The document describes 1st Detect's portable mass spectrometer system for detecting explosives. Key points: 1) 1st Detect has developed a portable cylindrical ion trap mass spectrometer that is 6"x12"x8" and 4-7kg, making it truly portable. It has high sensitivity down to ppb-ppt levels. 2) A miniature pre-concentrator is used to increase sensitivity by concentrating samples by factors of 10,000-100,000. This allows detection of parts-per-trillion levels. 3) The system has successfully detected vapor from several explosives including RDX, PETN, TNT, and urea nitrate using the pre-concentrator

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In-Vacuo Thermal Desorption and Detection of
Explosives Using a Miniature Mass Spectrometer
Warren Mino, David Rafferty, Abrar Riaz, Michael Spencer, William Stott, James Wylde
1st Detect Corp
April 2012
Trace Explosives Detection Workshop

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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-tune with internal standard
Deployments
 Pesticide detection (food products)
 Evolved gas analysis
 Explosives & CWA / threat detection
Cost Competitive with IMS

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MOTIVATION
Why mass spectrometry for explosives detection?
Increased specificity and resolution
Increased number of threats detected simultaneously
Confirmational / orthogonal analysis (e.g., GC-MS, MS/MS, etc.)
Easily adapted to new threats
Multiple ionization techniques
However, detection of explosives using MS is hampered by:
Mass specs are inherently vapor analyzers – explosives tend to have low vapor
pressures
Vacuum nature of MS – need to cross vacuum barrier
Thermal disassociation of explosives beyond recognition

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PRE-CONCENTRATOR
SBIR Phase I & Phase II awarded by DTRA &
DPG
Used to measure permeation rate through
protective clothing (ASTM F079*)
Enables fast analysis of swatch testing
Challenge:
Detect 13 TICs to 40 pg / l using miniature
mass spec
1 l / min flow
30 second cycle time
Non-cryogenic
Universal
Accommodate hydrophobic and hydrophilic
compounds
*Standard Test Method for Permeation of Liquids and Gases through
Protective Clothing Materials under Conditions of Continuous Contact

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PRE-CONCENTRATOR
Novel sorbent and design configuration
Increases concentration gain 103 to 105
Dramatically increases the sensitivity of the instrument
30 second cycle time
Gain effected by two means:
Chemical gain of sorbent
Evacuation gain

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Objective: Find lower limit of detection from membrane
inlet and determine gain in concentration (improvement in
sensitivity) with the pre-concentrator
Kin-Tek gas generator was used to create 4 different
concentrations of tetrachloroethylene (TCE) and toluene
TCE Conc: 1.338 ppm, 671 ppb, 340 ppb, and 170 ppb
Toluene Conc: 1.218 ppm, 610 ppb, 305 ppb, 155 ppb
The lowest concentrations (170 ppb TCE) and (155 ppb
Toluene) were used for measuring with the Pre-concentrator
Pre-concentrator was set to 5 seconds of sampling
Pre-concentrator temperature profile was ramped over 15
seconds
PRE-CONCENTRATOR

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PRE-CONCENTRATOR
TCE
m/z 166
Counts: 756
Toluene
m/z 91
Counts: 698
Sample output (TCE 1.338 PPM Toluene 1.218 PPM)

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PRE-CONCENTRATOR
0
5000
10000
15000
20000
25000
0
100
200
300
400
500
600
700
800
0 200 400 600 800 1000 1200 1400
IonCurrent(Counts)
Pre-concentratorInlet
IonCurrent(counts)
MembraneInlet
Concentration (ppb)
Toluene
Toluene (MIMS)
Toluene (PC)
P/C Gain ~252x
0
2000
4000
6000
8000
10000
12000
14000
16000
18000
0
100
200
300
400
500
600
700
800
0 200 400 600 800 1000 1200 1400 1600
IonCurrent(Counts)
Pre-concentratorInlet
IonCurrent(counts)
MembraneInlet
Concentration (ppb)
TCE
TCE(MIMS)
TCE(PC)
P/C Gain ~224x
Measured gains
TCE: 225x
Toluene: 252x
However:
Lower concentrations
governed by lower
limit of gas generator
Lowest gas generator
concentration
saturated detector
with P/C activated
Gains expected 103 - 105

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PRE-CONCENTRATOR
Measured gains on QQQ with diluted samples (< 1 ppb)
Gain 103 – 105 measured
Instrument ppb -> pptr
1.E-01
1.E+00
1.E+01
1.E+02
1.E+03
1.E+04
1.E+05
1.E+06
Direct Sorbent1 Sorbent2 Sorbent3 Sorbent4
TotalIonCurrent
Pre-concentratorGain
Nitrobenzene
1.E-01
1.E+00
1.E+01
1.E+02
1.E+03
1.E+04
1.E+05
Direct Sorbent1 Sorbent2 Sorbent3 Sorbent4
TotalIonCurrent
Pre-concentratorGain
Acetone
1.E-01
1.E+00
1.E+01
1.E+02
1.E+03
1.E+04
Direct Sorbent1 Sorbent2 Sorbent3 Sorbent4
TotalIonCurrent
Pre-concentratorGain
Ethyl Acetate

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EXPLOSIVES DETECTION
Objective: demonstrate that the MMS-1000 with EI is able to
measure a representative list of explosives
Experimental:
Explosive standards (1 mg/ml in MeOH) presented to pre-
concentrator
Headspace sampled for 10 seconds
Pre-concentrator evacuated (~1 mTorr)
Analyte desorbed using 30 second ramp profile

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EXPLOSIVES DETECTION
The requisite plot for vapor folks……

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PERFLUORODECALIN
443
RDX
EXPLOSIVES

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PERFLUORODECALIN
443
UREA NITRATE
EXPLOSIVES

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PERFLUORODECALIN
443
AMMONIUM NITRATE
EXPLOSIVES

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EXPLOSIVES
PERFLUORODECALIN
443
HMTD

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EXPLOSIVES
PERFLUORODECALIN
443
PETN

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EXPLOSIVES
PERFLUORODECALIN
443
EGDN

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PERFLUORODECALIN
443
EGDN
SEPARATION
P/C can be operated with a
temperature ramp rather
than ‘flash’ desorbed
Software also allows for
single ion monitoring
Will provide functionality
similar to GC but without the
time and power
requirements

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CONTACT SAMPLING

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CONTACT SAMPLING - EXAMPLE
PERFLUORODECALIN
443
199
179
152
138
162124
93
DIAZINON

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PHOTOIONIZATION
Xylene

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PHOTOIONIZATION
Methyl Salicylate

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Headspace over traditional and nitrate based HMEs
demonstrated with pre-concentrator
Characteristic spectra measured for candidate explosives
Thermal desorption demonstrated with vacuum based MS
Alternate ionization demonstrated for parent precursor
molecule detection
Next steps:
Salts
Characterization (detection limits, interferents, de-
convolution / identification, etc.)
Optimization
CONCLUSIONS

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Acknowledgements
Defense Threat Reduction Agency, JSTO-CBD
University of North Texas
1st Detect Houston R&D Team
Thank you for your time