GUARDION⢠7 Hand-Portable Gas Chromatograph-Toroid Ion Trap ...
GUARDION⢠7 Hand-Portable Gas Chromatograph-Toroid Ion Trap ...
GUARDION⢠7 Hand-Portable Gas Chromatograph-Toroid Ion Trap ...
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The GUARDION ® -7 <strong>Hand</strong>-<br />
<strong>Portable</strong> GC-TMS: Recent<br />
Enhancements and New<br />
Applications<br />
Douglas W. Later, Christopher R. Bowerbank,<br />
Joseph L. Oliphant, Tiffany C. Wirth, Edger D.<br />
Lee, and Charles S. Sadowski<br />
September 23 rd , 2009
Presentation Outline<br />
• Next Generation GC-TMS<br />
– <strong>Toroid</strong>al ion <strong>Trap</strong> Mass Spectrometer<br />
– Low Thermal Mass Capillary GC<br />
– SPME Sampling and Injection<br />
– Deconvolution Software<br />
• Recent TMS Enhancements<br />
• GC-TMS Applications
The Next Generation <strong>Hand</strong>-<strong>Portable</strong> GC-MS
Next Generation MS: Smaller-Lighter-Faster<br />
• Significant improvement from current instruments:<br />
– Size Reduction<br />
– Weight Reduction<br />
– Speed of Analysis<br />
– Ease of Use<br />
• Operates reliably in harsh environments<br />
• Lower sustainment costs<br />
– Consumables<br />
– Training<br />
• Broader Analytical capabilities<br />
– Volatile and Semivolatile Compounds
Advantages of <strong>Ion</strong> <strong>Trap</strong>s for HEMS<br />
• Simple, rugged design (no critical alignment<br />
of ion optics)<br />
• Less stringent vacuum requirements<br />
(requires 1 mtorr operating pressure)<br />
• High duty cycle High sensitivity<br />
• Low power (especially with small ion trap<br />
mass analyzers)<br />
• High sensitivity and selectivity<br />
• MS-MS capabilities
Different <strong>Ion</strong> <strong>Trap</strong> Configurations<br />
Quadrupole ion<br />
trap or Paul trap<br />
Cylindrical ion trap<br />
Rectilinear ion trap<br />
Quadrupole<br />
mass filter<br />
Linear ion trap<br />
<strong>Toroid</strong>al ion trap<br />
Halo ion trap
Mitigating Factors of <strong>Ion</strong> <strong>Trap</strong>s<br />
• 3-D ion trap is an “ion bottle” with<br />
somewhat fixed relative<br />
dimensions (r o vs. z o )<br />
• <strong>Ion</strong>-ion repulsion (space charge)<br />
• Commercial traps optimized at<br />
r o = 1 cm, ~16 kV p-p<br />
• Further increase in r o not practical<br />
due to arcing of RF high voltage<br />
• Decrease of r o yields lower RF<br />
power, but will lead to earlier onset<br />
of space charge<br />
−8eV<br />
q =<br />
2<br />
m(<br />
r 0<br />
+ 2z<br />
) Ω<br />
2 2<br />
0<br />
z o<br />
r o
Why <strong>Toroid</strong>al <strong>Ion</strong> <strong>Trap</strong> Mass Spectrometry?<br />
• Single mass analysis volume (compared to<br />
arrayed miniature cylindrical ion traps)<br />
– All ions experience the same trapping/mass<br />
analysis field<br />
– Easier coupling to ionization and detection<br />
optics<br />
• Compact geometry (compared to linear ion traps<br />
of similar storage capacity)<br />
• Homogenous field (compared to linear ion traps)<br />
– No end effects. All spatial positions within mass<br />
analyzer are equivalent
Innovation in <strong>Ion</strong> <strong>Trap</strong> MS<br />
Conventional <strong>Ion</strong> <strong>Trap</strong><br />
<strong>Toroid</strong>al <strong>Ion</strong> <strong>Trap</strong>
GUARDION ® -7 GC-TMS Specifications<br />
Specifications<br />
• Dimensions: 47 cm x 36 cm x 18 cm<br />
• Weight:
Torion GUARDION ® -7 GC-TMS Components<br />
Vacuum Chamber<br />
with <strong>Toroid</strong>al <strong>Ion</strong> <strong>Trap</strong><br />
Electronics<br />
Batteries<br />
Diaphragm<br />
Pump<br />
Turbo<br />
Molecular<br />
Pump<br />
GC System<br />
He <strong>Gas</strong><br />
Cartridge
Miniaturized <strong>Toroid</strong>al <strong>Ion</strong> <strong>Trap</strong> Mass Spectrometer<br />
• RF <strong>Trap</strong>ping Field:<br />
– 4 MHz<br />
– 1200 (max) V p-p<br />
• Resonance Ejection:<br />
– 1.8 MHz - 110 KHz<br />
– 5 V amplitude<br />
• Pressures:<br />
– He buffer gas: 10 -3 to 10 -4 mbar<br />
• r° = 2 mm
LTM Capillary <strong>Gas</strong> <strong>Chromatograph</strong><br />
Solenoid<br />
Valves<br />
LTM SPME<br />
Column: MXT-5 (5 m x 0.1 mm x 0.4 µm)<br />
Injector<br />
• Column:<br />
• Mobile Phase: Helium<br />
• Head Pressure: 25 psig<br />
Transferline<br />
to MS<br />
• Column Max Flow: 0.7 scc/min @ 20 o C<br />
• Split-splitless Injection:<br />
splitless Injection: Split ratio 20<br />
• Program: 40 o C (hold 10 s) to 300 o C (hold 10 s) @ 120 o C/min<br />
• GC-TMS run time:
Advantages of SPME Sample Collection and Injection<br />
• Solvent-free<br />
• Reusable<br />
• Finite sampling capacity<br />
• Simple to use<br />
• Faster than other extraction<br />
techniques<br />
• Low cost per sample<br />
• Applicable to air, liquid, and<br />
solid samples<br />
• Different phases available<br />
for selective sampling<br />
Ultem<br />
Body<br />
Memory Chip<br />
Board
Easy to Use Software<br />
• On-board and Computer-based Software<br />
• Three button instrument operation<br />
• Simple GUI interface - results are clear and concise<br />
• Automated target compound identification
On Board Peak Deconvolution<br />
• Original mass spectral data effectively resolved into components<br />
• Extract accurate individual mass spectra for each analyte<br />
• Accurately distribute the signal from masses shared by several<br />
components<br />
TIC<br />
91<br />
75<br />
83
Recent TMS Enhancements<br />
• Surface Finish<br />
• Electronic Pressure Control<br />
• Better Modeling<br />
• Improved Slit Design
Effects of Surface Finish on TMS Performance<br />
Resolution vs. Sample Repetition at m/z 173<br />
Gold Plating: Method #1<br />
Gold Plating: Method #2<br />
EXPORT CONTROLLED – ITAR RESTRICTED<br />
Any 'Technical Information' relating to Torion Technologies products included herein is considered technical data as defined in 22<br />
CFR 120.10 of the International Traffic in Arms Regulations (ITAR), and is subject to export control laws of the U.S. Department of<br />
State. Retransfer of this data to a foreign person, whether in the U.S. or abroad, requires U.S. Department of State approval.
Electronic Pressure Control<br />
• Increase chromatographic performance and reproducibility for more<br />
accurate target compound identification<br />
• Improves MS reproducibility due to constant helium levels in trap<br />
05-07-2009<br />
05-12-2009<br />
EXPORT CONTROLLED – ITAR RESTRICTED<br />
Any 'Technical Information' relating to Torion Technologies products included herein is considered technical data as defined in 22<br />
CFR 120.10 of the International Traffic in Arms Regulations (ITAR), and is subject to export control laws of the U.S. Department of<br />
State. Retransfer of this data to a foreign person, whether in the U.S. or abroad, requires U.S. Department of State approval.
Simion Equipotential and Potential Gradient Plots<br />
Symmetric <strong>Toroid</strong>al <strong>Trap</strong><br />
Asymmetric <strong>Toroid</strong>al <strong>Trap</strong><br />
EXPORT CONTROLLED – ITAR RESTRICTED<br />
Any 'Technical Information' relating to Torion Technologies products included herein is considered technical data as defined in 22<br />
CFR 120.10 of the International Traffic in Arms Regulations (ITAR), and is subject to export control laws of the U.S. Department of<br />
State. Retransfer of this data to a foreign person, whether in the U.S. or abroad, requires U.S. Department of State approval.
Electric Field Gradient Plots for TMS and CIT<br />
EXPORT CONTROLLED – ITAR RESTRICTED<br />
Any 'Technical Information' relating to Torion Technologies products included herein is considered technical data as defined in 22<br />
CFR 120.10 of the International Traffic in Arms Regulations (ITAR), and is subject to export control laws of the U.S. Department of<br />
State. Retransfer of this data to a foreign person, whether in the U.S. or abroad, requires U.S. Department of State approval.
Simion Potential Gradient Plot and <strong>Ion</strong> Flight Modeling<br />
Asymmetric <strong>Toroid</strong>al <strong>Trap</strong> with Screened Slit Modification<br />
Modeled Data<br />
TMS Data<br />
EXPORT CONTROLLED – ITAR RESTRICTED<br />
Any 'Technical Information' relating to Torion Technologies products included herein is considered technical data as defined in 22<br />
CFR 120.10 of the International Traffic in Arms Regulations (ITAR), and is subject to export control laws of the U.S. Department of<br />
State. Retransfer of this data to a foreign person, whether in the U.S. or abroad, requires U.S. Department of State approval.
EDM and Screened Slits: Detector-side End Cap<br />
EDM Slit<br />
Screened Slit<br />
23<br />
EXPORT CONTROLLED – ITAR RESTRICTED<br />
Any 'Technical Information' relating to Torion Technologies products included herein is considered technical data as defined in 22<br />
CFR 120.10 of the International Traffic in Arms Regulations (ITAR), and is subject to export control laws of the U.S. Department of<br />
State. Retransfer of this data to a foreign person, whether in the U.S. or abroad, requires U.S. Department of State approval.
Raw Data From EDM and Screened Slits<br />
Toluene Mass 91 and 92 EDM Slits<br />
Bromoform Mass 171, 173 and 175 EDM Slits<br />
Toluene Mass 91 and 92 Screened Slits<br />
Bromoform Mass 171,173 and 175 Screened Slits<br />
Average of All Scans Across <strong>Chromatograph</strong>ic Peak<br />
EXPORT CONTROLLED – ITAR RESTRICTED<br />
Any 'Technical Information' relating to Torion Technologies products included herein is considered technical data as defined in 22<br />
CFR 120.10 of the International Traffic in Arms Regulations (ITAR), and is subject to export control laws of the U.S. Department of<br />
State. Retransfer of this data to a foreign person, whether in the U.S. or abroad, requires U.S. Department of State approval.
Scan-to-Scan Reproducibility with EDM Slit <strong>Trap</strong><br />
Toluene<br />
Start<br />
Middle<br />
End<br />
EXPORT CONTROLLED – ITAR RESTRICTED<br />
Any 'Technical Information' relating to Torion Technologies products included herein is considered technical data as defined in 22<br />
CFR 120.10 of the International Traffic in Arms Regulations (ITAR), and is subject to export control laws of the U.S. Department of<br />
State. Retransfer of this data to a foreign person, whether in the U.S. or abroad, requires U.S. Department of State approval.
Scan-to-Scan Reproducibility with Screened Slits<br />
Toluene<br />
Start<br />
Middle<br />
End<br />
EXPORT CONTROLLED – ITAR RESTRICTED<br />
Any 'Technical Information' relating to Torion Technologies products included herein is considered technical data as defined in 22<br />
CFR 120.10 of the International Traffic in Arms Regulations (ITAR), and is subject to export control laws of the U.S. Department of<br />
State. Retransfer of this data to a foreign person, whether in the U.S. or abroad, requires U.S. Department of State approval.
Recent GC-TMS Applications
GC-TMS Analysis of Hazardous Compounds
Volatiles (VOCs) in Water<br />
Tetrachloroethylene<br />
Headspace<br />
75 ppb in water<br />
Chlorobenzene<br />
Direct sampling<br />
20 ppm in water
Volatiles (VOCs) in Soil<br />
10,11<br />
13<br />
14<br />
17<br />
16<br />
18<br />
19<br />
20<br />
PDMS/DVB SPME<br />
Phase<br />
9<br />
12<br />
15<br />
21<br />
7,8<br />
22<br />
23<br />
3<br />
6<br />
1,2<br />
4 5
Analysis of Semivolatile Compounds<br />
Alkanes<br />
C13 C15<br />
C12 C14<br />
C16<br />
C11<br />
C10<br />
C17<br />
C18<br />
C19<br />
C20<br />
C21<br />
C-20 BP = 342.7 o C<br />
Pesticides<br />
Lindane<br />
Heptachlor<br />
Heptachlor epoxide<br />
Endrin<br />
Melting point of Endrin = 200 o C
Analysis of Chemical Warfare Agents<br />
VX<br />
GUARDION ® -7<br />
m/z<br />
HD<br />
100<br />
50<br />
114<br />
O<br />
O<br />
P<br />
S<br />
NIST<br />
N<br />
m<br />
/<br />
z<br />
72 127<br />
72<br />
127<br />
30 43<br />
79<br />
107<br />
167<br />
27<br />
56<br />
139<br />
252<br />
0<br />
20 30 40 50 60 70 80 90 100 110 120 130 140 150 160 170 180 190 200 210 220 230 240 250 260 270 280<br />
(mainlib) VX
CWA Simulants and TICs<br />
4,5<br />
1. Benzene<br />
2. Toluene<br />
3. Diethyl malonate<br />
4. n-Butyl benzene<br />
5. Diisopropyl methylphosphonate<br />
6. Nitrobenzene<br />
7. Triethylphosphate<br />
8. n-Dodecane<br />
9. Methyl Salicylate<br />
10. Naphthalene<br />
11. Diethyl Phthalate<br />
12. Tributylphosphate<br />
1<br />
2 3<br />
67<br />
8<br />
9<br />
10 11<br />
12
Tetrachloroethylene (TCE) Contamination
BTEX & MTBE in Ground Water<br />
1. MTBE<br />
2. Benzene<br />
3. Toluene<br />
4. Ethylbenzene<br />
5. m-Xylene<br />
6. o-Xylene<br />
2 3<br />
4<br />
5<br />
6<br />
1<br />
15 s headspace sample, 10 ppm
SPME Analysis of Trihalomethanes in Water<br />
1. Chloroform<br />
2. Bromodichloromethane<br />
3. Toluene (DI water contaminant)<br />
4. Dibromochloromethane<br />
5. Bromoform<br />
4<br />
5 100 ppb<br />
1<br />
2<br />
3<br />
10 ppb
12,13,14,15<br />
18,19<br />
16,17<br />
Semivolatiles (SVOCs) in Water<br />
20,21<br />
22<br />
23,24<br />
25,26<br />
27<br />
28<br />
32,33 34<br />
29,30<br />
31<br />
35<br />
36<br />
38,39<br />
37<br />
40<br />
41<br />
42<br />
43,44<br />
45<br />
46<br />
47<br />
PEG SPME Phase<br />
52 compounds identified<br />
in 2.5 min<br />
48<br />
9,10,11<br />
49<br />
6<br />
7<br />
8<br />
50<br />
51<br />
4,5<br />
52<br />
1,2 ,3<br />
Spiked into Tap Water: 1-10 ppm each
Semivolatiles (SVOCs) in Water<br />
1 Aniline 19 2,4‐Dimethylphenol 37 2,4‐Dinitrotoluene<br />
2 Phenol 20 2,4‐Dichlorophenol 38 2,3,4,6‐Tetrachlorophenol<br />
3 Bis(2‐chloroethyl)ether 21 1,2,4‐Trichlorobenzene 39 2,3,5,6‐Tetrachlorophenol<br />
4 2‐Chlorophenol 22 Naphthalene 40 Diethylphthalate<br />
5 1,3‐Dichlorobenzene 23 4‐Chloroaniline 41 4‐Chlorophenyl phenyl ether<br />
6 1,4‐Dichlorobenzene 24 Hexachlorobutadiene 42 Fluorene<br />
7 1,2‐Dichlorobenzene 25 4‐Chloro‐3‐methylphenol 43 Diphenylamine<br />
8 Bis(2‐chloroisopropyl)ether 26 2‐Methylnaphthalene 44 Azobenzene<br />
9 Benzyl alcohol 27 1‐Methylnaphthalene 45 4‐Bromophenyl phenyl ether<br />
10 N‐Nitroso‐di‐n‐propylamine 28 Hexachlorocyclopentadiene 46 Hexachlorobenzene<br />
11 Hexachloroethane 29 2,4,6‐Trichlorophenol 47 Phenanthrene<br />
12 2‐Methylphenol 30 2,4,5‐Trichlorophenol 48 Anthracene<br />
13 4‐Methylphenol 31 2‐Chloronaphthalene 49 Di‐n‐butylphthalate<br />
14 3‐Methylphenol 32 2‐Nitroaniline 50 Fluoranthene<br />
15 Nitrobenzene 33 Dimethylphthalate 51 Pyrene<br />
16 Isophorone 34 Acenaphthylene 52 Benzyl butyl phthalate<br />
17 2‐Nitrophenol 35 Acenaphthene<br />
18 Bis(2‐chloroethoxy)methane 36 Dibenzofuran
Frankincense (spice)<br />
Source #1<br />
110000<br />
100000<br />
90000<br />
80000<br />
70000<br />
60000<br />
50000<br />
40000<br />
30000<br />
20000<br />
10000<br />
GUARDION ® -7<br />
3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.00 14.00<br />
42000<br />
40000<br />
38000<br />
36000<br />
34000<br />
32000<br />
30000<br />
GUARDION ® -7<br />
28000<br />
22000<br />
24000<br />
26000<br />
Source #2<br />
20000<br />
18000<br />
16000<br />
14000<br />
12000<br />
10000<br />
8000<br />
6000<br />
4000<br />
2000<br />
1.00 2.00 3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.00 14.00 15.00
Frankincense (Source #2)<br />
65000<br />
GUARDION ® -7<br />
<strong>Portable</strong> GC-TMS<br />
3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.00<br />
65000<br />
Agilent<br />
Laboratory GC-MS<br />
3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00
Raw Materials Food Quality Monitoring<br />
GUARDION ® -7<strong>Portable</strong> GC-TMS<br />
Cocoa Bean Samples<br />
Source #1<br />
Source #2<br />
*<br />
*<br />
*<br />
*<br />
Source #3<br />
0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6<br />
Time (min)<br />
PDMS/DVB SPME fiber, 20 min headspace exposure, 65 o C<br />
* Potential food quality biomarkers<br />
*<br />
*<br />
*
Thank You – Questions<br />
Questions-Discussion
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