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NOVEL SAMPLE INLETS TO ENABLE MASS
SPECTROMETRIC DETECTION OF
EXPLOSIVES
WARREN MINO, DAVID RAFFERTY, ABRAR RIAZ, MICHAEL SPENCER,
JAMES WYLDE
TEDW 2013
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INTRODUCTION
MASS SPECTROMETRY IN EXPLOSIVES DETECTION
RECAP OF PREVIOUS WORK
SAMPLE INTRODUCTION
CASE STUDY
CONCLUSION
PRESENTATION OUTLINE
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CORPORATE BACKGROUND
SUBSIDIARY OF ASTROTECH CORPORATION (NASDAQ:ASTC) – AUSTIN TX
‒ Leverage technology developed for space program into terrestrial
space
‒ Amibitious needs of space program = incubate cutting edge
technologies
1st DETECT FOUNDED NOV 2007 TO COMMERCIALIZE MS TECHNOLOGY
DESIGNED FOR SPACE PROGRAM
‒ Air quality monitoring for ISS
‒ 400 compounds to low ppb
‒ NO SERVICE DEPOTS NEARBY!
OVERVIEW – 1ST DETECT CORP
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OVERVIEW – 1ST DETECT MMS-1000™
TRUE PORTABLE MASS SPECTROMETER
 Cylindrical Ion Trap
 Commercial release at Pittcon 2012
PORTABLE SIZE & LIGHTWEIGHT
 6”x 12”x 8” / 4 - 7 kg (9-16 lbs.)
HIGHLY SENSITIVE
 ppm - direct leak
 ppb - membrane inlet
 ppt - pre-concentrator
KEY PERFORMANCE SPECIFICATIONS
 30 - 450 amu (customizable to ~650 amu)
 < 0.5 amu resolution (< 0.3 amu typical)
 1 sec cycle time (user programmable)
 MS2 capable (MS3 in manual mode) with > 90% efficiency
 ~ 45 W average power consumption (~65 W max)
 Auto mass tune with internal standard
DEPLOYMENTS
 Food and Beverage
 Evolved gas analysis
 CWA / threat detection
 Air quality monitoring
COST COMPETITIVE WITH IMS
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MASS SPECTROMETRY & EXPLOSIVES
Any detection technology is a trade off
More threats
Complexity
Information
SWaP
69
131
155
219
368
355
343
193
393
305
293
255
243
100
205
267
443
Simplicity
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MINIATURE ION TRAP
MINIATURE ION TRAP:
Easily miniaturized: hyperbolic -> cylindrical electrodes
No loss of resolution
No loss of mass range
Manufacturable architecture
Ruggedized for field use
“Free” MS/MS
BUT: Sensitivity can be impacted
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MINIATURE ION TRAP
MINIATURE ION TRAP:
Easily miniaturized: hyperbolic -> cylindrical electrodes
No loss of resolution
No loss of mass range
Manufacturable architecture
Ruggedized for field use
“Free” MS/MS
BUT: Sensitivity can be impacted
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MINIATURE ION TRAP
MINIATURE ION TRAP:
Easily miniaturized: hyperbolic -> cylindrical electrodes
No loss of resolution
No loss of mass range
Manufacturable architecture
Ruggedized for field use
“Free” MS/MS
BUT: Sensitivity can be impacted
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MINIATURE ION TRAP
MINIATURE ION TRAP:
Easily miniaturized: hyperbolic -> cylindrical electrodes
No loss of resolution
No loss of mass range
Manufacturable architecture
Ruggedized for field use
“Free” MS/MS
BUT: Sensitivity can be impacted
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SOLUTION
PRE-CONCENTRATOR (PRECON-1000™)
Resistive mesh coated with sorbent material
Mesh corrugated and inserted into ¼” ID quartz tube
Internal manifold & valve system
Dedicated internal controller and power supply boards
Internal sampling pump (MS roughing pump)
InstalledMesh AssemblyCorrugated MeshCoated Mesh
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104 Gain
PERFORMANCE
PERFORMANCE
Measured concentration gain ~104
Enabled low pptr to sub pptr sensitivity with miniature ion trap MS
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RDX EGDN
HMTD PETN
CASE STUDY – EXPLOSIVE HEADSPACE
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UREA NITRATE AMMONIUM NITRATE
SODIUM PERCHLORATE POTASSIUM PERMANGANATE
CASE STUDY – EXPLOSIVES HEADSPACE
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INTRODUCTION
MASS SPECTROMETRY IN EXPLOSIVES DETECTION
RECAP OF PREVIOUS WORK
SAMPLE INTRODUCTION
CASE STUDY
CONCLUSION
PRESENTATION OUTLINE
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Direct injection –vial
o Sample deposited in glass vial
o Chilled to freeze sample before
evacuation
Heated vial
o Direct or IR
o Internal desorber
Allows direct injection of sample
into vacuum chamber
Direct sampling and IR heating
under test
EXPLOSIVES SAMPLING – DIRECT
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EXPLOSIVES SAMPLING – DIRECT
HMX RDX
HMTD TNT
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MS ETD DETECTOR
MASS SPECTROMETRY: CROSSING THE VACUUM
Membrane Selectivity
Sensitivity
API Gas Load = Pumps
SWaP
Split Flow Sensitivity
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DESORPTION
SOLUTION: EVACUATED DESORBER
Sample collected on standard swab
Evacuated prior to desorption
Functionally mimics pre-concentrator
No sample loss, low power, no selectivoty
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DESORPTION
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EXPLOSIVES SAMPLING – SWAB
TNT HCE
EGDN
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PRECONCENTRATOR (HEADSPACE):
o RDX
o EGDN
o HMTD
o PETN
o Urea Nitrate
EVACUATED DESORBER :
o TNT
o Hexachloroethane
DIRECT INJECTION:
o HMX
o RDX
CONCLUSIONS:
o Demonstrated ionization with EI
o Demonstrated trapping in miniature CIT
o Characteristic peaks identified
o Demonstrated thermal desorption of particulate and SVOC compounds
o Ammonium Nitrate
o Sodium Permanganate
o Potassium Permanganate
o Sodium Perchlorate
o Potassium Perchlorate
EXPLOSIVES DETECTION - SUMMARY
SUMMARY OF EXPLOSIVES ANALYSIS
o HMTD
o TNT
o EGDN
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Residual toluene
Cinnamaldehyde
OATMEAL
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Optimized flow paths
Hybrid desorber -> P/C
Alternate heating methods
Alternate ionization
FUTURE WORK
Molecular Ion
Methyl Salicylate
152 Da
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CONCLUSION
THANK YOU FOR YOUR TIME!
Questions
Comments

1st Detect Corp - TEDW 2013 - rev 1