Mobile Mass Spectrometer in daily use Experiences made by non-scientific operators

Transcription

1 Mobile Mass Spectrometer in daily use Experiences made by non-scientific operators Franziska Lange, Thomas Ludwig, Bruker Daltonik GmbH HEMS Workshop, Florida, USA September, 211

2 E 2 M Enhanced Environmental Mass Spectrometer

3 small, lightweight, rugged, sensitive Measurement principle: Vacuum System: Electron source: Filament: Inlet: Mass range: Scan rate: External Power Supply: Quadrupole Mass Filter Ion getter pump < 1-6 mbar Electron Impact, 7 ev dual Silicone membrane, heated 1 52 da 75 da/s, resolution.1 da VDC Power Consumption: 25 Watt (switch-on: 5 W) Transputer Interface: Ethernet (1 Mbit/s) Dimensions: 436 x 368 x 442 (L x W x H) Volume: Weight: Specification: 58 litres 38 kg CE, IP42, IEC 61, IEC and 2-2, CISPR 16-1 and 16-2, IEC , -2-27

4 Various Use of the System MS Monitoring System SIM and Fullscan direct sample introduction GC/MS System Fullscan Pre separation for complex samples Various sample introduction

5 MS Monitoring System Air/Surface Probe direct measurement of air and surface contaminations separately heated probe head and probe line programmable up to 24 C 3.5 m length, flexible exchangeable probe head membranes

6 MS Monitoring System Selected Ion Monitoring Very sensitive Several SIM libraries available, adaptable by the user Up to 2 substances simultaneously Vertical bar graph Colour coded signals Identification in alarm window

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10 GC/MS System temperature controlled gas flow 3 programmable temperature gradients (T max : 24 C) Carrier gas: ambient air GC-capillary: type depends on application robust metal capillaries Standard: MXT -5, 12 m, ID.32 mm film thickness 1 µm or MXT -1, 15 m, ID.32 mm film thickness 5 µm Injector: a) Thermo desorber (various sampling material, tubes) b) Split injector (liquid) c) SPME thermo desorption

11 GC/MS System Chromatogram window Mass spectrum window Automated identification at the end of the run

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13 GC/MS System Fully automated identification within seconds Up to 3 different identification procedures (sensitivity, library used) File information displayed Convertible to pdf files Copy CAS# available for use in several first responder data bases

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16 Mass Spectrometer used by non scientific users

17 Typical non scientific users Fire fighter specialists First responder Mobile forensic investigators Police

18 Sample preparation source of problems

19 Butyric Acid in Dance Club Attack with butyric acid in dancing club in Leipzig odor pollution, evacuation necessary Fire fighter specialists Leipzig Samples of ambient air taken by hand pump, sampling tubes Identification of the agent by GC/MS System Identification of the source (sports bag) further investigations by police

20 Airport Lübeck Supervisory impaired Rusted containers from 2 nd world war with chlorosulfonic acid below ground cause fog all flights stopped Task force Hamburg Identification by MS Monitoring System Instrument partially destroyed due to highly acidic character Pre check with ph stripes essential

21 Shine on River Shine on popular river in Leipzig Fire fighter specialists Leipzig Analysis of water by purge and trap and GC/MS negative Analysis of sediment by solidliquid-extraction with Methanol and GC/MS identification of an old plant protective agent Old barrel found by divers

22 Swedish Coast Guard Ship Integration into gas detection system Combination with other sensors Gas detection 24/7 fullscan

23 Ground contamination Wide area contamination with chlorinated hydrocarbons On-site Measurments with MM2 to determine risks and area together with police and federal office of ground protection Ruin of a fur-manufacturing company in Niedersachsen

24 Ground contamination Intens. x MS, Dissect, s #( ) Nist: Trichloroethylene; Q EI +MS (P: 982, Cl F: 993, R: 982, M: 1) 1 Cl Cl H x MS, Dissect, s #( ) Nist: Tetrachloroethylene; Q EI +MS (P: 939, 166. Cl F: 995, Cl R: 939, M: 1) Cl Cl m/z Sampling of ground air (down to 7 m) Identified substances in ground air # RT [s] Area Compound Name Library CAS# Purity' Trichloroethylene Nist Tetrachloroethylene Nist

25 Dump Air Intens. x Time [s] TIC + Dissect:, Cmpd 1, s Dissect:, Cmpd 2, 343. s Dissect:, Cmpd 3, s Dissect:, Cmpd 4, s Dissect:, Cmpd 5, 73. s Dissect:, Cmpd 6, s Dissect:, Cmpd 7, 8.6 s Dissect:, Cmpd 8, s Dissect:, Cmpd 9, s Dissect:, Cmpd 1, s Dissect:, Cmpd 11, s Dissect:, Cmpd 12, s Identified substances in dump air # RT [s] Area Compound Name Library CAS# Purity' Carbon disulfide Nist Furan, tetrahydro- Nist Toluene Nist Tetrachloroethylene Nist Ethylbenzene Nist Benzene, 1,3-dimethyl- Nist p-xylene Nist Benzene, 1,3,5-trimethyl- Nist Benzene, 1,3-ichloro- Nist Naphthalene Nist

26 Combustion Air Sample 1 stroke Combustion gas sample: Material: unknown Product information: during combustion only CO 2 produced

27 Result: Combustion Air Sample Identified subsatnces in combustion gas # RT [s] Area Compound Name Library CAS# Purity' Phenol Nist Benzaldehyde Nist ,3-Dioxane, 4-phenyl- Nist Hexanol, 2,2-dimethyl- Nist Pyrimidinamine Nist Diaminopyridine Nist Naphthalene Nist Phenoxypropan-2-ol Nist Neodecanoic acid Nist Indole Nist Benzocycloheptatriene Nist Biphenyl Nist Biphenylene Nist Hexanoic acid, 1-naphthyl ester Nist Benz[cd]indol-2(1H)-one Nist Fluorene Nist Phenoxazine Nist Pyridine, 2-(2-phenylethenyl)- Nist ,1b(2H)-Dihydropyrano [3,4,5-jk]fluorene Nist Dibutyl phthalate Nist Isopropyl Palmitate Nist Naphthalene, 2-phenyl- Nist (2-Benzothiazolyl)benzofurane Nist Ethylhexyl trans-4- methoxycinnamate Nist

28 SPME from Tedlar-bag Intens. 1. x MS, Dissect, s #( ) x Nist: Toluene; Q EI +MS (P: 914, F: 974, R: 914, M: 1) MS, Dissect, s #( ) PDMS SPME-fibre Gas sample from Tedlar-Bag (1 min sampling time) 2. Nist: Tetrachloroethylene; Q EI +MS (P: 929, F: 998, R: 929, M: 1) 166. Cl Cl Cl Cl x MS, Dissect, s #( ) Nist: Dimethyl methylphosphonate; Q EI +MS (P: 927, F: 967, R: 939, M: 1) 94. O P O O x MS, Dissect, s #( ) Nist: Methyl Salicylate; Q EI +MS (P: 962, F: 994, R: 962, M: 1) 12. OH O O m/z Identified substances # RT [s] Area Compound Name Library CAS# Purity' Toluene Nist Tetrachloroethylene Nist Dimethyl methylphosphonate Nist Methyl Salicylate Nist

29 Drugs: Cannabis Injection 1 µl (2mg/ml in Methanol)Cannabis; 3,5 m HP5ms,,32 mm ID, 1µm Film Intens. 1. x1 5 +MS, 314. Dissect, s #(179-19) Nist: 6H-Dibenzo[b,D]pyran-1-ol, 6a,7,8,1a-tetrahydro-6,6,9-trimethyl-3-pentyl-; Q EI +MS (P: 847, F: 93, R: 912, M: 1) OH x MS, Dissect, s #( ) O Nist: Cannabinol; Q EI +MS (P: 939, F: 945, R: 98, M: 1) 295. OH m/z 31. O Identified substances # RT [s] Area Compound Name Library CAS# Purity' Tetrahydrocannabinol (THC) Nist Cannabinol Nist

30 Drugs: Cocaine Direcet measurement with probe; 1 µl (2mg/ml in Methanol)Cocaine Intens. x MS, s #(42-112) Nist: Cocaine; Q EI +MS (P: 847, F: 952, R: 847, M: 1) O N 82. H O 182. O H O m/z Identified substances # RT [s] Area Compound Name Library CAS# Purity' Cocaine Nist

31 Drugs: Heroine (Street sample) Injection 1 µl (2mg/ml in Methanol) Heroine; 3,5 m HP5ms,,32 mm ID, 1µm Film Intens. x MS, Dissect, s #(187-22) Nist: Diacetylmorphine; Q EI +MS (P: 882, F: 954, R: 913, M: 1) O N O O O O m/z Identified substances # RT [s] Area Compound Name Library CAS# Purity Novocaine Nist Acetylcodein Nist Diacetylmorphine (Heroine) Nist

32 Military Reconnaissance Mission Response time: 3 2 sec Reconnessaince Mission Spectra Series with Identification Analysis time: 2 3 min Analysis time: 1-15 min

33 Military Reconnaisance Mission Intens. x TIC Time [s] Intens. x MS, Dissect, s #(46-56) Nist: Mustard Gas; (P: 931, F: 981, R: 932, M: 999) 19. S 75 Cl Cl x MS, Dissect, s #( ) Nist: O-Mustard; (P: 949, F: 957, R: 956, M: 999) Cl S O S Cl m/z

34 Things to take care on Good initial education and training necessary to use all available components and options Standard operation procedures may help to handle correctly Basic chemical knowledge essential (also to protect the instrument against damage)

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