Micro GCs: Current Capabilities and Future Trends

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1 Micro GCs: Current Capabilities and Future Trends

2 Analytical Rational, Data Quality Objectives, Cost, Time Sample Collection Sample Extraction Extract Analysis Data Analysis Decisions & Actions Detection Limits Standards for Calibration Blanks for QA/QC Actions

3 Types of Air Pollution Criteria Pollutants Acid Rain Industrial Pollutants Oxidized organics (TO15) Ozone Precursors Greenhouse Gases Air Toxics (TO14) Indoor Air

4 GCMS Chromatogram of Rural Air Sample collected in the middle of a field Biogenic Emissions

5 Refinery Site: GC Analysis of Selected Free Product Samples and Airborne Butane Conc.

6 Vapor trail Elephants also possess one of the most well developed senses of smell in the animal kingdom. This keen sense of smell is used not only to locate food and water sources but also for communication. Elephants detect and process many chemical signals in a wide variety of smells throughout their environment. Sources of odors used in chemical communication between elephants include urine, feces, saliva, and secretions from the temporal gland.

7 Breathometer

8 Environmental monitoring Emergency response Chemical Weapons Convention Chemical Warfare Agent Detection Infectious Disease Detection Mobile Labs

9 Volatile Organic Compounds VOCs > to ~0.1mm Hg VP VC to DCB Organic Compound Analysis Semi-volatile Organic Compounds SVOCs ~01mm to mm Hg VP

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11 Issues: false positives vs false negatives

12 Analytical Horsepower GC, IMS Sensors GCMS Ease of Use, Cost

13 Michromonitor 500 Stanford GC on a chip

14 MTI M200 Diagram Silicon TCD M200 GC module insulated Acrylic encapsulated Silicon injector chip

15 Stanford Silicon GC Silicon micro GC Evolution Gas Only Analyzers MTI Michromonitor 500 Inficon Fusion Silicon Injector Chip Agilent 3000 SLS µgc Agilent 490 PRO C2V MTI Chrompack MTI Michromonitor 200 M200 CP 2000 CP 3200 Varian

16 either open tubular or PLOT Temp Ramp 1 C/s 15 C/sec Cooldown columns oven sheath ~1mm ID column #1 100 micron ID DB-5 column #2 100 column micron #2ID DB-1701 column heater column heater sheath The microfast GC s Column Temperature vs. Heating Rates 5 C/sec Temp Ramp 5 C/s Cooldown under research for the CWC sponsored by the DNA via a subcontract to General Research Corp, Santa Barbara CA Robert V Mustacich, PI

17 ultra fast temperature programming the microfast GC

18 C1 C2 C3 microfast GC Analysis of Natural Gas 30 C to C/sec C4 C5 C6 T=0 T=35 sec Permanent Gases, Volatiles and Semivolatiles on a micro GC 60s 120s

19 Septum cap injector Bottom of injector Trap and Heater Injector heater Port to columns micro trap and heater Concentration Trap Injector Facilitates Multi Sampling Capacity: Normal/large volume injections Gases, dilute gases (ppb level) Static and dynamic headspace SPME Membrane & external concentrators Purge and trap extracts Liquid organic solvent extracts Neat organic liquid mixtures Aqueous liquids Thermal desorption tubes Thermal and SCF extracts

20 Fast microgc using Bruker Scion TQ as a fast scanning MS detector 50 µid deactivated fused silica capillary connected from the columns end directly into ion source

21 Inject Time B T Xy EB BrB fast microgc using Bruker TQ MS Detector DB µ column, 30 to 200 C at 3 C/sec Scam Speed = 100ms 50 to 300 amu IPB TMB TMB n-bub Scan Speed 80ms 50 to 300 amu TCB Nap TCB Scan Speed 50ms 50 to 300 amu B= benzene T= tpulene Xy= xylenes EB= ethyl benzene BrB= bromobenzene TMB= trimethylbenzene IPB= isopropylbenzene N-BuB= butylbenzene TCB=trichlorobenzene Nap= naphthalene 0.25 min 0.5 min 0.75 min 1 min

22 1,2,4-trichlorobenzene fast microgc using Bruker TQ MS Detector DB µ column, 30 to 200 C at 3 C/sec 50 to 300 amu, 50 ms scan speed Retention times off due to manual injection

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24 microfast GC Analysis 30 second separations Green: BTEX 10 ppm Red: Headspace Bakken Oil Falcon Calidus 101HT µgc microfast GC

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27 near atmospheric pressure Ion Trap Mass Spectrometer 908 Devices 27 Drydock Ave., 8th Floor Boston, MA 02210

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29 Where do we go from here? micro small, fast in Conventional applications small? microgc small, fast inexpensive in nonconventional applications by Analyt ca

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