fully automated trace level gas generation and its
TRANSCRIPT
Fully automated Trace Level gas generation and its
application for calibration, linearization, LOD validation in
hydrocarbon analysis.
17th October 2018Galveston, TexasLaurent COURTHAUDON
New!
About AlyTech
❖Founded in1999
❖Headquartered in Paris area
❖Team of analytical chemists, electronics and software
engineers
❖Expertise in laboratory and on-line instrumentation
❖Since 2007 develops, manufacture and sell customized gas
preparation systems under GasMix™ brand
Introducing the AlyTech
❖ Perfectly controlled mixing or dilution up to 10000 times of 2 to 16 Gases, and/or
1 liquid
❖ In compliance with ISO 6145-7 prepare Single and Multipoint Calibration Gas
Standards by dynamic dilution with high precision, accurate and with full
traceability.
❖ By user defined program makes binary or multi-component gas mixtures at
different concentrations from % levels down to traces level
❖ Deliver or Inject the gases to an analyzer, reactor or a canister
❖ Intuitive Software allows high versatility to fit any application
❖ All packaged in a compact instrument, bench-top, rack mounted or portable
Automated mixing or diluting gases and vaporized liquids in order to create a customized gas mixture
specific to the user's need and/or application, for example calibration standards or synthetic atmospheres.
Purpose of GasMix™?
A family of automated
Gas and Gas/Liquid Diluting-Mixing-Injection systems
Bench-top, portable or rack mounted
❖ Petrochemical
❖ Environmental
❖ Flavor & Fragrance
❖ Research
❖ Specialty Gases
Who Uses GasMix?
They trust AlyTech
“To provide our customers with the best
possible user experience, to continually
bring new and innovative products that
increase productivity, ensuring a rapid
return on investment”.
Benefits of the AlyTech GasMixTM?
Saves
money
Unique &
unstable
gases
Automatic!
Get more
out of your
gas
cylinders
❖ COST SAVINGReplace constraints of purchasing and storage multiple cylinders with different concentrations of the
component by on-site preparation of standards. GasMix needs 1 standard gas cylinder and 1 diluent to get a
whole range of concentrations.
❖ OPTIMIZING THE EFFICIENCY OF YOU GAS CYLINDERS STOCKCertified low level standards in cylinders are expensive, hard to obtain, have short shelf life, long delivery time,
and often concentration value certified with high uncertainty
With the GasMix from easily available high concentration standard, stable and accurate you produce on-site
low level concentrations at your choice with very little added uncertainty.
❖ MORE SAFETY AND LESS STORAGELess cylinders you need more safer your storage, easier logistics and less space you need for cylinders and
gas lines manifolds. In addition GasMix software will help you manage your cylinder expiration dates.
Benefits of GasMixTM?
Case studies prove, GasMix is paid back in about 1 year.
❖ UNSTABLE OR RARE STANDARDS
Some mixtures are unstable at storage, some are even not commercially available
LiqMix is the solution for such mixtures as BTX (Benzene, Toluene, Xylene), other organic solvents,
Siloxanes or create gases with defined level of humidity.
❖ AUTOMATION
Designed to run with minimum operator intervention GasMix™ is controlled via dedicated software. After a
setup of defined mixing/diluting sequences, the system allows unattended automatic operations. It can
interface and synchronize with the analyzer.
❖ EVOLUTIVE
Flexibility of GasMix platform allows future evolution of the system by adding additional gas channels or
specific calibration to adapt to future customer needs
Benefits of GasMixTM
Benefits of GasMixTM
❖ TRACEABILITY and DOCUMENTATION
The GasMix software calculates the final
concentration uncertainty of each mixture
generated.
An Audit Trail function included in the software
guarantees the operation traceability, recording
the actual flows sent to the analyzers.
A detailed certificate can be generated at the end
of the mixing/diluting process
Principle of operation
GasMixGas 1
Gas n
MFC 1
MFC n
Mixing chamber OutletGas 2 MFC 2
Up to 16 gases!
Virtually unlimited
number of
combinations
16
-
-
8
7
6
5
4
3
2
1
PerMix Line
Permeation/Gas
max
20
CA
SCA
DE
Liqu
id
Liqu
id
LiqMix Line
Liquid/Gas
GasMix line
Gas/Gas
LiqM
ix
ATM
O
AIO
LOSZEP
HY
R
HU
RR
ICA
NE
GM
RA
CK
LiqM
ixC
ascade
Pe
rMix A
TM
O
Mass Flow Controller Calibration (MFC)
Metrology of excellence
15
❖ GasMix fulfills highest standards in metrology
❖ The instrument design and manufacturing processes are optimized to ensure accuracy,
linearity, minimal uncertainty and long term stability
❖ Every MFC installed in GasMix undergoes a rigorous factory calibration
❖ MFC calibration is made by a primary standard traceable to NIST
❖ Each MFC is physically calibrated on gas matrix/matrices (He, Ar, N2, Air, CH4, CO2,
gas mixtures, …) on which it will be used !
Primary standard piston prover
Calibration process: A unique feature!
User friendly and dedicated software
❖ The a, b, Dmin, Dmax, n and p parameters are stored in the library of standards.
❖ Mixture generation automation.
❖ Possibility to create projects adapted to every need and every budget (repeatability, linearity…)
❖ An Audit Trail function included in the software guarantees the operation traceability, recording the actual flows sent to the analyzers.
LiqMix Cascade
17
TLiq 1
Gas 2
Gaz 3
Gas 4
MFC
MFC2
MFC3
MFC4
.
.
Vaporizer
T Mixingchamber
Output
T
Diluting gas
MFC2
MFC1
Vent
P
CASCADE
LiqMix Cascade
18
Thermodesorption has been used for some time. But
this method is becoming more and more popular
because of the needs for lowers and lower levels. Even
traces. Analyzers calibration is a concern
&
Thermodesorption
LiqMix CascadeThermal desortion
19
✓ Certified gases, if available, are expensive and have a limited lifetime
✓ Gas pressure entering an anlytical equipment has to be lowered; pressure regulators
may adsorb some analytes – more significant when working at trace levels
✓ Exact amount of calibration gas going through the analyzer must be known: need for a
flow meter
✓ Only one concentration for each analyte is available from a gas cylinder
✓ A very limited number of certified desorption tubes are available on the market (see
example on following slide)
✓ Any compound outside of those listed in the official methods may be difficult to obtain
as gas, or certified tube
✓ Some suppliers offer calibration tubes prepared according to ISO 6145-4 or -8 method
LiqMix CascadeThermal desortion
20
Commercial certified standard
LiqMix CascadeThermal desortion
Application: Hydrocarbon contaminants in hydrogen fuel
LiqMix Cascade solution
21
➢ Calibration gas generation using ISO 6145-4 method
➢ Multilevel (concentration) calibration starting from pure compounds
➢ Automatic process: concentration AND flow: The exact amount of each compound
which goeas through the tube is known, with corresponding uncertainties
LiqMix Cascade
Challenge!
22
➢ Calibrate an analytical system with 5 hydrocarbon compounds (C2 to C6) plus
Methanol, acetone and ethanol at the same time. See Table 1
➢ The eight compounds gas solutions are prepared from 20ppb to 2ppm, at seven
different levels
➢ UNIQUE: for each analyte and each concentration, the software calculates and
displays the maximum uncertainties, expressed in concentration. See Table 2
LiqMix CascadeExperimental set-up
Real Data!
23
Synoptic
IFE laboratory
LiqMix Cascade
Real Data!
24
Table 1
Table 2Compound
Analytical Method
Span / ppb
Gas
C2 GC-Precon-PHID
20035006800
10100134001670020000
C3 GC-Precon-PHID
C4’s GC-Precon-PHID
Liq
uid
C5’s GC-Precon-PHID
C6 GC-Precon-PHID
MeOH GC-Precon-PHID
Acetone GC-Precon-PHID
EtOH GC-Precon-PHID
LiqMix CascadeThermal desortion
25
Linearity check Performance determination: LOD & LOQ
LOD LOQ Tables
AnalyteConcentration,
ppb-molUncertainty,
ppbRSD % Liqmix
1-Pentene 0,981 0,057 5,810
1-Butene 1,019 0,057 5,594
Ethylene 3,000 0,127 4,233
Isopentane 3,846 0,164 4,264
Neopentane 3,904 0,166 4,252
Pentane 3,913 0,166 4,242
Propene 4,798 0,205 4,273
Isobutane 9,808 0,415 4,231
n-Butane 9,808 0,300 3,059
Propane 12,500 0,456 3,648
Ethane 19,615 0,721 3,676
Ethanol 13,396 0,445 3,322
Methanol 15,094 0,491 3,253
Acetone 20,010 0,630 3,150
AnalyteLOD,
ppb-molLOQ,
ppb-mol
1-Pentene 0,230 0,767
1-Butene 0,169 0,562
Ethylene 0,584 1,946
Isopentane 0,783 2,611
Neopentane 0,626 2,087
Pentane 0,600 1,999
Propene 1,054 3,512
iIsobutane 1,512 5,039
Butane 1,615 5,382
Propane 2,189 7,297
Ethanol 4,143 13,809
Methanol 4,650 15,499
Ethane 3,424 11,413
Acetone 5,915 19,716
THANK YOU!
AlyTech SARL
Centre Hoche
3 rue Condorcet
91260 Juvisy-sur-Orge
France
Tel;: +331 69 56 07 17
Fax: +331 69 44 49 81
E-mail: [email protected]
Booth 118