Development of Portable GC/MS System with Benchtop Performance for Critical DoD Applications. Mitch Wells, Ph.D. Philip Tackett, Ph.D.
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1 Development of Portable GC/MS System with Benchtop Performance for Critical DoD Applications Mitch Wells, Ph.D. Philip Tackett, Ph.D. HEMS Workshop 2017
2 FLIR Systems, Inc. Industrial Commercial Government & Defense 2
3 FLIR Detection 3
4 Chemical Analysis in the Field Chemistry happens outside the lab so should the analysis 4
5 Next Generation for Downrange Analysis Need real-time, actionable data from sites deemed as potential hot zones In 2014, US Department of Defense released set of product requirements of a next generation chemical detector (NGCD) Requirements specify that system should be able to detect a range of threats in all chemical phases Developmental effort to create GC/MS system to meet analysis requirements and also meet size, weight, and power requirements Fieldable GC/MS System Sample Collection Tools 5
6 Specification Driven Decisions GC/MS is gold standard for chemical analysis and can provide high fidelity data for data-driven decisions Size, weight, and power appropriate for a portable system Weight analysis single person portable Power budgeting and management mission compatible run-times Actionable data Easily interpreted and comparable NIST matchable data from quadrupole mass analyzer Capability to detect and identify analytes from all chemical phases 6
7 Size, Weight, and Power System capable of being carried to the sample by one person Operator-focused industrial design with IP65 rating Lightweight materials and compact subsystems 45 kg <15 kg without batteries Addition of 2.8 kg batteries for up to 4 hours of operation Electronics redesign Miniaturization and power reduction ~1900 cm 2 and ~3 kg ~400 cm 2 and ~0.5 kg 7
8 Pumping System 1. System that can be pumped down from atmosphere on battery operation without need for external pumping (i.e. no pumping station) 2. For GC/MS system, ideal to have direct interface of exit of GC column with ionization source: necessitates active pumping Compact & rugged turbomolecular pump Light-weight diaphragm roughing pump Minimized manifold volume for rapid evacuation 8
9 Quadrupole Mass Analyzer High fidelity mass spectral data that can be easily matched/compared to library of known compounds NIST mass spectral library: >240,000 compounds analyzed by EI MS with a quadrupole mass analyzer Ion trap analyzer vs. quadrupole mass analyzer Ion trap: easy to miniaturize but spectra can be concentration dependent Quadrupole: spectra more reproducible but can be difficult to make portable 50 ng Triethylphosphorothioate Quadrupole Mass Analyzer 95% probability NIST match 100 NIST Reference Spectrum O S P O O Ion Trap Analyzer 0% probability NIST match (mainlib) O,O,O-Triethyl thiophosphate 9
10 Liquid and Solid Sampling 10
11 Liquid and Solid Sampling Requirement to have capability to sample both liquids and solids Standard S/SL injector compatible with syringe liquid injections, solid-phase micro extraction (SPME) and head-space syringe samples Injector adapter which enables solid samples to be placed inside injector volume for thermal desorption Use of standard S/SL injector enables user to analyze wide range of samples in a similar manner to lab GC/MS systems Use of He carrier gas to maximize performance of GC Low thermal mass GC column (15 m) capable of ramping up to 100 C/min C9 C10 C12 C14 C16 C18 C20 C22 C24 C26 C28 Sarin VX Heroin 11
12 Liquid and Solid Sampling Liquid Injection EPA 8270P mixture (mix of organophosphorous pesticides) Sulfotep, RI 1681 BP ~310 C NIST Match >850 Famphur, RI 2315 BP ~390 C NIST Match >850 Phorate, RI 1686 BP ~290 C NIST Match >900 12
13 Liquid and Solid Sampling Liquid Injection Drugs of abuse (mix of meth and cocaine) Methamphetamine NIST Match >800 Cocaine NIST Match >800 13
14 Liquid and Solid Sampling Liquid Injection Drugs of abuse (mix of heroin and fentanyl) Heroin, RI 2643 BP ~490 C NIST Match >850 Fentanyl, RI 2732 BP ~460 C NIST Match >900 14
15 Liquid and Solid Sampling 2-Nitrotoluene NIST Match >900 Liquid Injection Explosives mixture 3-Nitrotoluene NIST Match >850 Trinitrotoluene NIST Match >850 4-Nitrotoluene NIST Match >900 3,5-Dinitro-p-Toluidine NIST Match >850 2,6-Dinitrotoluene NIST Match >900 15
16 Vapor Sampling 16
17 Vapor Sampling Requirement to both provide high-fidelity vapor identification and realtime sampling with alarming capability Sorbent preconcentration with GC-MS analysis for high-fidelity vapor identification Membrane-inlet MS (MIMS) for real-time vapor analysis Heated sample line with sampling head 17
18 Vapor Sampling Sorbent preconcentration Collect vapor sample of known volume onto sorbent bed Carrier gas is passed through sorbent bed and heat is applied to desorb analyte collected Desorbed analytes are transported to GC column for analysis GC Vapor Sample Sorbent Bed Desorption Gas 18
19 Vapor Sampling Sorbent preconcentration Headspace sample of n-octadecane (99% purity) showing octadecane and various semi-volatile impurities in sample n-octadecane ~400 ppb BP 316 C 19
20 Vapor Sampling Sorbent preconcentration Sample of methyl salicylate vapor (CWA simulant) at ppb levels Methyl Salicylate NIST Match >850 BP 222 C 20
21 Atmosphere Membrane High Vacuum Ionization Volume Vapor Sampling Air In MIMS Sampling Air Ions Mass Analyzer Analyte Air Out 21
22 Vapor Sampling MIMS Sampling TICs and CWAs Toluene TIC Methyl Salicylate CWA Simulant DMMP CWA Simulant 22
23 Operating Interface Simplified user interface 23
24 Summary Identified and responded to the need for advanced, portable downrange GC/MS system Supporting industry has responded with significant advancements Pumps Electronics Balance of performance, SWaP, and cost while maintaining operability in challenging environments 24
25 Thank you Mitch Wells
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