products designed to solve nagging gc problems · 2016. 9. 4. · column: agilent j&w hp-5ms ui...
TRANSCRIPT
![Page 1: Products Designed to Solve Nagging GC Problems · 2016. 9. 4. · Column: Agilent J&W HP-5ms UI 30 m x 0.25 mm x 0.25 um Oven: 100 C 4 min hold, 10 /min to 280 C, 6 /min to 300 C](https://reader035.vdocuments.us/reader035/viewer/2022063011/5fc5790ada820272594f13e9/html5/thumbnails/1.jpg)
Page 1
Products Designed to Solve
Nagging GC Problems
Daron Decker
Chromatography Technical Specialist
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Contaminated Gas Fouls the Whole GC
Dirty Lines, Inlet, Column, Detector
More Frequent Maintenance
More Down Time
Replacements Cost Money
Solution = Use only Clean Gas!
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Gas Clean Filters – The Insurance Policy
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Gas-Clean Filters Design
Sensitive indicators for moisture
and oxygen
Short filter equilibration time
Fast, leak-free filter replacement
• without turning off the gas
• NO tools needed
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Oxygen Damages GC columns
Repair of the GC column is impossible
Replacements means re-calibration
Replacement means delay
Replacement column costs money
Solution = No Leaks!
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Leak Test
- MS – Air/Water
- Leak Detector (G3188B)
Page 6
• Portable, handheld unit – only 105g
• USB cable for recharging
• Audible and visual alerts for 12 gases
• Minimum detection limit of 0.0005 mL/minute for hydrogen and helium
• Rechargeable lithium ion battery with over 5 hours of life
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Ferrule Pre-swaging & MS Interface Installation Tools
• Ensures proper length of column into the fittings, every time
• For graphite or metal ferrules
Metal ferrule tool Graphite ferrule tool
G3440-80218 G3440-80217
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What if you …
Could install the column easily
Finger tighten, without tools that cause over tightening
And make leak free connections
Which don’t need to be retightened
Every time?
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Self-Tightening Column Nuts
Page 9
Video at agilent.com/chem/STnutvideo
• Less wasted time: No retightening
needed after repeated thermal cycles
• Ease of use: Finger-tight,
consistent connections without tools
• Leak Free = Lower column bleed:
Longer column life
Innovative spring-driven piston continuously presses against ferrule
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Self Tightening Column Nuts
Page 10
For mass spec transfer line
p/n 5190-5233
For inlet or detector
p/n 5190-6194
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Self-Tightening Column Nuts
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Peak Tailing – What causes this?
1. ACTIVITY either in inlet or column
-Reversible adsorption of active compounds
(-OH, -NH, -SH)
2. FLOW PATH PROBLEM - dead volume, obstruction, poor installation, or severe column contamination
Miscellaneous – temperature issues for late eluters, overloading of PLOT columns, co-elution, polarity mismatch between phase, solute or solvent, and some compounds always tail
*Tip = Inject a light hydrocarbon, should not tail unless flow path problem.
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Symptom – Tailing of Active Compounds 1. n-Nitrosodimethylamine 2. Aniline 3. 1,4-Dichlorobenzene-d4 4. Benzoic Acid 5. Naphthalene-d8 6. Acenaphthene-d10 7. 2,4-Dinitrophenol 8. 4-Nitrophenol 9. 2-Me-4,6-dinitrophenol 10. 4-Aminobiphenyl 11. Pentachlorophenol 12. Phenanthrene-d10 13. Benzidine 14. Chrysene-d12 15. 3,3’-Dichlorobenzidine 16. Benzo[b]fluoranthene 17. Benzo[k]fluoranthene 18. Perylene-d12
Sample: 0.5 ng on column loading with ISTD
Column: 20m 0.18mm 0.18µm
Carrier: Helium 37cm/sec, Ramped flow; 0.7ml/min (0.1min) to 1.3ml/min (15ml/min2)
Oven: 35oC (2.5 min) to 80oC (40oC/min), 15oC/min to 200oC, 8oC/min to 275oC (2 min)
Injection: 0.5µl, Splitless, 280oC, purge flow 30ml/min at 0.75 min
MSD: Transfer Line 290oC, Source 300oC, Quad 180oC
2.00 4.00 6.00 8.00 10.00 12.00 14.00 16.00 18.00 20.00 22.00
0
50000
100000
Time (min)
Abundance
1
2
3 5 6
7
8
10
11
9
12
13
14
15
16
17
18
4
2.00 4.00 6.00 8.00 10.00 12.00 14.00 16.00 18.00 20.00 22.00
0
50000
100000
Time (min)
Abundance
1
2
3 5 6
7
8
10
11
9
12
13
14
15
16
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18
4
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Solution – Ultra Inert GC Column 1. n-Nitrosodimethylamine 2. Aniline 3. 1,4-Dichlorobenzene-d4 4. Benzoic Acid 5. Naphthalene-d8 6. Acenaphthene-d10 7. 2,4-Dinitrophenol 8. 4-Nitrophenol 9. 2-Me-4,6-dinitrophenol 10. 4-Aminobiphenyl 11. Pentachlorophenol 12. Phenanthrene-d10 13. Benzidine 14. Chrysene-d12 15. 3,3’-Dichlorobenzidine 16. Benzo[b]fluoranthene 17. Benzo[k]fluoranthene 18. Perylene-d12
Sample: 0.5 ng on column loading with ISTD
Column: 20m 0.18mm 0.18µm
Carrier: Helium 37cm/sec, Ramped flow; 0.7ml/min (0.1min) to 1.3ml/min (15ml/min2)
Oven: 35oC (2.5 min) to 80oC (40oC/min), 15oC/min to 200oC, 8oC/min to 275oC (2 min)
Injection: 0.5µl, Splitless, 280oC, purge flow 30ml/min at 0.75 min
MSD: Transfer Line 290oC, Source 300oC, Quad 180oC
2.00 4.00 6.00 8.00 10.00 12.00 14.00 16.00 18.00 20.00 22.00
0
50000
100000
Time (min)
Abundance
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
2.00 4.00 6.00 8.00 10.00 12.00 14.00 16.00 18.00 20.00 22.00
0
50000
100000
Time (min)
Abundance
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
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17
18
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AND Ultra Inert Liners
Touchless packaging
Easy installation of new, clean liner
without risk of contamination from touching
Includes non-stick plasma treated O-ring
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Agilent UI Gold Seal: Deactivated Gold Surface
• Soft gold plating is essential for proper sealing
• Ultra Inert chemistry blocks active sites
(gold is NOT inert)
• Smooth surface doesn't leak
Agilent MIM seal Competitor’s
machined seal
Reliable ppb and ppt
measurements require
attention to the little things!
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Use the Highest Quality Consumables in
“Touchless” Packaging
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You May Even Need the Agilent Inert Inlet
UltiMetal Plus treatment creates inert surface 7890 inlet weldment & shell
• Limits adsorption/degradation of active analytes
• Optimum for Trace GC/MS and GC-ECD
pesticide analyses
Agilent’s proven
proprietary Ultimetal
Plus surface
treatment
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Putting It All Together –
Inert Flow Path vs. Standard Flow Path
20.20 20.40 20.60 20.80 21.00 21.20 21.40 21.60
10000
20000
26000
Green = Inert Flow Path
Blue = Standard Flow Path
Column: Agilent J&W HP-5ms UI 30 m x 0.25 mm x 0.25 um
Oven: 100C 4 min hold, 10/min to 280C, 6 /min to 300C (4.67 min hold),
Carrier : Helium 52.7 cm/s (2 mL/min) set at 100C, EPC-Constant Flow
Inlet: Pulsed Splitless 35 PSI pulse until 0.73 min, 0.75 min purge 50 ml/min, gas saver 20, ml/min at 2 min
Inlet liner: Ultra Inert with wool / Standard single taper liner with wool (p/n 5190-3165)
Gold Seal: UI Gold Seal / Standard gold seal
Detector: MSD Scan mode 40 t0 450 m/z, 230 C source temp, 150 C Quad temp, 310 C transfer line
1
2
3
4
5
1. Dronabinol
2. Oxycodone
3. Temazepam
4. Flunitrazepam
5. Diacetyl morphine
Drugs of Abuse 250 ppb using HP-5ms UI
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Broad Peaks – Why?
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INJECTOR -Poor Installation -Change in injection solvent -Change in settings (temps/flows) -Poor sample focusing -Large change in sample concentration -Breakdown or adsorption FLOW -Change in gas velocity -Constant Flow vs Constant Pressure COLUMN -Contamination -Damaged/old stationary phase -Breakdown or adsorption -Reverse Solvent Effect
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Splitless Injection Reverse Solvent Effect
DB-1, 15 m x 0.25 mm I.D., 0.25 µm
50°C for 1 min, 50-210°C at 20°/min; Helium at 30 cm/sec
1. 1,3-DCP 2. 3-hexanol 3. butyl acetate 4. 1-heptanol 5. 3-octanone 6. 1,2-dichlorobenzene
0 1 2 3 4 5 6
Time (min.)
1 2 3 4 5 6
Time (min.)
Hexane Methanol
1
2 3
4
5 6
1
2
3
4
5 6
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Retention Gap Also Called A Guard Column
Usually 2-10 meters long and same diameter as the column
(or larger if needed)
Injector Detector
Deactivated Fused Silica Tubing
Union Column
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Fixing the Reverse Solvent Effect 3 m x 0.25 mm I.D. Retention Gap
DB-1, 15 m x 0.25 mm I.D., 0.25 µm
50°C for 1 min, 50-210°C at 20°/min; Helium at 30 cm/sec
1. 1,3-DCP 2. 3-hexanol 3. butyl acetate 4. 1-heptanol 5. 3-octanone 6. 1,2-dichlorobenzene
0 1 2 3 4 5 6
Time (min.)
Hexane
1 2 3 4 5 6
Time (min.)
Methanol 1
2 3
4
5 6
1
2
3
4
5 6
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Agilent Ultra Inert Press Fit
Press Fit Connectors
Inertness, seal and transparency are key parameters
Competitor Press-Tight
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Maximum Force Required to “pull apart”
0.0
0.5
1.0
1.5
2.0
2.5
1 2 3 4
Po
un
ds (
forc
e)
Pull Value, 0.25 mm I.D. Columns
Ultra Inert Quartz Fused Silica Glass
Press Fit Connector Type
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Strong bond between FS polyimide
&
press fit UI deactivation layer
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Ultimate Union and Retention Gap
(Preferred by Many)
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Two Connection Options from Agilent
Ultra Inert Press Fit Connectors Capillary Flow Technology
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Peak Response All Change in Size
DETECTOR (response problem)
-Settings or flows changed
-Electronics failing
-Contamination
-Split ratio set incorrectly
-Wrong purge activation time
-Septum purge flow too high
-Injector temperature too low*
INJECTOR
-Leaky syringe
*Tip = Ask is it all of them or some of them, if all then injector or detector
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Traditional PDMS column- Coating of Reactor Tubes
Overlay of before (green) and after 2 x 2 uL neat toluene Injection (red)
1. Hydrogen Sulfide
2. Carbonyl Sulfide
3. Methyl Mercaptan
4. Ethyl Mercaptan
1 2 3
FID: No response changes
4 3
4
SCD:
10% drop in
sensitivity
Data courtesy of Jim Luong, Ronda Gras, Myron Hawryluk of Dow Chemical Canada
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Configuration to test SCD Quenching Issue
Inlet
Pulsed SCD
FID
4:5
Thick film PDMS type Column
325 torr
710 torr
CFT splitter
1:5
Data courtesy of Jim Luong, Ronda Gras, Myron Hawryluk of Dow Chemical Canada
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Solution = New DB-Sulfur SCD column
Last Three Runs of the day (n=20, 100 ppmv std)
250C Cool down
1. H2S
2. COS
3. CH3SH
4. C2H5SH
1
2 3
4
FID
SCD
40C 3
4
Data courtesy of Jim Luong, Ronda Gras, Myron Hawryluk of Dow Chemical Canada
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Long Term SCD Performance with DB-Sulfur SCD
500000
550000
600000
650000
700000
750000
800000
850000
900000
950000
1000000
1 2 3 4 5
H2S
COS
Methyl Mercaptan
No observable
SCD sensitivity
change in
subsequent runs
Months!
Are
a C
ou
nts
Data courtesy of Jim Luong, Ronda Gras, Myron Hawryluk of Dow Chemical Canada
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Used to do SCD maintenance every 3 weeks!
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Spiking Baseline
DETECTOR
-Particles entering the detector
-Random: poor connection
-Regular: nearby "cycling" equipment (electronics)
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Integrated Particle Trap PLOT Column
2.5 meter integrated particle traps on both ends
Compatible with GC/MS and valve switching systems,
and Capillary Flow Technology
Very similar selectivity, plates and peak shape to
existing Agilent PLOT columns
PLOT
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The PLOT Column and Integrated Particle Trap
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No spikes at Fixed Gases Analysis
on CP-Molsieve 5Å PLOT PT column
CP-Molsieve 5Å, 25m×0.53mm,50um
(30m total length)
Carrier : H2, 3mL/min
Oven: : 80°C isothermal
Injection: 70°C, split ratio 5:1
Detector: TCD, 250 ℃
Sample: 100uL
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Halocarbons by GCMS Column: PoraPLOT Q PT, 25m×0.32mm,10um (P/N CP7551PT)
(30m total length)
Carrier : Helium, 42cm/s @55 ℃
Oven: : 55 °C for 5min
55 °C - 200 °C at 12°C/min
200 °C for 10min
Injection: 250 ℃, splitless, 0.2min purge activation time
Detector: MSD, 280 ℃ Transfer line, full Scan at m/z 45-185
Sample: 1uL
1. Fluoroform (Freon-23)
2. 1,1,1-trifluoroethane (Freon-143a)
3. Pentafluoroethane (Freon-125)
4. Bromotrifluoromethane (Freon-13b1)
5. 1,1,1,2-Tetrafluoroethane (Freon-134a)
6. 1,1-difluoroethane (Freon-152a)
7. Difluorochloromethane (Freon-22)
8. 1,1,2,2-tetrafluoroethane (Freon-134)
9. 1-chloro-1,1-difluoroethane (Freon-142)
10. Bromochlorodifluoromethane (Freon-12b1)
11. Ethyl Chloride (Freon-160)
12. Fluorodichloromethane (Freon-21)
13. Trichloromonofluoromethane (Freon-11)
14. 1,1-Dichloro-1-fluoroethane (Freon-141)
15. 2,2-dichloro-1,1,1-trifluoroethane (Freon-123)
16. 1,1,2-trichloro-1,2,2-trifluoroethane (Freon-113)
17. 1,2-dibromo-1,1,2,2-tetrafluoroethane (Freon-114b2)
18. Trichloromethane (Freon-20)
19. 1,2-dichloroethane
20. 1,1,1-trichloro-ethane
21. Trichloroethylene
22. 1,1,2-trichloroethane
2.00 4.00 6.00 8.00 10.00 12.00 14.00 16.00 18.00
1 2
3
4
5
6
7
8
9 10
11
12
13
14
15
16
17
18 19
20
21
22
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Agilent J&W
PLOT PT Columns Available PLOT PT columns:
•Porous polymers: – PoraPLOT Q
– PoraBOND Q
– PoraBOND Q HT
– HP-PLOT Q
– GS-Q
– PoraPLOT U
– HP-PLOT U
•NEW! Aluminum oxide – HP-PLOT Al2O3 S
– HP-PLOT Al2O3 M
– HP-PLOT Al2O3 KCl
– GS-Alumina
– GS-Alumina/KCl
– CP-Al2O3 KCl
– CP-Al2O3 Na2SO4
•NEW! Molsieve – CP-Molsieve 5A
Custom PLOT PT columns are
available for these phases
Phase type Part number Description DimensionsCP7348PT PoraBOND Q PT 25m x 0.25mm x 3µm
CP7351PT PoraBOND Q PT 25m x 0.32mm x 5µm
CP7352PT PoraBOND Q PT 50m x 0.32mm x 5µm
CP7353PT PoraBOND Q PT 10m x 0.53mm x 10µm
CP7354PT PoraBOND Q PT 25m x 0.53mm x 10µm
CP7550PT PoraPLOT Q PT 10m x 0.32mm x 10µm
CP7551PT PoraPLOT Q PT 25m x 0.32mm x 10µm
CP7554PT PoraPLOT Q PT 25m x 0.53mm x 20µm
CP7557PT PoraPLOT Q-HT PT 25m x 0.32mm x 10µm
115-3432PT GS-Q PT 30m x 0.53mm
19091P-QO3PT HP-PLOT Q PT 15m x 0.32mm x 20µm
19091P-QO4PT HP-PLOT Q PT 30m x 0.32mm x 20µm
19095P-QO3PT HP-PLOT Q PT 15m x 0.53mm x 40µm
19095P-QO4PT HP-PLOT Q PT 30m x 0.53mm x 40µm
CP7584PT PoraPLOT U PT 25m x 0.53mm x 20µm
19095P-UO4PT HP-PLOT U PT 30m x 0.53mm x 20µm
CP7515PT CP-Al2O3/KCl PT 50m x 0.32mm x 5µm
CP7517PT CP-Al2O3/KCl PT 25m x 0.53mm x 10µm
CP7518PT CP-Al2O3/KCl PT 50m x 0.53mm x 10µm
19091P-K15PT HP-PLOT Al2O3 KCl PT 50m x 0.32mm x 8µm
19095P-K23PT HP-PLOT Al2O3 KCl PT 30m x 0.53mm x 15µm
19095P-K25PT HP-PLOT Al2O3 KCl PT 50m x 0.53mm x 15µm
115-3352PT GS-Alumina/KCl PT 50m x 0.53mm
CP7565PT CP-Al2O3/Na2SO4 PT 50m x 0.32mm x 5µm
CP7568PT CP-Al2O3/Na2SO4 PT 50m x 0.53mm x 10µm
19091P-S12PT HP-PLOT Al2O3 S PT 25m x 0.32mm x 8µm
19091P-S15PT HP-PLOT Al2O3 S PT 50m x 0.32mm x 8µm
19095P-S23PT HP-PLOT Al2O3 S PT 30m x 0.53mm x 15µm
19095P-S25PT HP-PLOT Al2O3 S PT 50m x 0.53mm x 15µm
115-3532PT GS-Alumina PT 30m x 0.53mm
115-3552PT GS-Alumina PT 50m x 0.53mm
19095P-M25PT HP-PLOT Al2O3 M PT 50m x 0.53mm x 15µm
CP7534PT CP-Molsieve 5A PT 30m x 0.32mm x 10µm
CP7536PT CP-Molsieve 5A PT 25m x 0.32mm x 30µm
CP7538PT CP-Molsieve 5A PT 25m x 0.53mm x 50µm
CP7539PT CP-Molsieve 5A PT 50m x 0.53mm x 50µm
Molsieve
Al2O3 Na2SO4
deactivated
Al2O3 with
proprietary
deactivation
PLOT Q
PLOT U
Al2O3 KCl
deactivated
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The BIGGEST Problem in GC is…
There are more things that DON’T go through a GC than DO!
….therefore, don’t inject anything and you’ll never have
problems.
OK, inject, but realize that everything just got dirty…deal with it!
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Where Does it Get Dirty?
Here
Here
Here
Here
Here
Here
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What Are You Doing!?
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It’s in the Inlet!
Do Inlet Maintenance
- Trim the Column
- Replace the Liner
- Replace the Gold Seal
- Replace the Syringe
- Replace the Split Vent Trap, Split Vent Line
- Rinse the Inlet
Start as clean and inert as possible
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Page 44
Conclusions for a Problem Free GC
Start With Ultra Inert/High Quality Consumables
Never Have a Leak (no oxygen)
Use Gas Clean Filters
Never Inject Anything (dirty or reactive)
Don’t Touch Anything
Do Routine Inlet Maintenance Often
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Troubleshooting Resources
Online Troubleshooting and Maintenance Videos
http://www.chem.agilent.com/en-US/Technical-Support/Instruments-Systems/Gas-
Chromatography/Pages/troubleshootingvideos.aspx
GC Troubleshooting Guide
http://www.chem.agilent.com/en-US/Products-Services/Instruments-Systems/Gas-
Chromatography/pages/gp6770.aspx
Method Translation Software
http://www.chem.agilent.com/en-US/Technical-Support/Instruments-Systems/Gas-
Chromatography/utilities/Pages/gcmethodtranslation.aspx
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Agilent Better GC Connections
www.agilent.com/chem/betterGCconnections
Order the poster… View the video…