
bull Nickel ndash Typically replace 3 or 5 each year (assumes measuring 250-350 environmental samples each day)
bull Platinum ndash Typically replace 1 or 2 each year (assumes measuring 20-50 semiconductor samples each day)
bull If not clean then can result in analytical problems eg poor signal stability elemental contamination
20
ICP-MS Maintenance amp Trouble Shooting
May 2012
System Cleanliness - Cone Cleaning Procedure
Caution - Take care to avoid damage to the cone tip when removing ndash and place base down - Check the graphite gasket and replace if creased or damaged - Sonicate in a 2 Citranox or 2 Nitric Acid solution for a few minutes - Rinse well with de-ionized water - If still dirty or memory problems remain polish using an alumina powder slurry on a Q-tip then sonicate in 2 Citranox solution and rinse well with de-ionized water - Dry with nitrogen before installing
22
ICP-MS Maintenance amp Trouble Shooting
May 2012
Precision - Why is This Important
What does ldquoPrecisionrdquo mean
ndash Ability to get the same result for the same
sample when measured multiple times
ndash Usually measured as RSD or sometimes SD
RSD = (SD Mean Result) 100
ndash Low values indicate good precision
bull For ICP-MS expect 1-2 RSD
Why is this important
ndash User loses confidence in the system
What impacts on precision
ndash Nebulizerplasma stability
ndash Sample introduction system
ndash Method parameters
23
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash System stabilized
bull Allow 10 mins for plasma warm-up before
analysis
ndash Plasma status
bull ldquoBulletrdquo in the plasma should be stable
bull Check for deposits in the injector of the torch
ndash Check condition of interface cones and
clean if necessary
ndash Clean the Extraction Lens - Omega Lens
assembly
ndash Method parameters
bull Appropriate times set for sample uptake
delay and stabilization times
24
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash Sample Intro
What to Check ndash Nebulizer
bull Nebulizer type used can impact on sensitivity and precision
ndash MicroMist (glass concentric type) is the standard nebulizer ndash handles most sample
types
ndash PFA MicroFlow nebulizer best for low volume samples aggressive samples (HF
digests) and when low contamination required (semi-con)
ndash Babington gives poorer precision - best for high TDS samples
bull Check nebulizer condition regularly
ndash Chips in the nebulizer tip impact on aerosol formation ndash poor precision
(use a magnifying glass if necessary)
ndash Check for deposits or blockage in the tip
bull Sample uptake or flow rate
ndash Lower pump speed or using narrow bore pump tubing will reduce uptake rate
- better for high TDS samples
25
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Sample Introduction bull Contamination in the spray chamber
ndash When was the spray chamber cleaned
bull Any blockages in the nebulizer injector
ndash Check for stable aerosol formation
bull Air leaks in spray chamber end cap or connecting tubes
ndash Are they in good condition with tight connections
bull Damaged pump tubes
ndash When did you check the pump tubes
bull Is the pump speed too slow
ndash Low pump speeds may cause signal pulsation
ndash If required use narrower bore pump tube and increase pump speed
bull Samples have a high TDS content
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
26
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Memory effects
bull If possible avoid running high concentrations of these analytes
(Ag Au B Hg Mo Si Sn W Zn Zr)
ndash Maybe necessary to pre-dilute samples (if known to be high in concentration)
bull Ensure an adequate rinse time
ndash Should be at least equal to the sample uptake delay
(30-40 seconds typical)
bull May require an acidified rinse solution between samples
(2 HNO3)
bull Other strategies to minimize memory effects
ndash Use an inert spray chamber
ndash Use the ISIS to introduce discrete amounts of sample This means
bull Cones are exposed to less sample matrix = improved stability
bull Less memorycarry-over
bull Reduced uptake amp rinse times = faster measurement
27
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy - Why is This Important
What does ldquoAccuracyrdquo mean
ndash Ability to get the ldquorightrdquo answer for the sample
ndash Heavily dependent on operatorrsquos skill
Why is this important
ndash User loses confidence in the system
ndash Your reputationhellip
bull Customerrsquos question the results
bull Poor performance in ldquoround robinrdquo comparisons
How do You Confirm Accuracy
ndash Check the result for a prepared standard
ndash Measure a certified reference material
ndash Use other quality control checks to check analysis
28
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Calibration standards properly prepared
bull See earlier recommendations ndash important to match to samples prepare
accurately and use them ldquofreshrdquo
ndash Any interferences impacting on results
ndash Use matched standards or standard additions
ndash Ensure isotope selected has no polyatomic interferences
ndash If necessary use ORS3
ndash Precision optimized
bull Optimum signal to noise performance improves accuracy
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
29
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Reprocess data post
run using an
alternate internal
standard
bull Ensure Internal
Standard used is
similar in mass
bull Check whether the
Internal Standard is
present in the
sample
ndash If necessary do a Semi-
Quant measurement
bull Dilute with cal blk
matrix
30
Accuracy ndash Suspect Internal Standard Recovery
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Sample preparation
bull Is the most appropriate digestion being used
bull Are all of the analytes being quantitatively (and reproducibly) extracted and
dissolved
ndash Many digestions are only partial extracts ndash efficiency will vary with the
sample matrix
ndash Some volatile analytes may be ldquolostrdquo during digestion
bull Confirm by taking a solid certified reference material
through your preparation and analysis procedure
bull Is the digest stable ndash or are you seeing any precipitates or a suspension
bull Do you see any potential contamination from either reagents or the digestion
equipment eg especially with Si B or Ca
bull Include a ldquoReagent Blankrdquo with every sample batch to
monitor
31
ICP-MS Maintenance amp Trouble Shooting
May 2012
Laboratory environment can have
direct impact on quality of results
bull Clean uncluttered work area
bull Proper ventilation
bull Safety considerations
bull Instrument lifetime consideration
ICP-MS Maintenance amp Trouble Shooting
May 2012 32
Laboratory Environment
ICP-MS ndash Potential Autosampler Issues
ndash More customers use autosamplers with ICP for automation
ndash Issues to consider
bull Long transfer tube between sampler and ICP-MS
ndash May need to program a longer sample uptake delay
ndash May exacerbate problems with memory effects
ndash Use ldquoFast Pumprdquo during sample uptake delay
bull Caution ndash not always possible
Not recommended with high TDS samples and organics
bull Ensure probe diameter is appropriate for sample matrix
ndash Use wider bore for high TDS or viscous samples
bull Sample stability - potential for sample changes while uncovered in racks ndash impacts accuracy
ndash Dust ingress can introduce contamination
ndash Sample evaporation may occur during long unattended runs
ndash Sediment in the sample may settle out esp with wear metals or suspensions
bull Ensure transfer line to ICP-MS is in good condition
ndash Kinks in the line may cause poor uptake or pulsing in the sample
ndash Impacts on precision and accuracy
33
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sample Throughput ndash What to Check
ndash Samples fully digested
bull No excess particulates in the sample that may cause blockage
ndash Sample Introduction System optimized
ndash Capable of handling the TDS levels in the sample
ndash TorchNebulizer cleaned and ready for analysis
ndash Method parameters optimized
bull Sample uptake delay and stabilization times are appropriate ndash optimized
bull Integration time is appropriate for the expected concentration
ndash Use a longer integration time at low concentrations
bull Rinse time is appropriate
bull Use ldquoISISrdquo discrete sampling for faster measurement and faster washout
34
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Handles tough sample matrices better
than any other ICP-MS
ndash Highest plasma temperature (lowest
CeOCe) as standard
ndash HMI (high matrix introduction) allows direct
analysis of difficult samples
eg sea water
bull ORS3 operates in He collision mode to
remove ALL polyatomic interferences
ndash Enables reliable removal of all polyatomic
interferences using a single set of
conditions
ndash Gives lower levels of interference and
better long-term stability HMI gives lower suppression and
better long-term stability
Relative signal (suppression) in undiluted seawater
Long-term stability in undiluted seawater
35
Agilent ICP-MS Performance - Benefits
Best matrix tolerance amp less interferences
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS ndash Recommended Maintenance Schedule
ICP-MS Maintenance amp Trouble Shooting
May 2012 37
These functions
(and more) are
completed as part
of a Preventative
Maintenance
program by an
Agilent Field
Service Engineer
Summary ndash Key Consumables for ICP-MS
Sample preparationpresentation
ndash Peristaltic pump tubing
ndash Transfer and drain tubing
ndash ICP-MS standard solutions
ndash Internal Standard solutions
ndash Torches
ndash Spray chambers
ndash Nebulizers
Ion Extraction
ndash Sampler and skimmer cones
Autosampling
ndash Sample tubes racks probes and transfer tubing
ISIS
ndash Peristaltic pump tubing ferrules amp fittings
38
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sample Introduction
Key consumables requiring frequent replacement
bull Pump tubing
bull Torches and quartz transfer tube
bull Nebulizers
bull Spray chambers
bull Interface cones (skimmer amp sampler)
bull Transfer amp connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalogue
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24406(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 39
Autosampler Supplies
Key consumables requiring frequent replacement
ndash Peristaltic pump tubing
ndash Sample racks
ndash Sample tubes
ndash Spare probes
ndash Standard racks
ndash Connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24407(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 40
ISIS Supplies
Key consumables requiring frequent replacement
bull Peristaltic pump tubing
bull Ferrules and fittings
bull Valving
For ISIS Hydride Generation Accessory
bull Membrane filter
bull Concentric nebulizer
bull Gas-liquid separator
bull Other tubing and connectors
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceProductListingaspxcat=SubCat2ECS_24437(Agilent)amppcat=SubCat1ECS_24407(Agilent)amprcat=ClassECS_22674(Agilent)
41
ICP-MS Maintenance amp Trouble Shooting
May 2012
Where to Find the Right Consumable Analytical Consumables Agilent Assist
Consumables amp Supplies Instrument Sales ampServices 1-800-227-9770 (Option 11) 1-800-227-9770 (Option 13) wwwagilentcomchemcontactus wwwagilentcomchemcontactus
On-Line resources
ICP-MS Supplies
2nd Edition Speciation Handbook
ICP-MS Journal Archives
Recorded Agilent e-Seminars
ICP-OES Supplies
Atomic Absorption Supplies
Instrument Parts amp Supplies
Atomic Spec Application Notes
Agilent Quick Reference Guide for 77008800 ICP-MS (pub 5990-8182EN)
Agilent Atomic Spec Supplies Catalogue (pub 5990-8767EN)
Agilent Consumables Catalogue (pub 5990-6674EN)
Instrument User Manuals
42
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
System Cleanliness - Sampling Cone
1 mm Orifice Nickel or Platinum Centres
bull Nickel
bull Physically stronger
bull Tip runs hotter ndash less sample deposition
bull Platinum
bull Chemically stronger
bull Used for higher acid conc (incl HF)
bull 2 centre sizes 10-18 mm
bull Higher cost
Potential Problems
bull Biggest risk is physical damage to the orifice due to excessively aggressive cleaning
bull Cones also affected by sample matrix (acid strength amp type) and number of samples analyzed each day
bull Nickel - Typically replace 3 or 5 each year (assumes measuring 250-350 environmental samples each day)
bull Platinum - Typically replace 1 or 2 each year (assumes measuring 20-50 semiconductor samples each day)
bull If not clean then can result in analytical problems eg poor signal stability elemental contamination
ICP-MS Maintenance amp Trouble Shooting
May 2012 19
System Cleanliness - Skimmer Cone
04 mm Orifice Nickel or Platinum
bull The Nickel skimmer cone is the standard interface
bull The skimmer cone is relatively robust to samples containing high concentrations of matrix and salts and is suitable for a wide variety of samples It is usually used with the Nickel sampling cone
bull The Platinum skimmer cone is usually used for introduction of hydrofluoric acid and other reagents It is usually used with the Platinum sampling cone
Potential Problems
bull Biggest risk is from physical damage to the orifice due to excessively aggressive cleaning
bull Cones also affected by sample matrix (acid strength amp type) and number of samples analyzed each day
bull Nickel ndash Typically replace 3 or 5 each year (assumes measuring 250-350 environmental samples each day)
bull Platinum ndash Typically replace 1 or 2 each year (assumes measuring 20-50 semiconductor samples each day)
bull If not clean then can result in analytical problems eg poor signal stability elemental contamination
20
ICP-MS Maintenance amp Trouble Shooting
May 2012
System Cleanliness - Cone Cleaning Procedure
Caution - Take care to avoid damage to the cone tip when removing ndash and place base down - Check the graphite gasket and replace if creased or damaged - Sonicate in a 2 Citranox or 2 Nitric Acid solution for a few minutes - Rinse well with de-ionized water - If still dirty or memory problems remain polish using an alumina powder slurry on a Q-tip then sonicate in 2 Citranox solution and rinse well with de-ionized water - Dry with nitrogen before installing
22
ICP-MS Maintenance amp Trouble Shooting
May 2012
Precision - Why is This Important
What does ldquoPrecisionrdquo mean
ndash Ability to get the same result for the same
sample when measured multiple times
ndash Usually measured as RSD or sometimes SD
RSD = (SD Mean Result) 100
ndash Low values indicate good precision
bull For ICP-MS expect 1-2 RSD
Why is this important
ndash User loses confidence in the system
What impacts on precision
ndash Nebulizerplasma stability
ndash Sample introduction system
ndash Method parameters
23
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash System stabilized
bull Allow 10 mins for plasma warm-up before
analysis
ndash Plasma status
bull ldquoBulletrdquo in the plasma should be stable
bull Check for deposits in the injector of the torch
ndash Check condition of interface cones and
clean if necessary
ndash Clean the Extraction Lens - Omega Lens
assembly
ndash Method parameters
bull Appropriate times set for sample uptake
delay and stabilization times
24
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash Sample Intro
What to Check ndash Nebulizer
bull Nebulizer type used can impact on sensitivity and precision
ndash MicroMist (glass concentric type) is the standard nebulizer ndash handles most sample
types
ndash PFA MicroFlow nebulizer best for low volume samples aggressive samples (HF
digests) and when low contamination required (semi-con)
ndash Babington gives poorer precision - best for high TDS samples
bull Check nebulizer condition regularly
ndash Chips in the nebulizer tip impact on aerosol formation ndash poor precision
(use a magnifying glass if necessary)
ndash Check for deposits or blockage in the tip
bull Sample uptake or flow rate
ndash Lower pump speed or using narrow bore pump tubing will reduce uptake rate
- better for high TDS samples
25
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Sample Introduction bull Contamination in the spray chamber
ndash When was the spray chamber cleaned
bull Any blockages in the nebulizer injector
ndash Check for stable aerosol formation
bull Air leaks in spray chamber end cap or connecting tubes
ndash Are they in good condition with tight connections
bull Damaged pump tubes
ndash When did you check the pump tubes
bull Is the pump speed too slow
ndash Low pump speeds may cause signal pulsation
ndash If required use narrower bore pump tube and increase pump speed
bull Samples have a high TDS content
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
26
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Memory effects
bull If possible avoid running high concentrations of these analytes
(Ag Au B Hg Mo Si Sn W Zn Zr)
ndash Maybe necessary to pre-dilute samples (if known to be high in concentration)
bull Ensure an adequate rinse time
ndash Should be at least equal to the sample uptake delay
(30-40 seconds typical)
bull May require an acidified rinse solution between samples
(2 HNO3)
bull Other strategies to minimize memory effects
ndash Use an inert spray chamber
ndash Use the ISIS to introduce discrete amounts of sample This means
bull Cones are exposed to less sample matrix = improved stability
bull Less memorycarry-over
bull Reduced uptake amp rinse times = faster measurement
27
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy - Why is This Important
What does ldquoAccuracyrdquo mean
ndash Ability to get the ldquorightrdquo answer for the sample
ndash Heavily dependent on operatorrsquos skill
Why is this important
ndash User loses confidence in the system
ndash Your reputationhellip
bull Customerrsquos question the results
bull Poor performance in ldquoround robinrdquo comparisons
How do You Confirm Accuracy
ndash Check the result for a prepared standard
ndash Measure a certified reference material
ndash Use other quality control checks to check analysis
28
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Calibration standards properly prepared
bull See earlier recommendations ndash important to match to samples prepare
accurately and use them ldquofreshrdquo
ndash Any interferences impacting on results
ndash Use matched standards or standard additions
ndash Ensure isotope selected has no polyatomic interferences
ndash If necessary use ORS3
ndash Precision optimized
bull Optimum signal to noise performance improves accuracy
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
29
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Reprocess data post
run using an
alternate internal
standard
bull Ensure Internal
Standard used is
similar in mass
bull Check whether the
Internal Standard is
present in the
sample
ndash If necessary do a Semi-
Quant measurement
bull Dilute with cal blk
matrix
30
Accuracy ndash Suspect Internal Standard Recovery
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Sample preparation
bull Is the most appropriate digestion being used
bull Are all of the analytes being quantitatively (and reproducibly) extracted and
dissolved
ndash Many digestions are only partial extracts ndash efficiency will vary with the
sample matrix
ndash Some volatile analytes may be ldquolostrdquo during digestion
bull Confirm by taking a solid certified reference material
through your preparation and analysis procedure
bull Is the digest stable ndash or are you seeing any precipitates or a suspension
bull Do you see any potential contamination from either reagents or the digestion
equipment eg especially with Si B or Ca
bull Include a ldquoReagent Blankrdquo with every sample batch to
monitor
31
ICP-MS Maintenance amp Trouble Shooting
May 2012
Laboratory environment can have
direct impact on quality of results
bull Clean uncluttered work area
bull Proper ventilation
bull Safety considerations
bull Instrument lifetime consideration
ICP-MS Maintenance amp Trouble Shooting
May 2012 32
Laboratory Environment
ICP-MS ndash Potential Autosampler Issues
ndash More customers use autosamplers with ICP for automation
ndash Issues to consider
bull Long transfer tube between sampler and ICP-MS
ndash May need to program a longer sample uptake delay
ndash May exacerbate problems with memory effects
ndash Use ldquoFast Pumprdquo during sample uptake delay
bull Caution ndash not always possible
Not recommended with high TDS samples and organics
bull Ensure probe diameter is appropriate for sample matrix
ndash Use wider bore for high TDS or viscous samples
bull Sample stability - potential for sample changes while uncovered in racks ndash impacts accuracy
ndash Dust ingress can introduce contamination
ndash Sample evaporation may occur during long unattended runs
ndash Sediment in the sample may settle out esp with wear metals or suspensions
bull Ensure transfer line to ICP-MS is in good condition
ndash Kinks in the line may cause poor uptake or pulsing in the sample
ndash Impacts on precision and accuracy
33
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sample Throughput ndash What to Check
ndash Samples fully digested
bull No excess particulates in the sample that may cause blockage
ndash Sample Introduction System optimized
ndash Capable of handling the TDS levels in the sample
ndash TorchNebulizer cleaned and ready for analysis
ndash Method parameters optimized
bull Sample uptake delay and stabilization times are appropriate ndash optimized
bull Integration time is appropriate for the expected concentration
ndash Use a longer integration time at low concentrations
bull Rinse time is appropriate
bull Use ldquoISISrdquo discrete sampling for faster measurement and faster washout
34
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Handles tough sample matrices better
than any other ICP-MS
ndash Highest plasma temperature (lowest
CeOCe) as standard
ndash HMI (high matrix introduction) allows direct
analysis of difficult samples
eg sea water
bull ORS3 operates in He collision mode to
remove ALL polyatomic interferences
ndash Enables reliable removal of all polyatomic
interferences using a single set of
conditions
ndash Gives lower levels of interference and
better long-term stability HMI gives lower suppression and
better long-term stability
Relative signal (suppression) in undiluted seawater
Long-term stability in undiluted seawater
35
Agilent ICP-MS Performance - Benefits
Best matrix tolerance amp less interferences
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS ndash Recommended Maintenance Schedule
ICP-MS Maintenance amp Trouble Shooting
May 2012 37
These functions
(and more) are
completed as part
of a Preventative
Maintenance
program by an
Agilent Field
Service Engineer
Summary ndash Key Consumables for ICP-MS
Sample preparationpresentation
ndash Peristaltic pump tubing
ndash Transfer and drain tubing
ndash ICP-MS standard solutions
ndash Internal Standard solutions
ndash Torches
ndash Spray chambers
ndash Nebulizers
Ion Extraction
ndash Sampler and skimmer cones
Autosampling
ndash Sample tubes racks probes and transfer tubing
ISIS
ndash Peristaltic pump tubing ferrules amp fittings
38
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sample Introduction
Key consumables requiring frequent replacement
bull Pump tubing
bull Torches and quartz transfer tube
bull Nebulizers
bull Spray chambers
bull Interface cones (skimmer amp sampler)
bull Transfer amp connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalogue
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24406(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 39
Autosampler Supplies
Key consumables requiring frequent replacement
ndash Peristaltic pump tubing
ndash Sample racks
ndash Sample tubes
ndash Spare probes
ndash Standard racks
ndash Connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24407(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 40
ISIS Supplies
Key consumables requiring frequent replacement
bull Peristaltic pump tubing
bull Ferrules and fittings
bull Valving
For ISIS Hydride Generation Accessory
bull Membrane filter
bull Concentric nebulizer
bull Gas-liquid separator
bull Other tubing and connectors
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceProductListingaspxcat=SubCat2ECS_24437(Agilent)amppcat=SubCat1ECS_24407(Agilent)amprcat=ClassECS_22674(Agilent)
41
ICP-MS Maintenance amp Trouble Shooting
May 2012
Where to Find the Right Consumable Analytical Consumables Agilent Assist
Consumables amp Supplies Instrument Sales ampServices 1-800-227-9770 (Option 11) 1-800-227-9770 (Option 13) wwwagilentcomchemcontactus wwwagilentcomchemcontactus
On-Line resources
ICP-MS Supplies
2nd Edition Speciation Handbook
ICP-MS Journal Archives
Recorded Agilent e-Seminars
ICP-OES Supplies
Atomic Absorption Supplies
Instrument Parts amp Supplies
Atomic Spec Application Notes
Agilent Quick Reference Guide for 77008800 ICP-MS (pub 5990-8182EN)
Agilent Atomic Spec Supplies Catalogue (pub 5990-8767EN)
Agilent Consumables Catalogue (pub 5990-6674EN)
Instrument User Manuals
42
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
System Cleanliness - Skimmer Cone
04 mm Orifice Nickel or Platinum
bull The Nickel skimmer cone is the standard interface
bull The skimmer cone is relatively robust to samples containing high concentrations of matrix and salts and is suitable for a wide variety of samples It is usually used with the Nickel sampling cone
bull The Platinum skimmer cone is usually used for introduction of hydrofluoric acid and other reagents It is usually used with the Platinum sampling cone
Potential Problems
bull Biggest risk is from physical damage to the orifice due to excessively aggressive cleaning
bull Cones also affected by sample matrix (acid strength amp type) and number of samples analyzed each day
bull Nickel ndash Typically replace 3 or 5 each year (assumes measuring 250-350 environmental samples each day)
bull Platinum ndash Typically replace 1 or 2 each year (assumes measuring 20-50 semiconductor samples each day)
bull If not clean then can result in analytical problems eg poor signal stability elemental contamination
20
ICP-MS Maintenance amp Trouble Shooting
May 2012
System Cleanliness - Cone Cleaning Procedure
Caution - Take care to avoid damage to the cone tip when removing ndash and place base down - Check the graphite gasket and replace if creased or damaged - Sonicate in a 2 Citranox or 2 Nitric Acid solution for a few minutes - Rinse well with de-ionized water - If still dirty or memory problems remain polish using an alumina powder slurry on a Q-tip then sonicate in 2 Citranox solution and rinse well with de-ionized water - Dry with nitrogen before installing
22
ICP-MS Maintenance amp Trouble Shooting
May 2012
Precision - Why is This Important
What does ldquoPrecisionrdquo mean
ndash Ability to get the same result for the same
sample when measured multiple times
ndash Usually measured as RSD or sometimes SD
RSD = (SD Mean Result) 100
ndash Low values indicate good precision
bull For ICP-MS expect 1-2 RSD
Why is this important
ndash User loses confidence in the system
What impacts on precision
ndash Nebulizerplasma stability
ndash Sample introduction system
ndash Method parameters
23
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash System stabilized
bull Allow 10 mins for plasma warm-up before
analysis
ndash Plasma status
bull ldquoBulletrdquo in the plasma should be stable
bull Check for deposits in the injector of the torch
ndash Check condition of interface cones and
clean if necessary
ndash Clean the Extraction Lens - Omega Lens
assembly
ndash Method parameters
bull Appropriate times set for sample uptake
delay and stabilization times
24
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash Sample Intro
What to Check ndash Nebulizer
bull Nebulizer type used can impact on sensitivity and precision
ndash MicroMist (glass concentric type) is the standard nebulizer ndash handles most sample
types
ndash PFA MicroFlow nebulizer best for low volume samples aggressive samples (HF
digests) and when low contamination required (semi-con)
ndash Babington gives poorer precision - best for high TDS samples
bull Check nebulizer condition regularly
ndash Chips in the nebulizer tip impact on aerosol formation ndash poor precision
(use a magnifying glass if necessary)
ndash Check for deposits or blockage in the tip
bull Sample uptake or flow rate
ndash Lower pump speed or using narrow bore pump tubing will reduce uptake rate
- better for high TDS samples
25
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Sample Introduction bull Contamination in the spray chamber
ndash When was the spray chamber cleaned
bull Any blockages in the nebulizer injector
ndash Check for stable aerosol formation
bull Air leaks in spray chamber end cap or connecting tubes
ndash Are they in good condition with tight connections
bull Damaged pump tubes
ndash When did you check the pump tubes
bull Is the pump speed too slow
ndash Low pump speeds may cause signal pulsation
ndash If required use narrower bore pump tube and increase pump speed
bull Samples have a high TDS content
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
26
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Memory effects
bull If possible avoid running high concentrations of these analytes
(Ag Au B Hg Mo Si Sn W Zn Zr)
ndash Maybe necessary to pre-dilute samples (if known to be high in concentration)
bull Ensure an adequate rinse time
ndash Should be at least equal to the sample uptake delay
(30-40 seconds typical)
bull May require an acidified rinse solution between samples
(2 HNO3)
bull Other strategies to minimize memory effects
ndash Use an inert spray chamber
ndash Use the ISIS to introduce discrete amounts of sample This means
bull Cones are exposed to less sample matrix = improved stability
bull Less memorycarry-over
bull Reduced uptake amp rinse times = faster measurement
27
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy - Why is This Important
What does ldquoAccuracyrdquo mean
ndash Ability to get the ldquorightrdquo answer for the sample
ndash Heavily dependent on operatorrsquos skill
Why is this important
ndash User loses confidence in the system
ndash Your reputationhellip
bull Customerrsquos question the results
bull Poor performance in ldquoround robinrdquo comparisons
How do You Confirm Accuracy
ndash Check the result for a prepared standard
ndash Measure a certified reference material
ndash Use other quality control checks to check analysis
28
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Calibration standards properly prepared
bull See earlier recommendations ndash important to match to samples prepare
accurately and use them ldquofreshrdquo
ndash Any interferences impacting on results
ndash Use matched standards or standard additions
ndash Ensure isotope selected has no polyatomic interferences
ndash If necessary use ORS3
ndash Precision optimized
bull Optimum signal to noise performance improves accuracy
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
29
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Reprocess data post
run using an
alternate internal
standard
bull Ensure Internal
Standard used is
similar in mass
bull Check whether the
Internal Standard is
present in the
sample
ndash If necessary do a Semi-
Quant measurement
bull Dilute with cal blk
matrix
30
Accuracy ndash Suspect Internal Standard Recovery
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Sample preparation
bull Is the most appropriate digestion being used
bull Are all of the analytes being quantitatively (and reproducibly) extracted and
dissolved
ndash Many digestions are only partial extracts ndash efficiency will vary with the
sample matrix
ndash Some volatile analytes may be ldquolostrdquo during digestion
bull Confirm by taking a solid certified reference material
through your preparation and analysis procedure
bull Is the digest stable ndash or are you seeing any precipitates or a suspension
bull Do you see any potential contamination from either reagents or the digestion
equipment eg especially with Si B or Ca
bull Include a ldquoReagent Blankrdquo with every sample batch to
monitor
31
ICP-MS Maintenance amp Trouble Shooting
May 2012
Laboratory environment can have
direct impact on quality of results
bull Clean uncluttered work area
bull Proper ventilation
bull Safety considerations
bull Instrument lifetime consideration
ICP-MS Maintenance amp Trouble Shooting
May 2012 32
Laboratory Environment
ICP-MS ndash Potential Autosampler Issues
ndash More customers use autosamplers with ICP for automation
ndash Issues to consider
bull Long transfer tube between sampler and ICP-MS
ndash May need to program a longer sample uptake delay
ndash May exacerbate problems with memory effects
ndash Use ldquoFast Pumprdquo during sample uptake delay
bull Caution ndash not always possible
Not recommended with high TDS samples and organics
bull Ensure probe diameter is appropriate for sample matrix
ndash Use wider bore for high TDS or viscous samples
bull Sample stability - potential for sample changes while uncovered in racks ndash impacts accuracy
ndash Dust ingress can introduce contamination
ndash Sample evaporation may occur during long unattended runs
ndash Sediment in the sample may settle out esp with wear metals or suspensions
bull Ensure transfer line to ICP-MS is in good condition
ndash Kinks in the line may cause poor uptake or pulsing in the sample
ndash Impacts on precision and accuracy
33
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sample Throughput ndash What to Check
ndash Samples fully digested
bull No excess particulates in the sample that may cause blockage
ndash Sample Introduction System optimized
ndash Capable of handling the TDS levels in the sample
ndash TorchNebulizer cleaned and ready for analysis
ndash Method parameters optimized
bull Sample uptake delay and stabilization times are appropriate ndash optimized
bull Integration time is appropriate for the expected concentration
ndash Use a longer integration time at low concentrations
bull Rinse time is appropriate
bull Use ldquoISISrdquo discrete sampling for faster measurement and faster washout
34
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Handles tough sample matrices better
than any other ICP-MS
ndash Highest plasma temperature (lowest
CeOCe) as standard
ndash HMI (high matrix introduction) allows direct
analysis of difficult samples
eg sea water
bull ORS3 operates in He collision mode to
remove ALL polyatomic interferences
ndash Enables reliable removal of all polyatomic
interferences using a single set of
conditions
ndash Gives lower levels of interference and
better long-term stability HMI gives lower suppression and
better long-term stability
Relative signal (suppression) in undiluted seawater
Long-term stability in undiluted seawater
35
Agilent ICP-MS Performance - Benefits
Best matrix tolerance amp less interferences
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS ndash Recommended Maintenance Schedule
ICP-MS Maintenance amp Trouble Shooting
May 2012 37
These functions
(and more) are
completed as part
of a Preventative
Maintenance
program by an
Agilent Field
Service Engineer
Summary ndash Key Consumables for ICP-MS
Sample preparationpresentation
ndash Peristaltic pump tubing
ndash Transfer and drain tubing
ndash ICP-MS standard solutions
ndash Internal Standard solutions
ndash Torches
ndash Spray chambers
ndash Nebulizers
Ion Extraction
ndash Sampler and skimmer cones
Autosampling
ndash Sample tubes racks probes and transfer tubing
ISIS
ndash Peristaltic pump tubing ferrules amp fittings
38
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sample Introduction
Key consumables requiring frequent replacement
bull Pump tubing
bull Torches and quartz transfer tube
bull Nebulizers
bull Spray chambers
bull Interface cones (skimmer amp sampler)
bull Transfer amp connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalogue
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24406(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 39
Autosampler Supplies
Key consumables requiring frequent replacement
ndash Peristaltic pump tubing
ndash Sample racks
ndash Sample tubes
ndash Spare probes
ndash Standard racks
ndash Connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24407(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 40
ISIS Supplies
Key consumables requiring frequent replacement
bull Peristaltic pump tubing
bull Ferrules and fittings
bull Valving
For ISIS Hydride Generation Accessory
bull Membrane filter
bull Concentric nebulizer
bull Gas-liquid separator
bull Other tubing and connectors
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceProductListingaspxcat=SubCat2ECS_24437(Agilent)amppcat=SubCat1ECS_24407(Agilent)amprcat=ClassECS_22674(Agilent)
41
ICP-MS Maintenance amp Trouble Shooting
May 2012
Where to Find the Right Consumable Analytical Consumables Agilent Assist
Consumables amp Supplies Instrument Sales ampServices 1-800-227-9770 (Option 11) 1-800-227-9770 (Option 13) wwwagilentcomchemcontactus wwwagilentcomchemcontactus
On-Line resources
ICP-MS Supplies
2nd Edition Speciation Handbook
ICP-MS Journal Archives
Recorded Agilent e-Seminars
ICP-OES Supplies
Atomic Absorption Supplies
Instrument Parts amp Supplies
Atomic Spec Application Notes
Agilent Quick Reference Guide for 77008800 ICP-MS (pub 5990-8182EN)
Agilent Atomic Spec Supplies Catalogue (pub 5990-8767EN)
Agilent Consumables Catalogue (pub 5990-6674EN)
Instrument User Manuals
42
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
System Cleanliness - Cone Cleaning Procedure
Caution - Take care to avoid damage to the cone tip when removing ndash and place base down - Check the graphite gasket and replace if creased or damaged - Sonicate in a 2 Citranox or 2 Nitric Acid solution for a few minutes - Rinse well with de-ionized water - If still dirty or memory problems remain polish using an alumina powder slurry on a Q-tip then sonicate in 2 Citranox solution and rinse well with de-ionized water - Dry with nitrogen before installing
22
ICP-MS Maintenance amp Trouble Shooting
May 2012
Precision - Why is This Important
What does ldquoPrecisionrdquo mean
ndash Ability to get the same result for the same
sample when measured multiple times
ndash Usually measured as RSD or sometimes SD
RSD = (SD Mean Result) 100
ndash Low values indicate good precision
bull For ICP-MS expect 1-2 RSD
Why is this important
ndash User loses confidence in the system
What impacts on precision
ndash Nebulizerplasma stability
ndash Sample introduction system
ndash Method parameters
23
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash System stabilized
bull Allow 10 mins for plasma warm-up before
analysis
ndash Plasma status
bull ldquoBulletrdquo in the plasma should be stable
bull Check for deposits in the injector of the torch
ndash Check condition of interface cones and
clean if necessary
ndash Clean the Extraction Lens - Omega Lens
assembly
ndash Method parameters
bull Appropriate times set for sample uptake
delay and stabilization times
24
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash Sample Intro
What to Check ndash Nebulizer
bull Nebulizer type used can impact on sensitivity and precision
ndash MicroMist (glass concentric type) is the standard nebulizer ndash handles most sample
types
ndash PFA MicroFlow nebulizer best for low volume samples aggressive samples (HF
digests) and when low contamination required (semi-con)
ndash Babington gives poorer precision - best for high TDS samples
bull Check nebulizer condition regularly
ndash Chips in the nebulizer tip impact on aerosol formation ndash poor precision
(use a magnifying glass if necessary)
ndash Check for deposits or blockage in the tip
bull Sample uptake or flow rate
ndash Lower pump speed or using narrow bore pump tubing will reduce uptake rate
- better for high TDS samples
25
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Sample Introduction bull Contamination in the spray chamber
ndash When was the spray chamber cleaned
bull Any blockages in the nebulizer injector
ndash Check for stable aerosol formation
bull Air leaks in spray chamber end cap or connecting tubes
ndash Are they in good condition with tight connections
bull Damaged pump tubes
ndash When did you check the pump tubes
bull Is the pump speed too slow
ndash Low pump speeds may cause signal pulsation
ndash If required use narrower bore pump tube and increase pump speed
bull Samples have a high TDS content
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
26
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Memory effects
bull If possible avoid running high concentrations of these analytes
(Ag Au B Hg Mo Si Sn W Zn Zr)
ndash Maybe necessary to pre-dilute samples (if known to be high in concentration)
bull Ensure an adequate rinse time
ndash Should be at least equal to the sample uptake delay
(30-40 seconds typical)
bull May require an acidified rinse solution between samples
(2 HNO3)
bull Other strategies to minimize memory effects
ndash Use an inert spray chamber
ndash Use the ISIS to introduce discrete amounts of sample This means
bull Cones are exposed to less sample matrix = improved stability
bull Less memorycarry-over
bull Reduced uptake amp rinse times = faster measurement
27
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy - Why is This Important
What does ldquoAccuracyrdquo mean
ndash Ability to get the ldquorightrdquo answer for the sample
ndash Heavily dependent on operatorrsquos skill
Why is this important
ndash User loses confidence in the system
ndash Your reputationhellip
bull Customerrsquos question the results
bull Poor performance in ldquoround robinrdquo comparisons
How do You Confirm Accuracy
ndash Check the result for a prepared standard
ndash Measure a certified reference material
ndash Use other quality control checks to check analysis
28
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Calibration standards properly prepared
bull See earlier recommendations ndash important to match to samples prepare
accurately and use them ldquofreshrdquo
ndash Any interferences impacting on results
ndash Use matched standards or standard additions
ndash Ensure isotope selected has no polyatomic interferences
ndash If necessary use ORS3
ndash Precision optimized
bull Optimum signal to noise performance improves accuracy
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
29
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Reprocess data post
run using an
alternate internal
standard
bull Ensure Internal
Standard used is
similar in mass
bull Check whether the
Internal Standard is
present in the
sample
ndash If necessary do a Semi-
Quant measurement
bull Dilute with cal blk
matrix
30
Accuracy ndash Suspect Internal Standard Recovery
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Sample preparation
bull Is the most appropriate digestion being used
bull Are all of the analytes being quantitatively (and reproducibly) extracted and
dissolved
ndash Many digestions are only partial extracts ndash efficiency will vary with the
sample matrix
ndash Some volatile analytes may be ldquolostrdquo during digestion
bull Confirm by taking a solid certified reference material
through your preparation and analysis procedure
bull Is the digest stable ndash or are you seeing any precipitates or a suspension
bull Do you see any potential contamination from either reagents or the digestion
equipment eg especially with Si B or Ca
bull Include a ldquoReagent Blankrdquo with every sample batch to
monitor
31
ICP-MS Maintenance amp Trouble Shooting
May 2012
Laboratory environment can have
direct impact on quality of results
bull Clean uncluttered work area
bull Proper ventilation
bull Safety considerations
bull Instrument lifetime consideration
ICP-MS Maintenance amp Trouble Shooting
May 2012 32
Laboratory Environment
ICP-MS ndash Potential Autosampler Issues
ndash More customers use autosamplers with ICP for automation
ndash Issues to consider
bull Long transfer tube between sampler and ICP-MS
ndash May need to program a longer sample uptake delay
ndash May exacerbate problems with memory effects
ndash Use ldquoFast Pumprdquo during sample uptake delay
bull Caution ndash not always possible
Not recommended with high TDS samples and organics
bull Ensure probe diameter is appropriate for sample matrix
ndash Use wider bore for high TDS or viscous samples
bull Sample stability - potential for sample changes while uncovered in racks ndash impacts accuracy
ndash Dust ingress can introduce contamination
ndash Sample evaporation may occur during long unattended runs
ndash Sediment in the sample may settle out esp with wear metals or suspensions
bull Ensure transfer line to ICP-MS is in good condition
ndash Kinks in the line may cause poor uptake or pulsing in the sample
ndash Impacts on precision and accuracy
33
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sample Throughput ndash What to Check
ndash Samples fully digested
bull No excess particulates in the sample that may cause blockage
ndash Sample Introduction System optimized
ndash Capable of handling the TDS levels in the sample
ndash TorchNebulizer cleaned and ready for analysis
ndash Method parameters optimized
bull Sample uptake delay and stabilization times are appropriate ndash optimized
bull Integration time is appropriate for the expected concentration
ndash Use a longer integration time at low concentrations
bull Rinse time is appropriate
bull Use ldquoISISrdquo discrete sampling for faster measurement and faster washout
34
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Handles tough sample matrices better
than any other ICP-MS
ndash Highest plasma temperature (lowest
CeOCe) as standard
ndash HMI (high matrix introduction) allows direct
analysis of difficult samples
eg sea water
bull ORS3 operates in He collision mode to
remove ALL polyatomic interferences
ndash Enables reliable removal of all polyatomic
interferences using a single set of
conditions
ndash Gives lower levels of interference and
better long-term stability HMI gives lower suppression and
better long-term stability
Relative signal (suppression) in undiluted seawater
Long-term stability in undiluted seawater
35
Agilent ICP-MS Performance - Benefits
Best matrix tolerance amp less interferences
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS ndash Recommended Maintenance Schedule
ICP-MS Maintenance amp Trouble Shooting
May 2012 37
These functions
(and more) are
completed as part
of a Preventative
Maintenance
program by an
Agilent Field
Service Engineer
Summary ndash Key Consumables for ICP-MS
Sample preparationpresentation
ndash Peristaltic pump tubing
ndash Transfer and drain tubing
ndash ICP-MS standard solutions
ndash Internal Standard solutions
ndash Torches
ndash Spray chambers
ndash Nebulizers
Ion Extraction
ndash Sampler and skimmer cones
Autosampling
ndash Sample tubes racks probes and transfer tubing
ISIS
ndash Peristaltic pump tubing ferrules amp fittings
38
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sample Introduction
Key consumables requiring frequent replacement
bull Pump tubing
bull Torches and quartz transfer tube
bull Nebulizers
bull Spray chambers
bull Interface cones (skimmer amp sampler)
bull Transfer amp connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalogue
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24406(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 39
Autosampler Supplies
Key consumables requiring frequent replacement
ndash Peristaltic pump tubing
ndash Sample racks
ndash Sample tubes
ndash Spare probes
ndash Standard racks
ndash Connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24407(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 40
ISIS Supplies
Key consumables requiring frequent replacement
bull Peristaltic pump tubing
bull Ferrules and fittings
bull Valving
For ISIS Hydride Generation Accessory
bull Membrane filter
bull Concentric nebulizer
bull Gas-liquid separator
bull Other tubing and connectors
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceProductListingaspxcat=SubCat2ECS_24437(Agilent)amppcat=SubCat1ECS_24407(Agilent)amprcat=ClassECS_22674(Agilent)
41
ICP-MS Maintenance amp Trouble Shooting
May 2012
Where to Find the Right Consumable Analytical Consumables Agilent Assist
Consumables amp Supplies Instrument Sales ampServices 1-800-227-9770 (Option 11) 1-800-227-9770 (Option 13) wwwagilentcomchemcontactus wwwagilentcomchemcontactus
On-Line resources
ICP-MS Supplies
2nd Edition Speciation Handbook
ICP-MS Journal Archives
Recorded Agilent e-Seminars
ICP-OES Supplies
Atomic Absorption Supplies
Instrument Parts amp Supplies
Atomic Spec Application Notes
Agilent Quick Reference Guide for 77008800 ICP-MS (pub 5990-8182EN)
Agilent Atomic Spec Supplies Catalogue (pub 5990-8767EN)
Agilent Consumables Catalogue (pub 5990-6674EN)
Instrument User Manuals
42
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
Precision - Why is This Important
What does ldquoPrecisionrdquo mean
ndash Ability to get the same result for the same
sample when measured multiple times
ndash Usually measured as RSD or sometimes SD
RSD = (SD Mean Result) 100
ndash Low values indicate good precision
bull For ICP-MS expect 1-2 RSD
Why is this important
ndash User loses confidence in the system
What impacts on precision
ndash Nebulizerplasma stability
ndash Sample introduction system
ndash Method parameters
23
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash System stabilized
bull Allow 10 mins for plasma warm-up before
analysis
ndash Plasma status
bull ldquoBulletrdquo in the plasma should be stable
bull Check for deposits in the injector of the torch
ndash Check condition of interface cones and
clean if necessary
ndash Clean the Extraction Lens - Omega Lens
assembly
ndash Method parameters
bull Appropriate times set for sample uptake
delay and stabilization times
24
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash Sample Intro
What to Check ndash Nebulizer
bull Nebulizer type used can impact on sensitivity and precision
ndash MicroMist (glass concentric type) is the standard nebulizer ndash handles most sample
types
ndash PFA MicroFlow nebulizer best for low volume samples aggressive samples (HF
digests) and when low contamination required (semi-con)
ndash Babington gives poorer precision - best for high TDS samples
bull Check nebulizer condition regularly
ndash Chips in the nebulizer tip impact on aerosol formation ndash poor precision
(use a magnifying glass if necessary)
ndash Check for deposits or blockage in the tip
bull Sample uptake or flow rate
ndash Lower pump speed or using narrow bore pump tubing will reduce uptake rate
- better for high TDS samples
25
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Sample Introduction bull Contamination in the spray chamber
ndash When was the spray chamber cleaned
bull Any blockages in the nebulizer injector
ndash Check for stable aerosol formation
bull Air leaks in spray chamber end cap or connecting tubes
ndash Are they in good condition with tight connections
bull Damaged pump tubes
ndash When did you check the pump tubes
bull Is the pump speed too slow
ndash Low pump speeds may cause signal pulsation
ndash If required use narrower bore pump tube and increase pump speed
bull Samples have a high TDS content
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
26
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Memory effects
bull If possible avoid running high concentrations of these analytes
(Ag Au B Hg Mo Si Sn W Zn Zr)
ndash Maybe necessary to pre-dilute samples (if known to be high in concentration)
bull Ensure an adequate rinse time
ndash Should be at least equal to the sample uptake delay
(30-40 seconds typical)
bull May require an acidified rinse solution between samples
(2 HNO3)
bull Other strategies to minimize memory effects
ndash Use an inert spray chamber
ndash Use the ISIS to introduce discrete amounts of sample This means
bull Cones are exposed to less sample matrix = improved stability
bull Less memorycarry-over
bull Reduced uptake amp rinse times = faster measurement
27
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy - Why is This Important
What does ldquoAccuracyrdquo mean
ndash Ability to get the ldquorightrdquo answer for the sample
ndash Heavily dependent on operatorrsquos skill
Why is this important
ndash User loses confidence in the system
ndash Your reputationhellip
bull Customerrsquos question the results
bull Poor performance in ldquoround robinrdquo comparisons
How do You Confirm Accuracy
ndash Check the result for a prepared standard
ndash Measure a certified reference material
ndash Use other quality control checks to check analysis
28
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Calibration standards properly prepared
bull See earlier recommendations ndash important to match to samples prepare
accurately and use them ldquofreshrdquo
ndash Any interferences impacting on results
ndash Use matched standards or standard additions
ndash Ensure isotope selected has no polyatomic interferences
ndash If necessary use ORS3
ndash Precision optimized
bull Optimum signal to noise performance improves accuracy
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
29
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Reprocess data post
run using an
alternate internal
standard
bull Ensure Internal
Standard used is
similar in mass
bull Check whether the
Internal Standard is
present in the
sample
ndash If necessary do a Semi-
Quant measurement
bull Dilute with cal blk
matrix
30
Accuracy ndash Suspect Internal Standard Recovery
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Sample preparation
bull Is the most appropriate digestion being used
bull Are all of the analytes being quantitatively (and reproducibly) extracted and
dissolved
ndash Many digestions are only partial extracts ndash efficiency will vary with the
sample matrix
ndash Some volatile analytes may be ldquolostrdquo during digestion
bull Confirm by taking a solid certified reference material
through your preparation and analysis procedure
bull Is the digest stable ndash or are you seeing any precipitates or a suspension
bull Do you see any potential contamination from either reagents or the digestion
equipment eg especially with Si B or Ca
bull Include a ldquoReagent Blankrdquo with every sample batch to
monitor
31
ICP-MS Maintenance amp Trouble Shooting
May 2012
Laboratory environment can have
direct impact on quality of results
bull Clean uncluttered work area
bull Proper ventilation
bull Safety considerations
bull Instrument lifetime consideration
ICP-MS Maintenance amp Trouble Shooting
May 2012 32
Laboratory Environment
ICP-MS ndash Potential Autosampler Issues
ndash More customers use autosamplers with ICP for automation
ndash Issues to consider
bull Long transfer tube between sampler and ICP-MS
ndash May need to program a longer sample uptake delay
ndash May exacerbate problems with memory effects
ndash Use ldquoFast Pumprdquo during sample uptake delay
bull Caution ndash not always possible
Not recommended with high TDS samples and organics
bull Ensure probe diameter is appropriate for sample matrix
ndash Use wider bore for high TDS or viscous samples
bull Sample stability - potential for sample changes while uncovered in racks ndash impacts accuracy
ndash Dust ingress can introduce contamination
ndash Sample evaporation may occur during long unattended runs
ndash Sediment in the sample may settle out esp with wear metals or suspensions
bull Ensure transfer line to ICP-MS is in good condition
ndash Kinks in the line may cause poor uptake or pulsing in the sample
ndash Impacts on precision and accuracy
33
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sample Throughput ndash What to Check
ndash Samples fully digested
bull No excess particulates in the sample that may cause blockage
ndash Sample Introduction System optimized
ndash Capable of handling the TDS levels in the sample
ndash TorchNebulizer cleaned and ready for analysis
ndash Method parameters optimized
bull Sample uptake delay and stabilization times are appropriate ndash optimized
bull Integration time is appropriate for the expected concentration
ndash Use a longer integration time at low concentrations
bull Rinse time is appropriate
bull Use ldquoISISrdquo discrete sampling for faster measurement and faster washout
34
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Handles tough sample matrices better
than any other ICP-MS
ndash Highest plasma temperature (lowest
CeOCe) as standard
ndash HMI (high matrix introduction) allows direct
analysis of difficult samples
eg sea water
bull ORS3 operates in He collision mode to
remove ALL polyatomic interferences
ndash Enables reliable removal of all polyatomic
interferences using a single set of
conditions
ndash Gives lower levels of interference and
better long-term stability HMI gives lower suppression and
better long-term stability
Relative signal (suppression) in undiluted seawater
Long-term stability in undiluted seawater
35
Agilent ICP-MS Performance - Benefits
Best matrix tolerance amp less interferences
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS ndash Recommended Maintenance Schedule
ICP-MS Maintenance amp Trouble Shooting
May 2012 37
These functions
(and more) are
completed as part
of a Preventative
Maintenance
program by an
Agilent Field
Service Engineer
Summary ndash Key Consumables for ICP-MS
Sample preparationpresentation
ndash Peristaltic pump tubing
ndash Transfer and drain tubing
ndash ICP-MS standard solutions
ndash Internal Standard solutions
ndash Torches
ndash Spray chambers
ndash Nebulizers
Ion Extraction
ndash Sampler and skimmer cones
Autosampling
ndash Sample tubes racks probes and transfer tubing
ISIS
ndash Peristaltic pump tubing ferrules amp fittings
38
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sample Introduction
Key consumables requiring frequent replacement
bull Pump tubing
bull Torches and quartz transfer tube
bull Nebulizers
bull Spray chambers
bull Interface cones (skimmer amp sampler)
bull Transfer amp connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalogue
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24406(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 39
Autosampler Supplies
Key consumables requiring frequent replacement
ndash Peristaltic pump tubing
ndash Sample racks
ndash Sample tubes
ndash Spare probes
ndash Standard racks
ndash Connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24407(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 40
ISIS Supplies
Key consumables requiring frequent replacement
bull Peristaltic pump tubing
bull Ferrules and fittings
bull Valving
For ISIS Hydride Generation Accessory
bull Membrane filter
bull Concentric nebulizer
bull Gas-liquid separator
bull Other tubing and connectors
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceProductListingaspxcat=SubCat2ECS_24437(Agilent)amppcat=SubCat1ECS_24407(Agilent)amprcat=ClassECS_22674(Agilent)
41
ICP-MS Maintenance amp Trouble Shooting
May 2012
Where to Find the Right Consumable Analytical Consumables Agilent Assist
Consumables amp Supplies Instrument Sales ampServices 1-800-227-9770 (Option 11) 1-800-227-9770 (Option 13) wwwagilentcomchemcontactus wwwagilentcomchemcontactus
On-Line resources
ICP-MS Supplies
2nd Edition Speciation Handbook
ICP-MS Journal Archives
Recorded Agilent e-Seminars
ICP-OES Supplies
Atomic Absorption Supplies
Instrument Parts amp Supplies
Atomic Spec Application Notes
Agilent Quick Reference Guide for 77008800 ICP-MS (pub 5990-8182EN)
Agilent Atomic Spec Supplies Catalogue (pub 5990-8767EN)
Agilent Consumables Catalogue (pub 5990-6674EN)
Instrument User Manuals
42
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash System stabilized
bull Allow 10 mins for plasma warm-up before
analysis
ndash Plasma status
bull ldquoBulletrdquo in the plasma should be stable
bull Check for deposits in the injector of the torch
ndash Check condition of interface cones and
clean if necessary
ndash Clean the Extraction Lens - Omega Lens
assembly
ndash Method parameters
bull Appropriate times set for sample uptake
delay and stabilization times
24
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash Sample Intro
What to Check ndash Nebulizer
bull Nebulizer type used can impact on sensitivity and precision
ndash MicroMist (glass concentric type) is the standard nebulizer ndash handles most sample
types
ndash PFA MicroFlow nebulizer best for low volume samples aggressive samples (HF
digests) and when low contamination required (semi-con)
ndash Babington gives poorer precision - best for high TDS samples
bull Check nebulizer condition regularly
ndash Chips in the nebulizer tip impact on aerosol formation ndash poor precision
(use a magnifying glass if necessary)
ndash Check for deposits or blockage in the tip
bull Sample uptake or flow rate
ndash Lower pump speed or using narrow bore pump tubing will reduce uptake rate
- better for high TDS samples
25
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Sample Introduction bull Contamination in the spray chamber
ndash When was the spray chamber cleaned
bull Any blockages in the nebulizer injector
ndash Check for stable aerosol formation
bull Air leaks in spray chamber end cap or connecting tubes
ndash Are they in good condition with tight connections
bull Damaged pump tubes
ndash When did you check the pump tubes
bull Is the pump speed too slow
ndash Low pump speeds may cause signal pulsation
ndash If required use narrower bore pump tube and increase pump speed
bull Samples have a high TDS content
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
26
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Memory effects
bull If possible avoid running high concentrations of these analytes
(Ag Au B Hg Mo Si Sn W Zn Zr)
ndash Maybe necessary to pre-dilute samples (if known to be high in concentration)
bull Ensure an adequate rinse time
ndash Should be at least equal to the sample uptake delay
(30-40 seconds typical)
bull May require an acidified rinse solution between samples
(2 HNO3)
bull Other strategies to minimize memory effects
ndash Use an inert spray chamber
ndash Use the ISIS to introduce discrete amounts of sample This means
bull Cones are exposed to less sample matrix = improved stability
bull Less memorycarry-over
bull Reduced uptake amp rinse times = faster measurement
27
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy - Why is This Important
What does ldquoAccuracyrdquo mean
ndash Ability to get the ldquorightrdquo answer for the sample
ndash Heavily dependent on operatorrsquos skill
Why is this important
ndash User loses confidence in the system
ndash Your reputationhellip
bull Customerrsquos question the results
bull Poor performance in ldquoround robinrdquo comparisons
How do You Confirm Accuracy
ndash Check the result for a prepared standard
ndash Measure a certified reference material
ndash Use other quality control checks to check analysis
28
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Calibration standards properly prepared
bull See earlier recommendations ndash important to match to samples prepare
accurately and use them ldquofreshrdquo
ndash Any interferences impacting on results
ndash Use matched standards or standard additions
ndash Ensure isotope selected has no polyatomic interferences
ndash If necessary use ORS3
ndash Precision optimized
bull Optimum signal to noise performance improves accuracy
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
29
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Reprocess data post
run using an
alternate internal
standard
bull Ensure Internal
Standard used is
similar in mass
bull Check whether the
Internal Standard is
present in the
sample
ndash If necessary do a Semi-
Quant measurement
bull Dilute with cal blk
matrix
30
Accuracy ndash Suspect Internal Standard Recovery
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Sample preparation
bull Is the most appropriate digestion being used
bull Are all of the analytes being quantitatively (and reproducibly) extracted and
dissolved
ndash Many digestions are only partial extracts ndash efficiency will vary with the
sample matrix
ndash Some volatile analytes may be ldquolostrdquo during digestion
bull Confirm by taking a solid certified reference material
through your preparation and analysis procedure
bull Is the digest stable ndash or are you seeing any precipitates or a suspension
bull Do you see any potential contamination from either reagents or the digestion
equipment eg especially with Si B or Ca
bull Include a ldquoReagent Blankrdquo with every sample batch to
monitor
31
ICP-MS Maintenance amp Trouble Shooting
May 2012
Laboratory environment can have
direct impact on quality of results
bull Clean uncluttered work area
bull Proper ventilation
bull Safety considerations
bull Instrument lifetime consideration
ICP-MS Maintenance amp Trouble Shooting
May 2012 32
Laboratory Environment
ICP-MS ndash Potential Autosampler Issues
ndash More customers use autosamplers with ICP for automation
ndash Issues to consider
bull Long transfer tube between sampler and ICP-MS
ndash May need to program a longer sample uptake delay
ndash May exacerbate problems with memory effects
ndash Use ldquoFast Pumprdquo during sample uptake delay
bull Caution ndash not always possible
Not recommended with high TDS samples and organics
bull Ensure probe diameter is appropriate for sample matrix
ndash Use wider bore for high TDS or viscous samples
bull Sample stability - potential for sample changes while uncovered in racks ndash impacts accuracy
ndash Dust ingress can introduce contamination
ndash Sample evaporation may occur during long unattended runs
ndash Sediment in the sample may settle out esp with wear metals or suspensions
bull Ensure transfer line to ICP-MS is in good condition
ndash Kinks in the line may cause poor uptake or pulsing in the sample
ndash Impacts on precision and accuracy
33
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sample Throughput ndash What to Check
ndash Samples fully digested
bull No excess particulates in the sample that may cause blockage
ndash Sample Introduction System optimized
ndash Capable of handling the TDS levels in the sample
ndash TorchNebulizer cleaned and ready for analysis
ndash Method parameters optimized
bull Sample uptake delay and stabilization times are appropriate ndash optimized
bull Integration time is appropriate for the expected concentration
ndash Use a longer integration time at low concentrations
bull Rinse time is appropriate
bull Use ldquoISISrdquo discrete sampling for faster measurement and faster washout
34
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Handles tough sample matrices better
than any other ICP-MS
ndash Highest plasma temperature (lowest
CeOCe) as standard
ndash HMI (high matrix introduction) allows direct
analysis of difficult samples
eg sea water
bull ORS3 operates in He collision mode to
remove ALL polyatomic interferences
ndash Enables reliable removal of all polyatomic
interferences using a single set of
conditions
ndash Gives lower levels of interference and
better long-term stability HMI gives lower suppression and
better long-term stability
Relative signal (suppression) in undiluted seawater
Long-term stability in undiluted seawater
35
Agilent ICP-MS Performance - Benefits
Best matrix tolerance amp less interferences
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS ndash Recommended Maintenance Schedule
ICP-MS Maintenance amp Trouble Shooting
May 2012 37
These functions
(and more) are
completed as part
of a Preventative
Maintenance
program by an
Agilent Field
Service Engineer
Summary ndash Key Consumables for ICP-MS
Sample preparationpresentation
ndash Peristaltic pump tubing
ndash Transfer and drain tubing
ndash ICP-MS standard solutions
ndash Internal Standard solutions
ndash Torches
ndash Spray chambers
ndash Nebulizers
Ion Extraction
ndash Sampler and skimmer cones
Autosampling
ndash Sample tubes racks probes and transfer tubing
ISIS
ndash Peristaltic pump tubing ferrules amp fittings
38
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sample Introduction
Key consumables requiring frequent replacement
bull Pump tubing
bull Torches and quartz transfer tube
bull Nebulizers
bull Spray chambers
bull Interface cones (skimmer amp sampler)
bull Transfer amp connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalogue
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24406(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 39
Autosampler Supplies
Key consumables requiring frequent replacement
ndash Peristaltic pump tubing
ndash Sample racks
ndash Sample tubes
ndash Spare probes
ndash Standard racks
ndash Connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24407(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 40
ISIS Supplies
Key consumables requiring frequent replacement
bull Peristaltic pump tubing
bull Ferrules and fittings
bull Valving
For ISIS Hydride Generation Accessory
bull Membrane filter
bull Concentric nebulizer
bull Gas-liquid separator
bull Other tubing and connectors
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceProductListingaspxcat=SubCat2ECS_24437(Agilent)amppcat=SubCat1ECS_24407(Agilent)amprcat=ClassECS_22674(Agilent)
41
ICP-MS Maintenance amp Trouble Shooting
May 2012
Where to Find the Right Consumable Analytical Consumables Agilent Assist
Consumables amp Supplies Instrument Sales ampServices 1-800-227-9770 (Option 11) 1-800-227-9770 (Option 13) wwwagilentcomchemcontactus wwwagilentcomchemcontactus
On-Line resources
ICP-MS Supplies
2nd Edition Speciation Handbook
ICP-MS Journal Archives
Recorded Agilent e-Seminars
ICP-OES Supplies
Atomic Absorption Supplies
Instrument Parts amp Supplies
Atomic Spec Application Notes
Agilent Quick Reference Guide for 77008800 ICP-MS (pub 5990-8182EN)
Agilent Atomic Spec Supplies Catalogue (pub 5990-8767EN)
Agilent Consumables Catalogue (pub 5990-6674EN)
Instrument User Manuals
42
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash Sample Intro
What to Check ndash Nebulizer
bull Nebulizer type used can impact on sensitivity and precision
ndash MicroMist (glass concentric type) is the standard nebulizer ndash handles most sample
types
ndash PFA MicroFlow nebulizer best for low volume samples aggressive samples (HF
digests) and when low contamination required (semi-con)
ndash Babington gives poorer precision - best for high TDS samples
bull Check nebulizer condition regularly
ndash Chips in the nebulizer tip impact on aerosol formation ndash poor precision
(use a magnifying glass if necessary)
ndash Check for deposits or blockage in the tip
bull Sample uptake or flow rate
ndash Lower pump speed or using narrow bore pump tubing will reduce uptake rate
- better for high TDS samples
25
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Sample Introduction bull Contamination in the spray chamber
ndash When was the spray chamber cleaned
bull Any blockages in the nebulizer injector
ndash Check for stable aerosol formation
bull Air leaks in spray chamber end cap or connecting tubes
ndash Are they in good condition with tight connections
bull Damaged pump tubes
ndash When did you check the pump tubes
bull Is the pump speed too slow
ndash Low pump speeds may cause signal pulsation
ndash If required use narrower bore pump tube and increase pump speed
bull Samples have a high TDS content
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
26
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Memory effects
bull If possible avoid running high concentrations of these analytes
(Ag Au B Hg Mo Si Sn W Zn Zr)
ndash Maybe necessary to pre-dilute samples (if known to be high in concentration)
bull Ensure an adequate rinse time
ndash Should be at least equal to the sample uptake delay
(30-40 seconds typical)
bull May require an acidified rinse solution between samples
(2 HNO3)
bull Other strategies to minimize memory effects
ndash Use an inert spray chamber
ndash Use the ISIS to introduce discrete amounts of sample This means
bull Cones are exposed to less sample matrix = improved stability
bull Less memorycarry-over
bull Reduced uptake amp rinse times = faster measurement
27
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy - Why is This Important
What does ldquoAccuracyrdquo mean
ndash Ability to get the ldquorightrdquo answer for the sample
ndash Heavily dependent on operatorrsquos skill
Why is this important
ndash User loses confidence in the system
ndash Your reputationhellip
bull Customerrsquos question the results
bull Poor performance in ldquoround robinrdquo comparisons
How do You Confirm Accuracy
ndash Check the result for a prepared standard
ndash Measure a certified reference material
ndash Use other quality control checks to check analysis
28
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Calibration standards properly prepared
bull See earlier recommendations ndash important to match to samples prepare
accurately and use them ldquofreshrdquo
ndash Any interferences impacting on results
ndash Use matched standards or standard additions
ndash Ensure isotope selected has no polyatomic interferences
ndash If necessary use ORS3
ndash Precision optimized
bull Optimum signal to noise performance improves accuracy
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
29
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Reprocess data post
run using an
alternate internal
standard
bull Ensure Internal
Standard used is
similar in mass
bull Check whether the
Internal Standard is
present in the
sample
ndash If necessary do a Semi-
Quant measurement
bull Dilute with cal blk
matrix
30
Accuracy ndash Suspect Internal Standard Recovery
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Sample preparation
bull Is the most appropriate digestion being used
bull Are all of the analytes being quantitatively (and reproducibly) extracted and
dissolved
ndash Many digestions are only partial extracts ndash efficiency will vary with the
sample matrix
ndash Some volatile analytes may be ldquolostrdquo during digestion
bull Confirm by taking a solid certified reference material
through your preparation and analysis procedure
bull Is the digest stable ndash or are you seeing any precipitates or a suspension
bull Do you see any potential contamination from either reagents or the digestion
equipment eg especially with Si B or Ca
bull Include a ldquoReagent Blankrdquo with every sample batch to
monitor
31
ICP-MS Maintenance amp Trouble Shooting
May 2012
Laboratory environment can have
direct impact on quality of results
bull Clean uncluttered work area
bull Proper ventilation
bull Safety considerations
bull Instrument lifetime consideration
ICP-MS Maintenance amp Trouble Shooting
May 2012 32
Laboratory Environment
ICP-MS ndash Potential Autosampler Issues
ndash More customers use autosamplers with ICP for automation
ndash Issues to consider
bull Long transfer tube between sampler and ICP-MS
ndash May need to program a longer sample uptake delay
ndash May exacerbate problems with memory effects
ndash Use ldquoFast Pumprdquo during sample uptake delay
bull Caution ndash not always possible
Not recommended with high TDS samples and organics
bull Ensure probe diameter is appropriate for sample matrix
ndash Use wider bore for high TDS or viscous samples
bull Sample stability - potential for sample changes while uncovered in racks ndash impacts accuracy
ndash Dust ingress can introduce contamination
ndash Sample evaporation may occur during long unattended runs
ndash Sediment in the sample may settle out esp with wear metals or suspensions
bull Ensure transfer line to ICP-MS is in good condition
ndash Kinks in the line may cause poor uptake or pulsing in the sample
ndash Impacts on precision and accuracy
33
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sample Throughput ndash What to Check
ndash Samples fully digested
bull No excess particulates in the sample that may cause blockage
ndash Sample Introduction System optimized
ndash Capable of handling the TDS levels in the sample
ndash TorchNebulizer cleaned and ready for analysis
ndash Method parameters optimized
bull Sample uptake delay and stabilization times are appropriate ndash optimized
bull Integration time is appropriate for the expected concentration
ndash Use a longer integration time at low concentrations
bull Rinse time is appropriate
bull Use ldquoISISrdquo discrete sampling for faster measurement and faster washout
34
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Handles tough sample matrices better
than any other ICP-MS
ndash Highest plasma temperature (lowest
CeOCe) as standard
ndash HMI (high matrix introduction) allows direct
analysis of difficult samples
eg sea water
bull ORS3 operates in He collision mode to
remove ALL polyatomic interferences
ndash Enables reliable removal of all polyatomic
interferences using a single set of
conditions
ndash Gives lower levels of interference and
better long-term stability HMI gives lower suppression and
better long-term stability
Relative signal (suppression) in undiluted seawater
Long-term stability in undiluted seawater
35
Agilent ICP-MS Performance - Benefits
Best matrix tolerance amp less interferences
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS ndash Recommended Maintenance Schedule
ICP-MS Maintenance amp Trouble Shooting
May 2012 37
These functions
(and more) are
completed as part
of a Preventative
Maintenance
program by an
Agilent Field
Service Engineer
Summary ndash Key Consumables for ICP-MS
Sample preparationpresentation
ndash Peristaltic pump tubing
ndash Transfer and drain tubing
ndash ICP-MS standard solutions
ndash Internal Standard solutions
ndash Torches
ndash Spray chambers
ndash Nebulizers
Ion Extraction
ndash Sampler and skimmer cones
Autosampling
ndash Sample tubes racks probes and transfer tubing
ISIS
ndash Peristaltic pump tubing ferrules amp fittings
38
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sample Introduction
Key consumables requiring frequent replacement
bull Pump tubing
bull Torches and quartz transfer tube
bull Nebulizers
bull Spray chambers
bull Interface cones (skimmer amp sampler)
bull Transfer amp connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalogue
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24406(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 39
Autosampler Supplies
Key consumables requiring frequent replacement
ndash Peristaltic pump tubing
ndash Sample racks
ndash Sample tubes
ndash Spare probes
ndash Standard racks
ndash Connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24407(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 40
ISIS Supplies
Key consumables requiring frequent replacement
bull Peristaltic pump tubing
bull Ferrules and fittings
bull Valving
For ISIS Hydride Generation Accessory
bull Membrane filter
bull Concentric nebulizer
bull Gas-liquid separator
bull Other tubing and connectors
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceProductListingaspxcat=SubCat2ECS_24437(Agilent)amppcat=SubCat1ECS_24407(Agilent)amprcat=ClassECS_22674(Agilent)
41
ICP-MS Maintenance amp Trouble Shooting
May 2012
Where to Find the Right Consumable Analytical Consumables Agilent Assist
Consumables amp Supplies Instrument Sales ampServices 1-800-227-9770 (Option 11) 1-800-227-9770 (Option 13) wwwagilentcomchemcontactus wwwagilentcomchemcontactus
On-Line resources
ICP-MS Supplies
2nd Edition Speciation Handbook
ICP-MS Journal Archives
Recorded Agilent e-Seminars
ICP-OES Supplies
Atomic Absorption Supplies
Instrument Parts amp Supplies
Atomic Spec Application Notes
Agilent Quick Reference Guide for 77008800 ICP-MS (pub 5990-8182EN)
Agilent Atomic Spec Supplies Catalogue (pub 5990-8767EN)
Agilent Consumables Catalogue (pub 5990-6674EN)
Instrument User Manuals
42
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Sample Introduction bull Contamination in the spray chamber
ndash When was the spray chamber cleaned
bull Any blockages in the nebulizer injector
ndash Check for stable aerosol formation
bull Air leaks in spray chamber end cap or connecting tubes
ndash Are they in good condition with tight connections
bull Damaged pump tubes
ndash When did you check the pump tubes
bull Is the pump speed too slow
ndash Low pump speeds may cause signal pulsation
ndash If required use narrower bore pump tube and increase pump speed
bull Samples have a high TDS content
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
26
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Memory effects
bull If possible avoid running high concentrations of these analytes
(Ag Au B Hg Mo Si Sn W Zn Zr)
ndash Maybe necessary to pre-dilute samples (if known to be high in concentration)
bull Ensure an adequate rinse time
ndash Should be at least equal to the sample uptake delay
(30-40 seconds typical)
bull May require an acidified rinse solution between samples
(2 HNO3)
bull Other strategies to minimize memory effects
ndash Use an inert spray chamber
ndash Use the ISIS to introduce discrete amounts of sample This means
bull Cones are exposed to less sample matrix = improved stability
bull Less memorycarry-over
bull Reduced uptake amp rinse times = faster measurement
27
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy - Why is This Important
What does ldquoAccuracyrdquo mean
ndash Ability to get the ldquorightrdquo answer for the sample
ndash Heavily dependent on operatorrsquos skill
Why is this important
ndash User loses confidence in the system
ndash Your reputationhellip
bull Customerrsquos question the results
bull Poor performance in ldquoround robinrdquo comparisons
How do You Confirm Accuracy
ndash Check the result for a prepared standard
ndash Measure a certified reference material
ndash Use other quality control checks to check analysis
28
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Calibration standards properly prepared
bull See earlier recommendations ndash important to match to samples prepare
accurately and use them ldquofreshrdquo
ndash Any interferences impacting on results
ndash Use matched standards or standard additions
ndash Ensure isotope selected has no polyatomic interferences
ndash If necessary use ORS3
ndash Precision optimized
bull Optimum signal to noise performance improves accuracy
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
29
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Reprocess data post
run using an
alternate internal
standard
bull Ensure Internal
Standard used is
similar in mass
bull Check whether the
Internal Standard is
present in the
sample
ndash If necessary do a Semi-
Quant measurement
bull Dilute with cal blk
matrix
30
Accuracy ndash Suspect Internal Standard Recovery
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Sample preparation
bull Is the most appropriate digestion being used
bull Are all of the analytes being quantitatively (and reproducibly) extracted and
dissolved
ndash Many digestions are only partial extracts ndash efficiency will vary with the
sample matrix
ndash Some volatile analytes may be ldquolostrdquo during digestion
bull Confirm by taking a solid certified reference material
through your preparation and analysis procedure
bull Is the digest stable ndash or are you seeing any precipitates or a suspension
bull Do you see any potential contamination from either reagents or the digestion
equipment eg especially with Si B or Ca
bull Include a ldquoReagent Blankrdquo with every sample batch to
monitor
31
ICP-MS Maintenance amp Trouble Shooting
May 2012
Laboratory environment can have
direct impact on quality of results
bull Clean uncluttered work area
bull Proper ventilation
bull Safety considerations
bull Instrument lifetime consideration
ICP-MS Maintenance amp Trouble Shooting
May 2012 32
Laboratory Environment
ICP-MS ndash Potential Autosampler Issues
ndash More customers use autosamplers with ICP for automation
ndash Issues to consider
bull Long transfer tube between sampler and ICP-MS
ndash May need to program a longer sample uptake delay
ndash May exacerbate problems with memory effects
ndash Use ldquoFast Pumprdquo during sample uptake delay
bull Caution ndash not always possible
Not recommended with high TDS samples and organics
bull Ensure probe diameter is appropriate for sample matrix
ndash Use wider bore for high TDS or viscous samples
bull Sample stability - potential for sample changes while uncovered in racks ndash impacts accuracy
ndash Dust ingress can introduce contamination
ndash Sample evaporation may occur during long unattended runs
ndash Sediment in the sample may settle out esp with wear metals or suspensions
bull Ensure transfer line to ICP-MS is in good condition
ndash Kinks in the line may cause poor uptake or pulsing in the sample
ndash Impacts on precision and accuracy
33
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sample Throughput ndash What to Check
ndash Samples fully digested
bull No excess particulates in the sample that may cause blockage
ndash Sample Introduction System optimized
ndash Capable of handling the TDS levels in the sample
ndash TorchNebulizer cleaned and ready for analysis
ndash Method parameters optimized
bull Sample uptake delay and stabilization times are appropriate ndash optimized
bull Integration time is appropriate for the expected concentration
ndash Use a longer integration time at low concentrations
bull Rinse time is appropriate
bull Use ldquoISISrdquo discrete sampling for faster measurement and faster washout
34
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Handles tough sample matrices better
than any other ICP-MS
ndash Highest plasma temperature (lowest
CeOCe) as standard
ndash HMI (high matrix introduction) allows direct
analysis of difficult samples
eg sea water
bull ORS3 operates in He collision mode to
remove ALL polyatomic interferences
ndash Enables reliable removal of all polyatomic
interferences using a single set of
conditions
ndash Gives lower levels of interference and
better long-term stability HMI gives lower suppression and
better long-term stability
Relative signal (suppression) in undiluted seawater
Long-term stability in undiluted seawater
35
Agilent ICP-MS Performance - Benefits
Best matrix tolerance amp less interferences
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS ndash Recommended Maintenance Schedule
ICP-MS Maintenance amp Trouble Shooting
May 2012 37
These functions
(and more) are
completed as part
of a Preventative
Maintenance
program by an
Agilent Field
Service Engineer
Summary ndash Key Consumables for ICP-MS
Sample preparationpresentation
ndash Peristaltic pump tubing
ndash Transfer and drain tubing
ndash ICP-MS standard solutions
ndash Internal Standard solutions
ndash Torches
ndash Spray chambers
ndash Nebulizers
Ion Extraction
ndash Sampler and skimmer cones
Autosampling
ndash Sample tubes racks probes and transfer tubing
ISIS
ndash Peristaltic pump tubing ferrules amp fittings
38
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sample Introduction
Key consumables requiring frequent replacement
bull Pump tubing
bull Torches and quartz transfer tube
bull Nebulizers
bull Spray chambers
bull Interface cones (skimmer amp sampler)
bull Transfer amp connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalogue
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24406(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 39
Autosampler Supplies
Key consumables requiring frequent replacement
ndash Peristaltic pump tubing
ndash Sample racks
ndash Sample tubes
ndash Spare probes
ndash Standard racks
ndash Connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24407(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 40
ISIS Supplies
Key consumables requiring frequent replacement
bull Peristaltic pump tubing
bull Ferrules and fittings
bull Valving
For ISIS Hydride Generation Accessory
bull Membrane filter
bull Concentric nebulizer
bull Gas-liquid separator
bull Other tubing and connectors
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceProductListingaspxcat=SubCat2ECS_24437(Agilent)amppcat=SubCat1ECS_24407(Agilent)amprcat=ClassECS_22674(Agilent)
41
ICP-MS Maintenance amp Trouble Shooting
May 2012
Where to Find the Right Consumable Analytical Consumables Agilent Assist
Consumables amp Supplies Instrument Sales ampServices 1-800-227-9770 (Option 11) 1-800-227-9770 (Option 13) wwwagilentcomchemcontactus wwwagilentcomchemcontactus
On-Line resources
ICP-MS Supplies
2nd Edition Speciation Handbook
ICP-MS Journal Archives
Recorded Agilent e-Seminars
ICP-OES Supplies
Atomic Absorption Supplies
Instrument Parts amp Supplies
Atomic Spec Application Notes
Agilent Quick Reference Guide for 77008800 ICP-MS (pub 5990-8182EN)
Agilent Atomic Spec Supplies Catalogue (pub 5990-8767EN)
Agilent Consumables Catalogue (pub 5990-6674EN)
Instrument User Manuals
42
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Precision ndash What to Check
ndash Memory effects
bull If possible avoid running high concentrations of these analytes
(Ag Au B Hg Mo Si Sn W Zn Zr)
ndash Maybe necessary to pre-dilute samples (if known to be high in concentration)
bull Ensure an adequate rinse time
ndash Should be at least equal to the sample uptake delay
(30-40 seconds typical)
bull May require an acidified rinse solution between samples
(2 HNO3)
bull Other strategies to minimize memory effects
ndash Use an inert spray chamber
ndash Use the ISIS to introduce discrete amounts of sample This means
bull Cones are exposed to less sample matrix = improved stability
bull Less memorycarry-over
bull Reduced uptake amp rinse times = faster measurement
27
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy - Why is This Important
What does ldquoAccuracyrdquo mean
ndash Ability to get the ldquorightrdquo answer for the sample
ndash Heavily dependent on operatorrsquos skill
Why is this important
ndash User loses confidence in the system
ndash Your reputationhellip
bull Customerrsquos question the results
bull Poor performance in ldquoround robinrdquo comparisons
How do You Confirm Accuracy
ndash Check the result for a prepared standard
ndash Measure a certified reference material
ndash Use other quality control checks to check analysis
28
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Calibration standards properly prepared
bull See earlier recommendations ndash important to match to samples prepare
accurately and use them ldquofreshrdquo
ndash Any interferences impacting on results
ndash Use matched standards or standard additions
ndash Ensure isotope selected has no polyatomic interferences
ndash If necessary use ORS3
ndash Precision optimized
bull Optimum signal to noise performance improves accuracy
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
29
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Reprocess data post
run using an
alternate internal
standard
bull Ensure Internal
Standard used is
similar in mass
bull Check whether the
Internal Standard is
present in the
sample
ndash If necessary do a Semi-
Quant measurement
bull Dilute with cal blk
matrix
30
Accuracy ndash Suspect Internal Standard Recovery
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Sample preparation
bull Is the most appropriate digestion being used
bull Are all of the analytes being quantitatively (and reproducibly) extracted and
dissolved
ndash Many digestions are only partial extracts ndash efficiency will vary with the
sample matrix
ndash Some volatile analytes may be ldquolostrdquo during digestion
bull Confirm by taking a solid certified reference material
through your preparation and analysis procedure
bull Is the digest stable ndash or are you seeing any precipitates or a suspension
bull Do you see any potential contamination from either reagents or the digestion
equipment eg especially with Si B or Ca
bull Include a ldquoReagent Blankrdquo with every sample batch to
monitor
31
ICP-MS Maintenance amp Trouble Shooting
May 2012
Laboratory environment can have
direct impact on quality of results
bull Clean uncluttered work area
bull Proper ventilation
bull Safety considerations
bull Instrument lifetime consideration
ICP-MS Maintenance amp Trouble Shooting
May 2012 32
Laboratory Environment
ICP-MS ndash Potential Autosampler Issues
ndash More customers use autosamplers with ICP for automation
ndash Issues to consider
bull Long transfer tube between sampler and ICP-MS
ndash May need to program a longer sample uptake delay
ndash May exacerbate problems with memory effects
ndash Use ldquoFast Pumprdquo during sample uptake delay
bull Caution ndash not always possible
Not recommended with high TDS samples and organics
bull Ensure probe diameter is appropriate for sample matrix
ndash Use wider bore for high TDS or viscous samples
bull Sample stability - potential for sample changes while uncovered in racks ndash impacts accuracy
ndash Dust ingress can introduce contamination
ndash Sample evaporation may occur during long unattended runs
ndash Sediment in the sample may settle out esp with wear metals or suspensions
bull Ensure transfer line to ICP-MS is in good condition
ndash Kinks in the line may cause poor uptake or pulsing in the sample
ndash Impacts on precision and accuracy
33
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sample Throughput ndash What to Check
ndash Samples fully digested
bull No excess particulates in the sample that may cause blockage
ndash Sample Introduction System optimized
ndash Capable of handling the TDS levels in the sample
ndash TorchNebulizer cleaned and ready for analysis
ndash Method parameters optimized
bull Sample uptake delay and stabilization times are appropriate ndash optimized
bull Integration time is appropriate for the expected concentration
ndash Use a longer integration time at low concentrations
bull Rinse time is appropriate
bull Use ldquoISISrdquo discrete sampling for faster measurement and faster washout
34
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Handles tough sample matrices better
than any other ICP-MS
ndash Highest plasma temperature (lowest
CeOCe) as standard
ndash HMI (high matrix introduction) allows direct
analysis of difficult samples
eg sea water
bull ORS3 operates in He collision mode to
remove ALL polyatomic interferences
ndash Enables reliable removal of all polyatomic
interferences using a single set of
conditions
ndash Gives lower levels of interference and
better long-term stability HMI gives lower suppression and
better long-term stability
Relative signal (suppression) in undiluted seawater
Long-term stability in undiluted seawater
35
Agilent ICP-MS Performance - Benefits
Best matrix tolerance amp less interferences
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS ndash Recommended Maintenance Schedule
ICP-MS Maintenance amp Trouble Shooting
May 2012 37
These functions
(and more) are
completed as part
of a Preventative
Maintenance
program by an
Agilent Field
Service Engineer
Summary ndash Key Consumables for ICP-MS
Sample preparationpresentation
ndash Peristaltic pump tubing
ndash Transfer and drain tubing
ndash ICP-MS standard solutions
ndash Internal Standard solutions
ndash Torches
ndash Spray chambers
ndash Nebulizers
Ion Extraction
ndash Sampler and skimmer cones
Autosampling
ndash Sample tubes racks probes and transfer tubing
ISIS
ndash Peristaltic pump tubing ferrules amp fittings
38
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sample Introduction
Key consumables requiring frequent replacement
bull Pump tubing
bull Torches and quartz transfer tube
bull Nebulizers
bull Spray chambers
bull Interface cones (skimmer amp sampler)
bull Transfer amp connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalogue
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24406(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 39
Autosampler Supplies
Key consumables requiring frequent replacement
ndash Peristaltic pump tubing
ndash Sample racks
ndash Sample tubes
ndash Spare probes
ndash Standard racks
ndash Connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24407(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 40
ISIS Supplies
Key consumables requiring frequent replacement
bull Peristaltic pump tubing
bull Ferrules and fittings
bull Valving
For ISIS Hydride Generation Accessory
bull Membrane filter
bull Concentric nebulizer
bull Gas-liquid separator
bull Other tubing and connectors
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceProductListingaspxcat=SubCat2ECS_24437(Agilent)amppcat=SubCat1ECS_24407(Agilent)amprcat=ClassECS_22674(Agilent)
41
ICP-MS Maintenance amp Trouble Shooting
May 2012
Where to Find the Right Consumable Analytical Consumables Agilent Assist
Consumables amp Supplies Instrument Sales ampServices 1-800-227-9770 (Option 11) 1-800-227-9770 (Option 13) wwwagilentcomchemcontactus wwwagilentcomchemcontactus
On-Line resources
ICP-MS Supplies
2nd Edition Speciation Handbook
ICP-MS Journal Archives
Recorded Agilent e-Seminars
ICP-OES Supplies
Atomic Absorption Supplies
Instrument Parts amp Supplies
Atomic Spec Application Notes
Agilent Quick Reference Guide for 77008800 ICP-MS (pub 5990-8182EN)
Agilent Atomic Spec Supplies Catalogue (pub 5990-8767EN)
Agilent Consumables Catalogue (pub 5990-6674EN)
Instrument User Manuals
42
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy - Why is This Important
What does ldquoAccuracyrdquo mean
ndash Ability to get the ldquorightrdquo answer for the sample
ndash Heavily dependent on operatorrsquos skill
Why is this important
ndash User loses confidence in the system
ndash Your reputationhellip
bull Customerrsquos question the results
bull Poor performance in ldquoround robinrdquo comparisons
How do You Confirm Accuracy
ndash Check the result for a prepared standard
ndash Measure a certified reference material
ndash Use other quality control checks to check analysis
28
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Calibration standards properly prepared
bull See earlier recommendations ndash important to match to samples prepare
accurately and use them ldquofreshrdquo
ndash Any interferences impacting on results
ndash Use matched standards or standard additions
ndash Ensure isotope selected has no polyatomic interferences
ndash If necessary use ORS3
ndash Precision optimized
bull Optimum signal to noise performance improves accuracy
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
29
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Reprocess data post
run using an
alternate internal
standard
bull Ensure Internal
Standard used is
similar in mass
bull Check whether the
Internal Standard is
present in the
sample
ndash If necessary do a Semi-
Quant measurement
bull Dilute with cal blk
matrix
30
Accuracy ndash Suspect Internal Standard Recovery
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Sample preparation
bull Is the most appropriate digestion being used
bull Are all of the analytes being quantitatively (and reproducibly) extracted and
dissolved
ndash Many digestions are only partial extracts ndash efficiency will vary with the
sample matrix
ndash Some volatile analytes may be ldquolostrdquo during digestion
bull Confirm by taking a solid certified reference material
through your preparation and analysis procedure
bull Is the digest stable ndash or are you seeing any precipitates or a suspension
bull Do you see any potential contamination from either reagents or the digestion
equipment eg especially with Si B or Ca
bull Include a ldquoReagent Blankrdquo with every sample batch to
monitor
31
ICP-MS Maintenance amp Trouble Shooting
May 2012
Laboratory environment can have
direct impact on quality of results
bull Clean uncluttered work area
bull Proper ventilation
bull Safety considerations
bull Instrument lifetime consideration
ICP-MS Maintenance amp Trouble Shooting
May 2012 32
Laboratory Environment
ICP-MS ndash Potential Autosampler Issues
ndash More customers use autosamplers with ICP for automation
ndash Issues to consider
bull Long transfer tube between sampler and ICP-MS
ndash May need to program a longer sample uptake delay
ndash May exacerbate problems with memory effects
ndash Use ldquoFast Pumprdquo during sample uptake delay
bull Caution ndash not always possible
Not recommended with high TDS samples and organics
bull Ensure probe diameter is appropriate for sample matrix
ndash Use wider bore for high TDS or viscous samples
bull Sample stability - potential for sample changes while uncovered in racks ndash impacts accuracy
ndash Dust ingress can introduce contamination
ndash Sample evaporation may occur during long unattended runs
ndash Sediment in the sample may settle out esp with wear metals or suspensions
bull Ensure transfer line to ICP-MS is in good condition
ndash Kinks in the line may cause poor uptake or pulsing in the sample
ndash Impacts on precision and accuracy
33
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sample Throughput ndash What to Check
ndash Samples fully digested
bull No excess particulates in the sample that may cause blockage
ndash Sample Introduction System optimized
ndash Capable of handling the TDS levels in the sample
ndash TorchNebulizer cleaned and ready for analysis
ndash Method parameters optimized
bull Sample uptake delay and stabilization times are appropriate ndash optimized
bull Integration time is appropriate for the expected concentration
ndash Use a longer integration time at low concentrations
bull Rinse time is appropriate
bull Use ldquoISISrdquo discrete sampling for faster measurement and faster washout
34
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Handles tough sample matrices better
than any other ICP-MS
ndash Highest plasma temperature (lowest
CeOCe) as standard
ndash HMI (high matrix introduction) allows direct
analysis of difficult samples
eg sea water
bull ORS3 operates in He collision mode to
remove ALL polyatomic interferences
ndash Enables reliable removal of all polyatomic
interferences using a single set of
conditions
ndash Gives lower levels of interference and
better long-term stability HMI gives lower suppression and
better long-term stability
Relative signal (suppression) in undiluted seawater
Long-term stability in undiluted seawater
35
Agilent ICP-MS Performance - Benefits
Best matrix tolerance amp less interferences
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS ndash Recommended Maintenance Schedule
ICP-MS Maintenance amp Trouble Shooting
May 2012 37
These functions
(and more) are
completed as part
of a Preventative
Maintenance
program by an
Agilent Field
Service Engineer
Summary ndash Key Consumables for ICP-MS
Sample preparationpresentation
ndash Peristaltic pump tubing
ndash Transfer and drain tubing
ndash ICP-MS standard solutions
ndash Internal Standard solutions
ndash Torches
ndash Spray chambers
ndash Nebulizers
Ion Extraction
ndash Sampler and skimmer cones
Autosampling
ndash Sample tubes racks probes and transfer tubing
ISIS
ndash Peristaltic pump tubing ferrules amp fittings
38
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sample Introduction
Key consumables requiring frequent replacement
bull Pump tubing
bull Torches and quartz transfer tube
bull Nebulizers
bull Spray chambers
bull Interface cones (skimmer amp sampler)
bull Transfer amp connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalogue
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24406(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 39
Autosampler Supplies
Key consumables requiring frequent replacement
ndash Peristaltic pump tubing
ndash Sample racks
ndash Sample tubes
ndash Spare probes
ndash Standard racks
ndash Connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24407(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 40
ISIS Supplies
Key consumables requiring frequent replacement
bull Peristaltic pump tubing
bull Ferrules and fittings
bull Valving
For ISIS Hydride Generation Accessory
bull Membrane filter
bull Concentric nebulizer
bull Gas-liquid separator
bull Other tubing and connectors
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceProductListingaspxcat=SubCat2ECS_24437(Agilent)amppcat=SubCat1ECS_24407(Agilent)amprcat=ClassECS_22674(Agilent)
41
ICP-MS Maintenance amp Trouble Shooting
May 2012
Where to Find the Right Consumable Analytical Consumables Agilent Assist
Consumables amp Supplies Instrument Sales ampServices 1-800-227-9770 (Option 11) 1-800-227-9770 (Option 13) wwwagilentcomchemcontactus wwwagilentcomchemcontactus
On-Line resources
ICP-MS Supplies
2nd Edition Speciation Handbook
ICP-MS Journal Archives
Recorded Agilent e-Seminars
ICP-OES Supplies
Atomic Absorption Supplies
Instrument Parts amp Supplies
Atomic Spec Application Notes
Agilent Quick Reference Guide for 77008800 ICP-MS (pub 5990-8182EN)
Agilent Atomic Spec Supplies Catalogue (pub 5990-8767EN)
Agilent Consumables Catalogue (pub 5990-6674EN)
Instrument User Manuals
42
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Calibration standards properly prepared
bull See earlier recommendations ndash important to match to samples prepare
accurately and use them ldquofreshrdquo
ndash Any interferences impacting on results
ndash Use matched standards or standard additions
ndash Ensure isotope selected has no polyatomic interferences
ndash If necessary use ORS3
ndash Precision optimized
bull Optimum signal to noise performance improves accuracy
bull Measuring at an appropriate concentration
ndash Close to the detection limit noise is high and precisionaccuracy is impacted
29
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Reprocess data post
run using an
alternate internal
standard
bull Ensure Internal
Standard used is
similar in mass
bull Check whether the
Internal Standard is
present in the
sample
ndash If necessary do a Semi-
Quant measurement
bull Dilute with cal blk
matrix
30
Accuracy ndash Suspect Internal Standard Recovery
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Sample preparation
bull Is the most appropriate digestion being used
bull Are all of the analytes being quantitatively (and reproducibly) extracted and
dissolved
ndash Many digestions are only partial extracts ndash efficiency will vary with the
sample matrix
ndash Some volatile analytes may be ldquolostrdquo during digestion
bull Confirm by taking a solid certified reference material
through your preparation and analysis procedure
bull Is the digest stable ndash or are you seeing any precipitates or a suspension
bull Do you see any potential contamination from either reagents or the digestion
equipment eg especially with Si B or Ca
bull Include a ldquoReagent Blankrdquo with every sample batch to
monitor
31
ICP-MS Maintenance amp Trouble Shooting
May 2012
Laboratory environment can have
direct impact on quality of results
bull Clean uncluttered work area
bull Proper ventilation
bull Safety considerations
bull Instrument lifetime consideration
ICP-MS Maintenance amp Trouble Shooting
May 2012 32
Laboratory Environment
ICP-MS ndash Potential Autosampler Issues
ndash More customers use autosamplers with ICP for automation
ndash Issues to consider
bull Long transfer tube between sampler and ICP-MS
ndash May need to program a longer sample uptake delay
ndash May exacerbate problems with memory effects
ndash Use ldquoFast Pumprdquo during sample uptake delay
bull Caution ndash not always possible
Not recommended with high TDS samples and organics
bull Ensure probe diameter is appropriate for sample matrix
ndash Use wider bore for high TDS or viscous samples
bull Sample stability - potential for sample changes while uncovered in racks ndash impacts accuracy
ndash Dust ingress can introduce contamination
ndash Sample evaporation may occur during long unattended runs
ndash Sediment in the sample may settle out esp with wear metals or suspensions
bull Ensure transfer line to ICP-MS is in good condition
ndash Kinks in the line may cause poor uptake or pulsing in the sample
ndash Impacts on precision and accuracy
33
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sample Throughput ndash What to Check
ndash Samples fully digested
bull No excess particulates in the sample that may cause blockage
ndash Sample Introduction System optimized
ndash Capable of handling the TDS levels in the sample
ndash TorchNebulizer cleaned and ready for analysis
ndash Method parameters optimized
bull Sample uptake delay and stabilization times are appropriate ndash optimized
bull Integration time is appropriate for the expected concentration
ndash Use a longer integration time at low concentrations
bull Rinse time is appropriate
bull Use ldquoISISrdquo discrete sampling for faster measurement and faster washout
34
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Handles tough sample matrices better
than any other ICP-MS
ndash Highest plasma temperature (lowest
CeOCe) as standard
ndash HMI (high matrix introduction) allows direct
analysis of difficult samples
eg sea water
bull ORS3 operates in He collision mode to
remove ALL polyatomic interferences
ndash Enables reliable removal of all polyatomic
interferences using a single set of
conditions
ndash Gives lower levels of interference and
better long-term stability HMI gives lower suppression and
better long-term stability
Relative signal (suppression) in undiluted seawater
Long-term stability in undiluted seawater
35
Agilent ICP-MS Performance - Benefits
Best matrix tolerance amp less interferences
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS ndash Recommended Maintenance Schedule
ICP-MS Maintenance amp Trouble Shooting
May 2012 37
These functions
(and more) are
completed as part
of a Preventative
Maintenance
program by an
Agilent Field
Service Engineer
Summary ndash Key Consumables for ICP-MS
Sample preparationpresentation
ndash Peristaltic pump tubing
ndash Transfer and drain tubing
ndash ICP-MS standard solutions
ndash Internal Standard solutions
ndash Torches
ndash Spray chambers
ndash Nebulizers
Ion Extraction
ndash Sampler and skimmer cones
Autosampling
ndash Sample tubes racks probes and transfer tubing
ISIS
ndash Peristaltic pump tubing ferrules amp fittings
38
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sample Introduction
Key consumables requiring frequent replacement
bull Pump tubing
bull Torches and quartz transfer tube
bull Nebulizers
bull Spray chambers
bull Interface cones (skimmer amp sampler)
bull Transfer amp connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalogue
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24406(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 39
Autosampler Supplies
Key consumables requiring frequent replacement
ndash Peristaltic pump tubing
ndash Sample racks
ndash Sample tubes
ndash Spare probes
ndash Standard racks
ndash Connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24407(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 40
ISIS Supplies
Key consumables requiring frequent replacement
bull Peristaltic pump tubing
bull Ferrules and fittings
bull Valving
For ISIS Hydride Generation Accessory
bull Membrane filter
bull Concentric nebulizer
bull Gas-liquid separator
bull Other tubing and connectors
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceProductListingaspxcat=SubCat2ECS_24437(Agilent)amppcat=SubCat1ECS_24407(Agilent)amprcat=ClassECS_22674(Agilent)
41
ICP-MS Maintenance amp Trouble Shooting
May 2012
Where to Find the Right Consumable Analytical Consumables Agilent Assist
Consumables amp Supplies Instrument Sales ampServices 1-800-227-9770 (Option 11) 1-800-227-9770 (Option 13) wwwagilentcomchemcontactus wwwagilentcomchemcontactus
On-Line resources
ICP-MS Supplies
2nd Edition Speciation Handbook
ICP-MS Journal Archives
Recorded Agilent e-Seminars
ICP-OES Supplies
Atomic Absorption Supplies
Instrument Parts amp Supplies
Atomic Spec Application Notes
Agilent Quick Reference Guide for 77008800 ICP-MS (pub 5990-8182EN)
Agilent Atomic Spec Supplies Catalogue (pub 5990-8767EN)
Agilent Consumables Catalogue (pub 5990-6674EN)
Instrument User Manuals
42
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Reprocess data post
run using an
alternate internal
standard
bull Ensure Internal
Standard used is
similar in mass
bull Check whether the
Internal Standard is
present in the
sample
ndash If necessary do a Semi-
Quant measurement
bull Dilute with cal blk
matrix
30
Accuracy ndash Suspect Internal Standard Recovery
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Sample preparation
bull Is the most appropriate digestion being used
bull Are all of the analytes being quantitatively (and reproducibly) extracted and
dissolved
ndash Many digestions are only partial extracts ndash efficiency will vary with the
sample matrix
ndash Some volatile analytes may be ldquolostrdquo during digestion
bull Confirm by taking a solid certified reference material
through your preparation and analysis procedure
bull Is the digest stable ndash or are you seeing any precipitates or a suspension
bull Do you see any potential contamination from either reagents or the digestion
equipment eg especially with Si B or Ca
bull Include a ldquoReagent Blankrdquo with every sample batch to
monitor
31
ICP-MS Maintenance amp Trouble Shooting
May 2012
Laboratory environment can have
direct impact on quality of results
bull Clean uncluttered work area
bull Proper ventilation
bull Safety considerations
bull Instrument lifetime consideration
ICP-MS Maintenance amp Trouble Shooting
May 2012 32
Laboratory Environment
ICP-MS ndash Potential Autosampler Issues
ndash More customers use autosamplers with ICP for automation
ndash Issues to consider
bull Long transfer tube between sampler and ICP-MS
ndash May need to program a longer sample uptake delay
ndash May exacerbate problems with memory effects
ndash Use ldquoFast Pumprdquo during sample uptake delay
bull Caution ndash not always possible
Not recommended with high TDS samples and organics
bull Ensure probe diameter is appropriate for sample matrix
ndash Use wider bore for high TDS or viscous samples
bull Sample stability - potential for sample changes while uncovered in racks ndash impacts accuracy
ndash Dust ingress can introduce contamination
ndash Sample evaporation may occur during long unattended runs
ndash Sediment in the sample may settle out esp with wear metals or suspensions
bull Ensure transfer line to ICP-MS is in good condition
ndash Kinks in the line may cause poor uptake or pulsing in the sample
ndash Impacts on precision and accuracy
33
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sample Throughput ndash What to Check
ndash Samples fully digested
bull No excess particulates in the sample that may cause blockage
ndash Sample Introduction System optimized
ndash Capable of handling the TDS levels in the sample
ndash TorchNebulizer cleaned and ready for analysis
ndash Method parameters optimized
bull Sample uptake delay and stabilization times are appropriate ndash optimized
bull Integration time is appropriate for the expected concentration
ndash Use a longer integration time at low concentrations
bull Rinse time is appropriate
bull Use ldquoISISrdquo discrete sampling for faster measurement and faster washout
34
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Handles tough sample matrices better
than any other ICP-MS
ndash Highest plasma temperature (lowest
CeOCe) as standard
ndash HMI (high matrix introduction) allows direct
analysis of difficult samples
eg sea water
bull ORS3 operates in He collision mode to
remove ALL polyatomic interferences
ndash Enables reliable removal of all polyatomic
interferences using a single set of
conditions
ndash Gives lower levels of interference and
better long-term stability HMI gives lower suppression and
better long-term stability
Relative signal (suppression) in undiluted seawater
Long-term stability in undiluted seawater
35
Agilent ICP-MS Performance - Benefits
Best matrix tolerance amp less interferences
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS ndash Recommended Maintenance Schedule
ICP-MS Maintenance amp Trouble Shooting
May 2012 37
These functions
(and more) are
completed as part
of a Preventative
Maintenance
program by an
Agilent Field
Service Engineer
Summary ndash Key Consumables for ICP-MS
Sample preparationpresentation
ndash Peristaltic pump tubing
ndash Transfer and drain tubing
ndash ICP-MS standard solutions
ndash Internal Standard solutions
ndash Torches
ndash Spray chambers
ndash Nebulizers
Ion Extraction
ndash Sampler and skimmer cones
Autosampling
ndash Sample tubes racks probes and transfer tubing
ISIS
ndash Peristaltic pump tubing ferrules amp fittings
38
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sample Introduction
Key consumables requiring frequent replacement
bull Pump tubing
bull Torches and quartz transfer tube
bull Nebulizers
bull Spray chambers
bull Interface cones (skimmer amp sampler)
bull Transfer amp connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalogue
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24406(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 39
Autosampler Supplies
Key consumables requiring frequent replacement
ndash Peristaltic pump tubing
ndash Sample racks
ndash Sample tubes
ndash Spare probes
ndash Standard racks
ndash Connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24407(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 40
ISIS Supplies
Key consumables requiring frequent replacement
bull Peristaltic pump tubing
bull Ferrules and fittings
bull Valving
For ISIS Hydride Generation Accessory
bull Membrane filter
bull Concentric nebulizer
bull Gas-liquid separator
bull Other tubing and connectors
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceProductListingaspxcat=SubCat2ECS_24437(Agilent)amppcat=SubCat1ECS_24407(Agilent)amprcat=ClassECS_22674(Agilent)
41
ICP-MS Maintenance amp Trouble Shooting
May 2012
Where to Find the Right Consumable Analytical Consumables Agilent Assist
Consumables amp Supplies Instrument Sales ampServices 1-800-227-9770 (Option 11) 1-800-227-9770 (Option 13) wwwagilentcomchemcontactus wwwagilentcomchemcontactus
On-Line resources
ICP-MS Supplies
2nd Edition Speciation Handbook
ICP-MS Journal Archives
Recorded Agilent e-Seminars
ICP-OES Supplies
Atomic Absorption Supplies
Instrument Parts amp Supplies
Atomic Spec Application Notes
Agilent Quick Reference Guide for 77008800 ICP-MS (pub 5990-8182EN)
Agilent Atomic Spec Supplies Catalogue (pub 5990-8767EN)
Agilent Consumables Catalogue (pub 5990-6674EN)
Instrument User Manuals
42
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
Accuracy ndash What to Check
ndash Sample preparation
bull Is the most appropriate digestion being used
bull Are all of the analytes being quantitatively (and reproducibly) extracted and
dissolved
ndash Many digestions are only partial extracts ndash efficiency will vary with the
sample matrix
ndash Some volatile analytes may be ldquolostrdquo during digestion
bull Confirm by taking a solid certified reference material
through your preparation and analysis procedure
bull Is the digest stable ndash or are you seeing any precipitates or a suspension
bull Do you see any potential contamination from either reagents or the digestion
equipment eg especially with Si B or Ca
bull Include a ldquoReagent Blankrdquo with every sample batch to
monitor
31
ICP-MS Maintenance amp Trouble Shooting
May 2012
Laboratory environment can have
direct impact on quality of results
bull Clean uncluttered work area
bull Proper ventilation
bull Safety considerations
bull Instrument lifetime consideration
ICP-MS Maintenance amp Trouble Shooting
May 2012 32
Laboratory Environment
ICP-MS ndash Potential Autosampler Issues
ndash More customers use autosamplers with ICP for automation
ndash Issues to consider
bull Long transfer tube between sampler and ICP-MS
ndash May need to program a longer sample uptake delay
ndash May exacerbate problems with memory effects
ndash Use ldquoFast Pumprdquo during sample uptake delay
bull Caution ndash not always possible
Not recommended with high TDS samples and organics
bull Ensure probe diameter is appropriate for sample matrix
ndash Use wider bore for high TDS or viscous samples
bull Sample stability - potential for sample changes while uncovered in racks ndash impacts accuracy
ndash Dust ingress can introduce contamination
ndash Sample evaporation may occur during long unattended runs
ndash Sediment in the sample may settle out esp with wear metals or suspensions
bull Ensure transfer line to ICP-MS is in good condition
ndash Kinks in the line may cause poor uptake or pulsing in the sample
ndash Impacts on precision and accuracy
33
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sample Throughput ndash What to Check
ndash Samples fully digested
bull No excess particulates in the sample that may cause blockage
ndash Sample Introduction System optimized
ndash Capable of handling the TDS levels in the sample
ndash TorchNebulizer cleaned and ready for analysis
ndash Method parameters optimized
bull Sample uptake delay and stabilization times are appropriate ndash optimized
bull Integration time is appropriate for the expected concentration
ndash Use a longer integration time at low concentrations
bull Rinse time is appropriate
bull Use ldquoISISrdquo discrete sampling for faster measurement and faster washout
34
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Handles tough sample matrices better
than any other ICP-MS
ndash Highest plasma temperature (lowest
CeOCe) as standard
ndash HMI (high matrix introduction) allows direct
analysis of difficult samples
eg sea water
bull ORS3 operates in He collision mode to
remove ALL polyatomic interferences
ndash Enables reliable removal of all polyatomic
interferences using a single set of
conditions
ndash Gives lower levels of interference and
better long-term stability HMI gives lower suppression and
better long-term stability
Relative signal (suppression) in undiluted seawater
Long-term stability in undiluted seawater
35
Agilent ICP-MS Performance - Benefits
Best matrix tolerance amp less interferences
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS ndash Recommended Maintenance Schedule
ICP-MS Maintenance amp Trouble Shooting
May 2012 37
These functions
(and more) are
completed as part
of a Preventative
Maintenance
program by an
Agilent Field
Service Engineer
Summary ndash Key Consumables for ICP-MS
Sample preparationpresentation
ndash Peristaltic pump tubing
ndash Transfer and drain tubing
ndash ICP-MS standard solutions
ndash Internal Standard solutions
ndash Torches
ndash Spray chambers
ndash Nebulizers
Ion Extraction
ndash Sampler and skimmer cones
Autosampling
ndash Sample tubes racks probes and transfer tubing
ISIS
ndash Peristaltic pump tubing ferrules amp fittings
38
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sample Introduction
Key consumables requiring frequent replacement
bull Pump tubing
bull Torches and quartz transfer tube
bull Nebulizers
bull Spray chambers
bull Interface cones (skimmer amp sampler)
bull Transfer amp connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalogue
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24406(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 39
Autosampler Supplies
Key consumables requiring frequent replacement
ndash Peristaltic pump tubing
ndash Sample racks
ndash Sample tubes
ndash Spare probes
ndash Standard racks
ndash Connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24407(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 40
ISIS Supplies
Key consumables requiring frequent replacement
bull Peristaltic pump tubing
bull Ferrules and fittings
bull Valving
For ISIS Hydride Generation Accessory
bull Membrane filter
bull Concentric nebulizer
bull Gas-liquid separator
bull Other tubing and connectors
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceProductListingaspxcat=SubCat2ECS_24437(Agilent)amppcat=SubCat1ECS_24407(Agilent)amprcat=ClassECS_22674(Agilent)
41
ICP-MS Maintenance amp Trouble Shooting
May 2012
Where to Find the Right Consumable Analytical Consumables Agilent Assist
Consumables amp Supplies Instrument Sales ampServices 1-800-227-9770 (Option 11) 1-800-227-9770 (Option 13) wwwagilentcomchemcontactus wwwagilentcomchemcontactus
On-Line resources
ICP-MS Supplies
2nd Edition Speciation Handbook
ICP-MS Journal Archives
Recorded Agilent e-Seminars
ICP-OES Supplies
Atomic Absorption Supplies
Instrument Parts amp Supplies
Atomic Spec Application Notes
Agilent Quick Reference Guide for 77008800 ICP-MS (pub 5990-8182EN)
Agilent Atomic Spec Supplies Catalogue (pub 5990-8767EN)
Agilent Consumables Catalogue (pub 5990-6674EN)
Instrument User Manuals
42
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
Laboratory environment can have
direct impact on quality of results
bull Clean uncluttered work area
bull Proper ventilation
bull Safety considerations
bull Instrument lifetime consideration
ICP-MS Maintenance amp Trouble Shooting
May 2012 32
Laboratory Environment
ICP-MS ndash Potential Autosampler Issues
ndash More customers use autosamplers with ICP for automation
ndash Issues to consider
bull Long transfer tube between sampler and ICP-MS
ndash May need to program a longer sample uptake delay
ndash May exacerbate problems with memory effects
ndash Use ldquoFast Pumprdquo during sample uptake delay
bull Caution ndash not always possible
Not recommended with high TDS samples and organics
bull Ensure probe diameter is appropriate for sample matrix
ndash Use wider bore for high TDS or viscous samples
bull Sample stability - potential for sample changes while uncovered in racks ndash impacts accuracy
ndash Dust ingress can introduce contamination
ndash Sample evaporation may occur during long unattended runs
ndash Sediment in the sample may settle out esp with wear metals or suspensions
bull Ensure transfer line to ICP-MS is in good condition
ndash Kinks in the line may cause poor uptake or pulsing in the sample
ndash Impacts on precision and accuracy
33
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sample Throughput ndash What to Check
ndash Samples fully digested
bull No excess particulates in the sample that may cause blockage
ndash Sample Introduction System optimized
ndash Capable of handling the TDS levels in the sample
ndash TorchNebulizer cleaned and ready for analysis
ndash Method parameters optimized
bull Sample uptake delay and stabilization times are appropriate ndash optimized
bull Integration time is appropriate for the expected concentration
ndash Use a longer integration time at low concentrations
bull Rinse time is appropriate
bull Use ldquoISISrdquo discrete sampling for faster measurement and faster washout
34
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Handles tough sample matrices better
than any other ICP-MS
ndash Highest plasma temperature (lowest
CeOCe) as standard
ndash HMI (high matrix introduction) allows direct
analysis of difficult samples
eg sea water
bull ORS3 operates in He collision mode to
remove ALL polyatomic interferences
ndash Enables reliable removal of all polyatomic
interferences using a single set of
conditions
ndash Gives lower levels of interference and
better long-term stability HMI gives lower suppression and
better long-term stability
Relative signal (suppression) in undiluted seawater
Long-term stability in undiluted seawater
35
Agilent ICP-MS Performance - Benefits
Best matrix tolerance amp less interferences
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS ndash Recommended Maintenance Schedule
ICP-MS Maintenance amp Trouble Shooting
May 2012 37
These functions
(and more) are
completed as part
of a Preventative
Maintenance
program by an
Agilent Field
Service Engineer
Summary ndash Key Consumables for ICP-MS
Sample preparationpresentation
ndash Peristaltic pump tubing
ndash Transfer and drain tubing
ndash ICP-MS standard solutions
ndash Internal Standard solutions
ndash Torches
ndash Spray chambers
ndash Nebulizers
Ion Extraction
ndash Sampler and skimmer cones
Autosampling
ndash Sample tubes racks probes and transfer tubing
ISIS
ndash Peristaltic pump tubing ferrules amp fittings
38
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sample Introduction
Key consumables requiring frequent replacement
bull Pump tubing
bull Torches and quartz transfer tube
bull Nebulizers
bull Spray chambers
bull Interface cones (skimmer amp sampler)
bull Transfer amp connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalogue
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24406(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 39
Autosampler Supplies
Key consumables requiring frequent replacement
ndash Peristaltic pump tubing
ndash Sample racks
ndash Sample tubes
ndash Spare probes
ndash Standard racks
ndash Connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24407(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 40
ISIS Supplies
Key consumables requiring frequent replacement
bull Peristaltic pump tubing
bull Ferrules and fittings
bull Valving
For ISIS Hydride Generation Accessory
bull Membrane filter
bull Concentric nebulizer
bull Gas-liquid separator
bull Other tubing and connectors
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceProductListingaspxcat=SubCat2ECS_24437(Agilent)amppcat=SubCat1ECS_24407(Agilent)amprcat=ClassECS_22674(Agilent)
41
ICP-MS Maintenance amp Trouble Shooting
May 2012
Where to Find the Right Consumable Analytical Consumables Agilent Assist
Consumables amp Supplies Instrument Sales ampServices 1-800-227-9770 (Option 11) 1-800-227-9770 (Option 13) wwwagilentcomchemcontactus wwwagilentcomchemcontactus
On-Line resources
ICP-MS Supplies
2nd Edition Speciation Handbook
ICP-MS Journal Archives
Recorded Agilent e-Seminars
ICP-OES Supplies
Atomic Absorption Supplies
Instrument Parts amp Supplies
Atomic Spec Application Notes
Agilent Quick Reference Guide for 77008800 ICP-MS (pub 5990-8182EN)
Agilent Atomic Spec Supplies Catalogue (pub 5990-8767EN)
Agilent Consumables Catalogue (pub 5990-6674EN)
Instrument User Manuals
42
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS ndash Potential Autosampler Issues
ndash More customers use autosamplers with ICP for automation
ndash Issues to consider
bull Long transfer tube between sampler and ICP-MS
ndash May need to program a longer sample uptake delay
ndash May exacerbate problems with memory effects
ndash Use ldquoFast Pumprdquo during sample uptake delay
bull Caution ndash not always possible
Not recommended with high TDS samples and organics
bull Ensure probe diameter is appropriate for sample matrix
ndash Use wider bore for high TDS or viscous samples
bull Sample stability - potential for sample changes while uncovered in racks ndash impacts accuracy
ndash Dust ingress can introduce contamination
ndash Sample evaporation may occur during long unattended runs
ndash Sediment in the sample may settle out esp with wear metals or suspensions
bull Ensure transfer line to ICP-MS is in good condition
ndash Kinks in the line may cause poor uptake or pulsing in the sample
ndash Impacts on precision and accuracy
33
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sample Throughput ndash What to Check
ndash Samples fully digested
bull No excess particulates in the sample that may cause blockage
ndash Sample Introduction System optimized
ndash Capable of handling the TDS levels in the sample
ndash TorchNebulizer cleaned and ready for analysis
ndash Method parameters optimized
bull Sample uptake delay and stabilization times are appropriate ndash optimized
bull Integration time is appropriate for the expected concentration
ndash Use a longer integration time at low concentrations
bull Rinse time is appropriate
bull Use ldquoISISrdquo discrete sampling for faster measurement and faster washout
34
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Handles tough sample matrices better
than any other ICP-MS
ndash Highest plasma temperature (lowest
CeOCe) as standard
ndash HMI (high matrix introduction) allows direct
analysis of difficult samples
eg sea water
bull ORS3 operates in He collision mode to
remove ALL polyatomic interferences
ndash Enables reliable removal of all polyatomic
interferences using a single set of
conditions
ndash Gives lower levels of interference and
better long-term stability HMI gives lower suppression and
better long-term stability
Relative signal (suppression) in undiluted seawater
Long-term stability in undiluted seawater
35
Agilent ICP-MS Performance - Benefits
Best matrix tolerance amp less interferences
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS ndash Recommended Maintenance Schedule
ICP-MS Maintenance amp Trouble Shooting
May 2012 37
These functions
(and more) are
completed as part
of a Preventative
Maintenance
program by an
Agilent Field
Service Engineer
Summary ndash Key Consumables for ICP-MS
Sample preparationpresentation
ndash Peristaltic pump tubing
ndash Transfer and drain tubing
ndash ICP-MS standard solutions
ndash Internal Standard solutions
ndash Torches
ndash Spray chambers
ndash Nebulizers
Ion Extraction
ndash Sampler and skimmer cones
Autosampling
ndash Sample tubes racks probes and transfer tubing
ISIS
ndash Peristaltic pump tubing ferrules amp fittings
38
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sample Introduction
Key consumables requiring frequent replacement
bull Pump tubing
bull Torches and quartz transfer tube
bull Nebulizers
bull Spray chambers
bull Interface cones (skimmer amp sampler)
bull Transfer amp connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalogue
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24406(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 39
Autosampler Supplies
Key consumables requiring frequent replacement
ndash Peristaltic pump tubing
ndash Sample racks
ndash Sample tubes
ndash Spare probes
ndash Standard racks
ndash Connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24407(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 40
ISIS Supplies
Key consumables requiring frequent replacement
bull Peristaltic pump tubing
bull Ferrules and fittings
bull Valving
For ISIS Hydride Generation Accessory
bull Membrane filter
bull Concentric nebulizer
bull Gas-liquid separator
bull Other tubing and connectors
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceProductListingaspxcat=SubCat2ECS_24437(Agilent)amppcat=SubCat1ECS_24407(Agilent)amprcat=ClassECS_22674(Agilent)
41
ICP-MS Maintenance amp Trouble Shooting
May 2012
Where to Find the Right Consumable Analytical Consumables Agilent Assist
Consumables amp Supplies Instrument Sales ampServices 1-800-227-9770 (Option 11) 1-800-227-9770 (Option 13) wwwagilentcomchemcontactus wwwagilentcomchemcontactus
On-Line resources
ICP-MS Supplies
2nd Edition Speciation Handbook
ICP-MS Journal Archives
Recorded Agilent e-Seminars
ICP-OES Supplies
Atomic Absorption Supplies
Instrument Parts amp Supplies
Atomic Spec Application Notes
Agilent Quick Reference Guide for 77008800 ICP-MS (pub 5990-8182EN)
Agilent Atomic Spec Supplies Catalogue (pub 5990-8767EN)
Agilent Consumables Catalogue (pub 5990-6674EN)
Instrument User Manuals
42
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
Sample Throughput ndash What to Check
ndash Samples fully digested
bull No excess particulates in the sample that may cause blockage
ndash Sample Introduction System optimized
ndash Capable of handling the TDS levels in the sample
ndash TorchNebulizer cleaned and ready for analysis
ndash Method parameters optimized
bull Sample uptake delay and stabilization times are appropriate ndash optimized
bull Integration time is appropriate for the expected concentration
ndash Use a longer integration time at low concentrations
bull Rinse time is appropriate
bull Use ldquoISISrdquo discrete sampling for faster measurement and faster washout
34
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Handles tough sample matrices better
than any other ICP-MS
ndash Highest plasma temperature (lowest
CeOCe) as standard
ndash HMI (high matrix introduction) allows direct
analysis of difficult samples
eg sea water
bull ORS3 operates in He collision mode to
remove ALL polyatomic interferences
ndash Enables reliable removal of all polyatomic
interferences using a single set of
conditions
ndash Gives lower levels of interference and
better long-term stability HMI gives lower suppression and
better long-term stability
Relative signal (suppression) in undiluted seawater
Long-term stability in undiluted seawater
35
Agilent ICP-MS Performance - Benefits
Best matrix tolerance amp less interferences
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS ndash Recommended Maintenance Schedule
ICP-MS Maintenance amp Trouble Shooting
May 2012 37
These functions
(and more) are
completed as part
of a Preventative
Maintenance
program by an
Agilent Field
Service Engineer
Summary ndash Key Consumables for ICP-MS
Sample preparationpresentation
ndash Peristaltic pump tubing
ndash Transfer and drain tubing
ndash ICP-MS standard solutions
ndash Internal Standard solutions
ndash Torches
ndash Spray chambers
ndash Nebulizers
Ion Extraction
ndash Sampler and skimmer cones
Autosampling
ndash Sample tubes racks probes and transfer tubing
ISIS
ndash Peristaltic pump tubing ferrules amp fittings
38
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sample Introduction
Key consumables requiring frequent replacement
bull Pump tubing
bull Torches and quartz transfer tube
bull Nebulizers
bull Spray chambers
bull Interface cones (skimmer amp sampler)
bull Transfer amp connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalogue
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24406(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 39
Autosampler Supplies
Key consumables requiring frequent replacement
ndash Peristaltic pump tubing
ndash Sample racks
ndash Sample tubes
ndash Spare probes
ndash Standard racks
ndash Connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24407(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 40
ISIS Supplies
Key consumables requiring frequent replacement
bull Peristaltic pump tubing
bull Ferrules and fittings
bull Valving
For ISIS Hydride Generation Accessory
bull Membrane filter
bull Concentric nebulizer
bull Gas-liquid separator
bull Other tubing and connectors
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceProductListingaspxcat=SubCat2ECS_24437(Agilent)amppcat=SubCat1ECS_24407(Agilent)amprcat=ClassECS_22674(Agilent)
41
ICP-MS Maintenance amp Trouble Shooting
May 2012
Where to Find the Right Consumable Analytical Consumables Agilent Assist
Consumables amp Supplies Instrument Sales ampServices 1-800-227-9770 (Option 11) 1-800-227-9770 (Option 13) wwwagilentcomchemcontactus wwwagilentcomchemcontactus
On-Line resources
ICP-MS Supplies
2nd Edition Speciation Handbook
ICP-MS Journal Archives
Recorded Agilent e-Seminars
ICP-OES Supplies
Atomic Absorption Supplies
Instrument Parts amp Supplies
Atomic Spec Application Notes
Agilent Quick Reference Guide for 77008800 ICP-MS (pub 5990-8182EN)
Agilent Atomic Spec Supplies Catalogue (pub 5990-8767EN)
Agilent Consumables Catalogue (pub 5990-6674EN)
Instrument User Manuals
42
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Handles tough sample matrices better
than any other ICP-MS
ndash Highest plasma temperature (lowest
CeOCe) as standard
ndash HMI (high matrix introduction) allows direct
analysis of difficult samples
eg sea water
bull ORS3 operates in He collision mode to
remove ALL polyatomic interferences
ndash Enables reliable removal of all polyatomic
interferences using a single set of
conditions
ndash Gives lower levels of interference and
better long-term stability HMI gives lower suppression and
better long-term stability
Relative signal (suppression) in undiluted seawater
Long-term stability in undiluted seawater
35
Agilent ICP-MS Performance - Benefits
Best matrix tolerance amp less interferences
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS ndash Recommended Maintenance Schedule
ICP-MS Maintenance amp Trouble Shooting
May 2012 37
These functions
(and more) are
completed as part
of a Preventative
Maintenance
program by an
Agilent Field
Service Engineer
Summary ndash Key Consumables for ICP-MS
Sample preparationpresentation
ndash Peristaltic pump tubing
ndash Transfer and drain tubing
ndash ICP-MS standard solutions
ndash Internal Standard solutions
ndash Torches
ndash Spray chambers
ndash Nebulizers
Ion Extraction
ndash Sampler and skimmer cones
Autosampling
ndash Sample tubes racks probes and transfer tubing
ISIS
ndash Peristaltic pump tubing ferrules amp fittings
38
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sample Introduction
Key consumables requiring frequent replacement
bull Pump tubing
bull Torches and quartz transfer tube
bull Nebulizers
bull Spray chambers
bull Interface cones (skimmer amp sampler)
bull Transfer amp connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalogue
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24406(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 39
Autosampler Supplies
Key consumables requiring frequent replacement
ndash Peristaltic pump tubing
ndash Sample racks
ndash Sample tubes
ndash Spare probes
ndash Standard racks
ndash Connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24407(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 40
ISIS Supplies
Key consumables requiring frequent replacement
bull Peristaltic pump tubing
bull Ferrules and fittings
bull Valving
For ISIS Hydride Generation Accessory
bull Membrane filter
bull Concentric nebulizer
bull Gas-liquid separator
bull Other tubing and connectors
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceProductListingaspxcat=SubCat2ECS_24437(Agilent)amppcat=SubCat1ECS_24407(Agilent)amprcat=ClassECS_22674(Agilent)
41
ICP-MS Maintenance amp Trouble Shooting
May 2012
Where to Find the Right Consumable Analytical Consumables Agilent Assist
Consumables amp Supplies Instrument Sales ampServices 1-800-227-9770 (Option 11) 1-800-227-9770 (Option 13) wwwagilentcomchemcontactus wwwagilentcomchemcontactus
On-Line resources
ICP-MS Supplies
2nd Edition Speciation Handbook
ICP-MS Journal Archives
Recorded Agilent e-Seminars
ICP-OES Supplies
Atomic Absorption Supplies
Instrument Parts amp Supplies
Atomic Spec Application Notes
Agilent Quick Reference Guide for 77008800 ICP-MS (pub 5990-8182EN)
Agilent Atomic Spec Supplies Catalogue (pub 5990-8767EN)
Agilent Consumables Catalogue (pub 5990-6674EN)
Instrument User Manuals
42
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS ndash Recommended Maintenance Schedule
ICP-MS Maintenance amp Trouble Shooting
May 2012 37
These functions
(and more) are
completed as part
of a Preventative
Maintenance
program by an
Agilent Field
Service Engineer
Summary ndash Key Consumables for ICP-MS
Sample preparationpresentation
ndash Peristaltic pump tubing
ndash Transfer and drain tubing
ndash ICP-MS standard solutions
ndash Internal Standard solutions
ndash Torches
ndash Spray chambers
ndash Nebulizers
Ion Extraction
ndash Sampler and skimmer cones
Autosampling
ndash Sample tubes racks probes and transfer tubing
ISIS
ndash Peristaltic pump tubing ferrules amp fittings
38
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sample Introduction
Key consumables requiring frequent replacement
bull Pump tubing
bull Torches and quartz transfer tube
bull Nebulizers
bull Spray chambers
bull Interface cones (skimmer amp sampler)
bull Transfer amp connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalogue
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24406(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 39
Autosampler Supplies
Key consumables requiring frequent replacement
ndash Peristaltic pump tubing
ndash Sample racks
ndash Sample tubes
ndash Spare probes
ndash Standard racks
ndash Connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24407(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 40
ISIS Supplies
Key consumables requiring frequent replacement
bull Peristaltic pump tubing
bull Ferrules and fittings
bull Valving
For ISIS Hydride Generation Accessory
bull Membrane filter
bull Concentric nebulizer
bull Gas-liquid separator
bull Other tubing and connectors
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceProductListingaspxcat=SubCat2ECS_24437(Agilent)amppcat=SubCat1ECS_24407(Agilent)amprcat=ClassECS_22674(Agilent)
41
ICP-MS Maintenance amp Trouble Shooting
May 2012
Where to Find the Right Consumable Analytical Consumables Agilent Assist
Consumables amp Supplies Instrument Sales ampServices 1-800-227-9770 (Option 11) 1-800-227-9770 (Option 13) wwwagilentcomchemcontactus wwwagilentcomchemcontactus
On-Line resources
ICP-MS Supplies
2nd Edition Speciation Handbook
ICP-MS Journal Archives
Recorded Agilent e-Seminars
ICP-OES Supplies
Atomic Absorption Supplies
Instrument Parts amp Supplies
Atomic Spec Application Notes
Agilent Quick Reference Guide for 77008800 ICP-MS (pub 5990-8182EN)
Agilent Atomic Spec Supplies Catalogue (pub 5990-8767EN)
Agilent Consumables Catalogue (pub 5990-6674EN)
Instrument User Manuals
42
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
Summary ndash Key Consumables for ICP-MS
Sample preparationpresentation
ndash Peristaltic pump tubing
ndash Transfer and drain tubing
ndash ICP-MS standard solutions
ndash Internal Standard solutions
ndash Torches
ndash Spray chambers
ndash Nebulizers
Ion Extraction
ndash Sampler and skimmer cones
Autosampling
ndash Sample tubes racks probes and transfer tubing
ISIS
ndash Peristaltic pump tubing ferrules amp fittings
38
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sample Introduction
Key consumables requiring frequent replacement
bull Pump tubing
bull Torches and quartz transfer tube
bull Nebulizers
bull Spray chambers
bull Interface cones (skimmer amp sampler)
bull Transfer amp connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalogue
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24406(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 39
Autosampler Supplies
Key consumables requiring frequent replacement
ndash Peristaltic pump tubing
ndash Sample racks
ndash Sample tubes
ndash Spare probes
ndash Standard racks
ndash Connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24407(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 40
ISIS Supplies
Key consumables requiring frequent replacement
bull Peristaltic pump tubing
bull Ferrules and fittings
bull Valving
For ISIS Hydride Generation Accessory
bull Membrane filter
bull Concentric nebulizer
bull Gas-liquid separator
bull Other tubing and connectors
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceProductListingaspxcat=SubCat2ECS_24437(Agilent)amppcat=SubCat1ECS_24407(Agilent)amprcat=ClassECS_22674(Agilent)
41
ICP-MS Maintenance amp Trouble Shooting
May 2012
Where to Find the Right Consumable Analytical Consumables Agilent Assist
Consumables amp Supplies Instrument Sales ampServices 1-800-227-9770 (Option 11) 1-800-227-9770 (Option 13) wwwagilentcomchemcontactus wwwagilentcomchemcontactus
On-Line resources
ICP-MS Supplies
2nd Edition Speciation Handbook
ICP-MS Journal Archives
Recorded Agilent e-Seminars
ICP-OES Supplies
Atomic Absorption Supplies
Instrument Parts amp Supplies
Atomic Spec Application Notes
Agilent Quick Reference Guide for 77008800 ICP-MS (pub 5990-8182EN)
Agilent Atomic Spec Supplies Catalogue (pub 5990-8767EN)
Agilent Consumables Catalogue (pub 5990-6674EN)
Instrument User Manuals
42
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
ICP-MS Sample Introduction
Key consumables requiring frequent replacement
bull Pump tubing
bull Torches and quartz transfer tube
bull Nebulizers
bull Spray chambers
bull Interface cones (skimmer amp sampler)
bull Transfer amp connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalogue
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24406(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 39
Autosampler Supplies
Key consumables requiring frequent replacement
ndash Peristaltic pump tubing
ndash Sample racks
ndash Sample tubes
ndash Spare probes
ndash Standard racks
ndash Connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24407(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 40
ISIS Supplies
Key consumables requiring frequent replacement
bull Peristaltic pump tubing
bull Ferrules and fittings
bull Valving
For ISIS Hydride Generation Accessory
bull Membrane filter
bull Concentric nebulizer
bull Gas-liquid separator
bull Other tubing and connectors
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceProductListingaspxcat=SubCat2ECS_24437(Agilent)amppcat=SubCat1ECS_24407(Agilent)amprcat=ClassECS_22674(Agilent)
41
ICP-MS Maintenance amp Trouble Shooting
May 2012
Where to Find the Right Consumable Analytical Consumables Agilent Assist
Consumables amp Supplies Instrument Sales ampServices 1-800-227-9770 (Option 11) 1-800-227-9770 (Option 13) wwwagilentcomchemcontactus wwwagilentcomchemcontactus
On-Line resources
ICP-MS Supplies
2nd Edition Speciation Handbook
ICP-MS Journal Archives
Recorded Agilent e-Seminars
ICP-OES Supplies
Atomic Absorption Supplies
Instrument Parts amp Supplies
Atomic Spec Application Notes
Agilent Quick Reference Guide for 77008800 ICP-MS (pub 5990-8182EN)
Agilent Atomic Spec Supplies Catalogue (pub 5990-8767EN)
Agilent Consumables Catalogue (pub 5990-6674EN)
Instrument User Manuals
42
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
Autosampler Supplies
Key consumables requiring frequent replacement
ndash Peristaltic pump tubing
ndash Sample racks
ndash Sample tubes
ndash Spare probes
ndash Standard racks
ndash Connecting tubing
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceSubcategoryListingaspxcat=SubCat1ECS_24407(Agilent)amppcat=CatECS_24391(Agilent)amprcat=ClassECS_22674(Agilent)
ICP-MS Maintenance amp Trouble Shooting
May 2012 40
ISIS Supplies
Key consumables requiring frequent replacement
bull Peristaltic pump tubing
bull Ferrules and fittings
bull Valving
For ISIS Hydride Generation Accessory
bull Membrane filter
bull Concentric nebulizer
bull Gas-liquid separator
bull Other tubing and connectors
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceProductListingaspxcat=SubCat2ECS_24437(Agilent)amppcat=SubCat1ECS_24407(Agilent)amprcat=ClassECS_22674(Agilent)
41
ICP-MS Maintenance amp Trouble Shooting
May 2012
Where to Find the Right Consumable Analytical Consumables Agilent Assist
Consumables amp Supplies Instrument Sales ampServices 1-800-227-9770 (Option 11) 1-800-227-9770 (Option 13) wwwagilentcomchemcontactus wwwagilentcomchemcontactus
On-Line resources
ICP-MS Supplies
2nd Edition Speciation Handbook
ICP-MS Journal Archives
Recorded Agilent e-Seminars
ICP-OES Supplies
Atomic Absorption Supplies
Instrument Parts amp Supplies
Atomic Spec Application Notes
Agilent Quick Reference Guide for 77008800 ICP-MS (pub 5990-8182EN)
Agilent Atomic Spec Supplies Catalogue (pub 5990-8767EN)
Agilent Consumables Catalogue (pub 5990-6674EN)
Instrument User Manuals
42
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
ISIS Supplies
Key consumables requiring frequent replacement
bull Peristaltic pump tubing
bull Ferrules and fittings
bull Valving
For ISIS Hydride Generation Accessory
bull Membrane filter
bull Concentric nebulizer
bull Gas-liquid separator
bull Other tubing and connectors
Where to find ordering details
bull Agilent 7700 Quick Reference Guide ndash download from Agilent website
bull Agilent Spectroscopy Supplies Catalog
bull Agilent Consumables and Supplies Catalog (all products)
bull Agilent website ndash dedicated webpage Use this link
httpwwwchemagilentcomen-USStore_layoutsAgilentCommerceProductListingaspxcat=SubCat2ECS_24437(Agilent)amppcat=SubCat1ECS_24407(Agilent)amprcat=ClassECS_22674(Agilent)
41
ICP-MS Maintenance amp Trouble Shooting
May 2012
Where to Find the Right Consumable Analytical Consumables Agilent Assist
Consumables amp Supplies Instrument Sales ampServices 1-800-227-9770 (Option 11) 1-800-227-9770 (Option 13) wwwagilentcomchemcontactus wwwagilentcomchemcontactus
On-Line resources
ICP-MS Supplies
2nd Edition Speciation Handbook
ICP-MS Journal Archives
Recorded Agilent e-Seminars
ICP-OES Supplies
Atomic Absorption Supplies
Instrument Parts amp Supplies
Atomic Spec Application Notes
Agilent Quick Reference Guide for 77008800 ICP-MS (pub 5990-8182EN)
Agilent Atomic Spec Supplies Catalogue (pub 5990-8767EN)
Agilent Consumables Catalogue (pub 5990-6674EN)
Instrument User Manuals
42
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
Where to Find the Right Consumable Analytical Consumables Agilent Assist
Consumables amp Supplies Instrument Sales ampServices 1-800-227-9770 (Option 11) 1-800-227-9770 (Option 13) wwwagilentcomchemcontactus wwwagilentcomchemcontactus
On-Line resources
ICP-MS Supplies
2nd Edition Speciation Handbook
ICP-MS Journal Archives
Recorded Agilent e-Seminars
ICP-OES Supplies
Atomic Absorption Supplies
Instrument Parts amp Supplies
Atomic Spec Application Notes
Agilent Quick Reference Guide for 77008800 ICP-MS (pub 5990-8182EN)
Agilent Atomic Spec Supplies Catalogue (pub 5990-8767EN)
Agilent Consumables Catalogue (pub 5990-6674EN)
Instrument User Manuals
42
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
Other Support Resources for Agilent ICP-MS Users
bull Are you a subscriber to the Agilent ICP-MS
journal
ndash An ICP-MS specific journal produced 4 timesyear
ndash Includes applications techniques ldquorealrdquo user
stories news updates and other product
information
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpwwwchemagilentcomen-
USNewslettersicpmsjournalPagesdefaultaspx
bull Are you a subscriber to the Access Agilent
newsletter
ndash A monthly e-newsletter newsletter tailored to your
preferences
ndash Includes in-depth articles new products literature
offers and events
bull To register use this link to the registration form on the
Agilent website (or ask your Agilent representative)
httpswwwchemagilentcomen-
US_layoutsAgilentSecurityProfileaspx
43
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
bull Most ldquoinstrumentrdquo failures occur in the sample introduction area
ndash Includes
bull Torch
bull Spray chamber
bull Nebulizer
bull Interface cones
bull All tubing and drain assembly
bull Improper maintenance of this area can result in poor data quality
bull Frequently less experienced analysts can fail to recognize problems resulting in
productivity losses
bull Establishing routine maintenance procedures can prevent problems before they
occur
Summary ndash To Achieve Quality Data
44
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012
Questions
The Market Leaders in Atomic Spectroscopy
Agilent MP-AES
Agilent ICP-MS Agilent ICP-OES Agilent AAS
45
ICP-MS Maintenance amp Trouble Shooting
May 2012