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Technology Transition Workshop
Introduction to Instrumental Detection Technology (Part 2): SPME and PSPME
Technology Transition Workshop| José R. Almirall, Ph.D.
Technology Transition Workshop
Outline • IMS detection of volatiles
− Identification of volatile target compounds − Sampling and preconcentration − Delivery of sample/analytes to detector − Optimization of IMS conditions for new target
compounds − Determine LODs for optimized sampling/detection − Identify sources of false +, false – and potential
interferences
• Comparison between canine and IMS • Novel geometry compatible with IMS • Performance characteristics for PSPME
Introduction to Instrumental Detection Technology: SPME & PSPME 2 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
Technology Transition Workshop
1. Identify the Volatile Chemical
Markers to Target for Detection. Category Vapor Pressure @ STP Boiling Point
Volatile >0.1 torr <100°C
Semi-Volatile 0.1 to 10-7 torr 100-325°C
Non-Volatile <10-7 torr >325°C
Pawliszyn (2002)
Illicit Drugs Pv (torr) Chemical Markers Pv (torr)
Cocaine 1.2 x 10-7 methyl benzoate 0.28 @ 20°C
MDMA (low) Piperonal (3,4-methylenedioxybenzaldehyde)
1.0 @ 87°C
Marijuana (THC) N/A (low) α/β –pinene, limomene,
β-caryophyllene
1 to 3 @ 20°C
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Cocaine Decomposes at *1 and *2
a b
Introduction to Instrumental Detection Technology: SPME & PSPME 4 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
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Cocaine SPME-GC/MS
• 25 g (relatively “fresh” cocaine) in gallon-sized can
• 14hr SPME (Carboxen™-PDMS) extraction at room temperature
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2. Sampling and Preconcentration Solid Phase Microextraction Plunger
Septum piercing needle
Fiber attachment needle
SPME fiber
Barrel
Plunger retaining screw
Advantages Analyte pre-concentration Selectivity Speed Sensitivity Ease of use Equilibrium-based
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Headspace or Air Sampling
When the sample volume is very large (Vf << Vs), the equation can be simplified to:
n = KfsVf C0
• The amount of extracted analyte is independent of the volume of the sample
• The amount extracted corresponds directly with the concentration in the matrix and is mediated by:
– The distribution constant between the fiber and the sample (and between the sample and the headspace)
– The amount of sorbent volume
Introduction to Instrumental Detection Technology: SPME & PSPME 7 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
Technology Transition Workshop
3. Delivery of Sampled Analytes to the Detector – SPME-IMS Interface
Septa Resistor
O-ring
Ion mobility spectrometer nozzle assembly
Carrier gas in
Thermocouple
PATENT PENDING (Almirall, Florida International University)
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RIP
Unidentified ions
Cocaine
? Suspected substance
• Current IMS analyzers and other electronic noses are not optimized to detect volatile signature compounds
Introduction to Instrumental Detection Technology: SPME & PSPME 9 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
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4. Optimize the IMS Instrumental Conditions to Detect Target Compounds
SPME Parameters
Compounds Ko (cm2/V·s)
Temperature (°C)
Drift Flow (ml·min-1)
Sample Flow
(ml·min-1)
Dopant Mode
Piperonal 1.51 80 350 500 Nicotinamide Positive
Methyl Benzoate
1.55 190 250 1000 Air Positive
α/β-Pinene, limomene, β-caryophyllene
1.28 110 50 1000 Nicotinamide Positive
Fiber type: Polydimethyl Siloxane (PDMS), 100μm
Interface temperature: 260° C
Interface warm up: 15 minutes
Introduction to Instrumental Detection Technology: SPME & PSPME 10 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
Technology Transition Workshop
Headspace Air Sampling & Detection of Cocaine By SPME-IMS (5 Minute Extraction, Room Temp.)
-1000
1000
3000
5000
7000
9000
0 5 10 15
Intensity (mV)
Drift Time (ms)
Methyl Benzoate
Blank fiber
Cocaine 5min extr
0.5g of cocaine HCl in a Ziploc bag, sealed in quart can Extracted compound was confirmed by GC/MS
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SPME Extraction Profile (Exposure Time) Cocaine (Methyl Benzoate Detected)
0
400
800
1200
1600
2000
0 5 10 15 20 25 30 35
Intensity (mV)
Extraction Time (min)
3.67 ng3.28 ng
2.67 ng
1.50 ng
5.31 ng
Introduction to Instrumental Detection Technology: SPME & PSPME 12 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
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td = 5.23 msec (MB)
td = 6.75 msec (EDME)
Headspace Air Sampling & Detection of Cocaine By SPME-IMS (30 Minute Extraction)
Introduction to Instrumental Detection Technology: SPME & PSPME 13 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
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Headspace Air Sampling & Detection of Marijuana By SPME-IMS (10 Min. Extraction, Room Temp.)
0
1500
3000
4500
6000
7500
0 2 4 6 8 10 12 14 16
Intensity (mV)
Drift time (msec)
Blank fiber
Marijuana 10min Extr.
1.4 g of marijuana sealed in a quart can
α/β-pinene, limomene
β-caryophyllene
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SPME Extraction Profile (Exposure Time) Marijuana (Pinenes/Caryophyllene Detected)
800
1200
1600
2000
2400
2800
0 2 4 6 8 10 12
Extraction Time (min)
Intensity
(mV)
Pinenes/Limonene
Caryophyllene
1.72 ng 1.70 ng2.12 ng 2.09ng
1.26 ng
Introduction to Instrumental Detection Technology: SPME & PSPME 15 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
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Headspace Air Sampling & Detection of MDMA By SPME-IMS (30 Minute Extraction, Room Temp.)
0
1000
2000
3000
4000
5000
0 2 4 6 8 10 12 14 16
Intensity
(mV)
Drift Time (ms)
Blank fiber
Piperonal
MDMA 30min extr
2.3 g of MDMA sealed in quart can
Introduction to Instrumental Detection Technology: SPME & PSPME 16 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
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SPME Extraction Profile (Exposure time) MDMA (Piperonal Detected)
0
500
1000
1500
2000
0 20 40 60 80 100 120 140 160
Extraction Time (min)
Intensity
(mV)
3.58 ng
3.23 ng
2.35 ng
1.92 ng
1.04 ng
0.49 ng
Introduction to Instrumental Detection Technology: SPME & PSPME 17 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
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Piperonal (Ecstasy Odor) Detection
0
10
20
30
40
50
60
70
80
90
100
1 10 100 1000 10000
Can
ine
Re
spo
nse
(%
)
Permeation Rate (ng s-1) Macias et al. (2010)
Introduction to Instrumental Detection Technology: SPME & PSPME 18 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
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Piperonal (Ecstasy Odor) Detection (Continued)
Macias et al. (2010)
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5. Identify Potential Sources of False Positives and False Negatives
SPME fiber/disk absorption/adsorption
competition
Breakthrough (for dynamic sampling)
Ionization competition
Peak location interference
Lai, Corbin and Almirall (2008)
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Sample flow
Fiber
Tube
Vessel
Suspended Particles Stirrer
Extraction Phase Sample
particle
SPME Configurations
Disk
Introduction to Instrumental Detection Technology: SPME & PSPME 21 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
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Ion Mobility Spectrometry – IMS
Drift Region
Shutter
Reaction Region
Drift Rings
Detector
Drift Gas Dopant Gas
Sample Introduction
Sample (on collection disk)
Heated Desorber
Separation of product ions by mass, charge and shape
All Gas exit
Ion Source
Introduction to Instrumental Detection Technology: SPME & PSPME 22 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
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Planar SPME Geometry
• PSPME increases surface area and capacity • Reduces sampling time • Geometry is amenable for IMS introduction
Modified-syringe SPME Planar SPME
Introduction to Instrumental Detection Technology: SPME & PSPME 23 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
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SEM of Planar SPME
PDMS 67 μm thick
Sol -gel PDMS 168 μm thick
Spin Coating
Dip Coating
Introduction to Instrumental Detection Technology: SPME & PSPME 24 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
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Sampling Approach
Gura et al. (2009)
Introduction to Instrumental Detection Technology: SPME & PSPME 25 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
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MDMA Tablets – Static Sampling (15 Min., Room Temp.)
Introduction to Instrumental Detection Technology: SPME & PSPME 26 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
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Introduction to Instrumental Detection Technology: SPME & PSPME 27 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
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Single Based SP
Ethyl Centralite
Diphenylamine
VV160 VV140 VV150 VV165 VV110
Accurate Arms
Ethyl Centralite 2,4-DNT 2,6-DNT
AA2520
AA2230
VihtaVuori
DNT
Introduction to Instrumental Detection Technology: SPME & PSPME 28 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
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Smiths 400B – Positive Mode, Default Settings Reactant Gas is Nicotinamide: DPA Alarm
RIP K0=1.86
DPA K0=1.61
Introduction to Instrumental Detection Technology: SPME & PSPME 29 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
Technology Transition Workshop
Smiths 400B – Positive Mode, Default Settings Reactant Gas is Nicotinamide: DPA Alarm
RIP K0=1.86
DPA K0=1.61
Introduction to Instrumental Detection Technology: SPME & PSPME 30 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
Technology Transition Workshop
Smiths 400B – Positive Mode, Default Settings Reactant Gas is Nicotinamide: DPA Alarm
RIP K0=1.86 DPA
K0=1.61
EC?, K0 EC=1.24 peak=1.24
Introduction to Instrumental Detection Technology: SPME & PSPME 31 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
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DPA: Planar Sol-Gel PDMS
ND
38 ng
ND 5.8 ng
14 ng 21 ng
Smiths Ionscan® 400B
Introduction to Instrumental Detection Technology: SPME & PSPME 32 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
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0
500
1000
1500
2000
2500
3000
0 20 40 60 80 100
Extraction Time (min)
27 ng
32 ng
48 ng
38 ng 49 ng 37 ng
~15 min extraction is sufficient
Cu
m A
(d
.u.)
DPA Extraction Curve Planar Sol-Gel PDMS: Smiths Ionscan® 400B
Introduction to Instrumental Detection Technology: SPME & PSPME 33 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
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Smokeless Powder Headspace Profiles
Introduction to Instrumental Detection Technology: SPME & PSPME 34 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
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SPME IMS extraction time curve for Flex X (untagged)
explosive
0
50
100
150
200
250
300
0 5 10 15 20 25 30 35
Time of extraction (min)
Mass
detected
(ng)
n-butyl acetate
(i)
Introduction to Instrumental Detection Technology: SPME & PSPME 35 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
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Detection of Plastic Explosives With a Universal Setting
Introduction to Instrumental Detection Technology: SPME & PSPME 36 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
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Dynamic PSPME SEM Characterization a b
c d
Introduction to Instrumental Detection Technology: SPME & PSPME 37 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
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Dynamic Planar SPME Sampling
uncoated coated coated
0
10
20
30
40
0 10 15 20 25 30 40
Mas
s d
ete
cte
d (
ng)
Sampling Time (s)
Sampling Time using 2,4-DNT COMPS (~ 14 ng/s) Q= 1.7 ×10-4 m3∙s-1 or 0.17 L s-1 (Filter is Q= 0.45 L s-1)
2,4- DNT Response Curve
Introduction to Instrumental Detection Technology: SPME & PSPME 38 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
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Introduction to Instrumental Detection Technology: SPME & PSPME 39 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
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Dynamic Extractions (0.17 L s-1)
• Smokeless powders
− 500 mg of All Unique
− 500 mg of IMR® 4198
• Instruments
− Smiths Detection
− IONSCAN-LS®
• Extraction device
− Planar SPME glass filters
Dynamic extractions at 0 cm above the can
Introduction to Instrumental Detection Technology: SPME & PSPME 40 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
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Introduction to Instrumental Detection Technology: SPME & PSPME 41 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
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Introduction to Instrumental Detection Technology: SPME & PSPME 42 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
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Introduction to Instrumental Detection Technology: SPME & PSPME 43 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
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SP and Pentolite Static Extractions (100 mg)
*white bars = 20cm above can; shaded bars = ~150cm (~5ft)
Introduction to Instrumental Detection Technology: SPME & PSPME 44 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
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SP/Pentolite Dynamic Mode Extractions
Introduction to Instrumental Detection Technology: SPME & PSPME 45 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
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Static Extraction of 10 mg of TATP
0
2000
4000
6000
8000
10000
12000
0 100 200 300 400
Am
plitu
de (
mV
)
Extraction time (sec.)
20 °C
25 °C
40 °C
Introduction to Instrumental Detection Technology: SPME & PSPME 46 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
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Dynamic Extraction – 10 mg TATP
-2000
0
2000
4000
6000
8000
10000
0 5 10 15
Max. am
p. (m
V)
Drift time (ms)
PSPME blank 5 sec. …
RIP
TATP
Introduction to Instrumental Detection Technology: SPME & PSPME 47 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
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Conclusions
• IMS can be used for detection of volatiles − Identification of volatile target compounds − Sampling and preconcentration − Delivery of sample/analytes to detector − Optimization of IMS conditions for new target
compounds − Identify sources of false +, false – and potential
interferences
• IMS detectors can complement canines • Novel PSPME geometry is compatible with IMS • PSPME enhances performance (sensitivity)
Introduction to Instrumental Detection Technology: SPME & PSPME 48 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
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Financial Support: National Institute of Justice (Grant # 2006-DN-BX-K027) NIST (Delivery of SPME-IMS interface to Gillen group - 2006) DHS Center of Excellence at URI (Peroxides volatiles - 2010) NIJ Forensic Technology Center of Excellence (NIJ Grant # 2010-DN-BX-K210)
Collaborators: Idaho National Laboratory Jill Scott , Timothy McJunkin, Carla Miller
DHS S&T Transportation Security Laboratory Richard Lareau, Anna Whitehead, Matthew Magee, Alfred Leung
Federal Bureau of Investigation Laboratory Ron Kelly (smokeless powders samples)
Miami Dade Police Department, Crime Laboratory Bureau Inge Corbin and Oliver Spicer (controlled substance sampling)
University of Rhode Island DHS Center of Excellence Jimmie Oxley, James Smith, Jon Canino
ACKNOWLEGMENTS
Introduction to Instrumental Detection Technology: SPME & PSPME 49 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
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Almirall Group – *IMS research
*Dr. Patty Diaz, Dr. Hanh Lai, Dr. Monica Joshi, Wen Fan, Dr. Sigalit Gura, Howard Holness and Mimy Young
Introduction to Instrumental Detection Technology: SPME & PSPME 50 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
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• Gura, S.; Guerra-Diaz, P.; Lai, H.; Almirall, J.R. Enhancement in Sample Collection for the Detection of MDMA Using a Novel Planar SPME (PSPME) Device Coupled to Ion Mobility Spectrometry (IMS). Drug Testing and Analysis 2009, 1, 355-362. http://clusters.fiu.edu/Meet-FIU-Researchers/11-03-09/Almirall-novel-planar-SPME.pdf (accessed August 30, 2011)
• Lai, H.; Corbin, I.; Almirall, J.R. Headspace Sampling and Detection of Cocaine, MDMA, and Marijuana Via Volatile Markers in the Presence of Potential Interferences by Solid Phase Microextraction-Ion Mobility Spectrometry (SPME-IMS). Analytical and Bioanalytical Chemistry 2008, 392(1-2), 105-113.
• Macias, M.S.; Guerra-Diaz, P.; Almirall, J.R.; Furton, K.G. Detection of Piperonal Emitted from Polymer Controlled Odor Mimic Permeation Systems Utilizing Canis familiaris and Solid Phase Microextraction-Ion Mobility Spectrometry. Forensic Science International 2010, 195(1), 132-138.
• Pawliszyn, J. Solid Phase Microextraction. In Sampling and Sample Preparation in Field and Laboratory: Fundamentals and New Directions in Sample Preparation; Pawliszyn, J., Ed.; Comprehensive Analytical Chemistry Series; Elsevier: Oxford, 2002.
Cited Scientific References
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Additional Scientific References
• Almirall, J.R.; Guerra-Diaz, P.; Holness, H.; Furton, K.G. Field Detection of Drugs and Explosives by SPME-IMS, Final Technical Report, Washington, D.C.: U.S. Department of Justice, National Institute of Justice, submitted July 2011.
• Guerra, P.; Lai, H.; Almirall, J.R. Analysis of the Volatile Chemical Markers of Explosives Using Novel Solid Phase Microextraction Coupled to Ion Mobility Spectrometry. Journal of Separation Science 2008, 31(15), 2891-2898.
• Guerra-Diaz, P.; Gura, S.; Almirall, J.R. Dynamic Planar Solid Phase Microextraction-Ion Mobility Spectrometry for Rapid Field Air Sampling and Analysis of Illicit Drugs and Explosives. Analytical Chemistry 2010, 82(7), 2826-2835.
• Gura, S.; Joshi, M.; Almirall, J.R. Solid-Phase Microextraction (SPME) Calibration Using Inkjet Microdrop Printing for Direct Loading of Known Analyte Mass on to SPME Fibers. Analytical and Bioanalytical Chemistry 2010, 398(2), 1049-1060.
• Joshi, M.; Delgado, Y.; Guerra, P.; Lai, H.; Almirall, J.R. Detection of Odor Signatures of Smokeless Powders Using Solid Phase Microextraction Coupled to an Ion Mobility Spectrometer. Forensic Science International 2009, 188, 112-118. http://clusters.fiu.edu/meet-fiu-researchers/11-03-09/almirall-smokeless-powders.pdf (accessed August 30, 2011)
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Additional Scientific References (Continued)
• Joshi, M.; Rigsby, K.; Almirall, J.R. Analysis of the Headspace Composition of Smokeless Powders Using GC-MS, GC-µECD and Ion Mobility Spectrometry. Forensic Science International 2011, 208(1-3), 29-36.
• Lai, H.; Guerra, P.; Joshi, M.; Almirall, J.R. Analysis of Volatile Components of Drugs and Explosives by Solid Phase Microextraction-Ion Mobility Spectrometry. Journal of Separation Science 2008, 31(2), 402-412.
• Lai, H.; Leung, A.; Magee, M.; Almirall, J.R. Identification of Volatile Chemical Signatures from Plastic Explosives by SPME-GC/MS and Detection by Ion Mobility Spectrometry. Analytical and Bioanalytical Chemistry 2010, 396(8), 2997-3007.
• Lai, H.; McJunkin, T.R.; Miller, C.J.; Scott, J.R.; Almirall, J.R. The Predictive Power of SIMION/SDS Simulation Software for Modeling Ion Mobility Spectrometry Instruments. International Journal of Mass Spectrometry 2008, 276(1), 1-8.
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Questions?
Technology Transition Workshops are a project of NIJ’s Forensic Technology Center of Excellence, operated by the National Forensic Science Technology Center (www.nfstc.org), funded through cooperative agreement #2010-DN-BX-K210. These training materials are only for the course instructors and course participants and are for purposes associated solely for this course. Some of the materials may be subject to copyrights held by third parties. None of these materials may be: a) further disseminated or b) accessed by or made available to others. Individuals with questions concerning the permissibility of using these materials are advised to consult NFSTC at [email protected].
Introduction to Instrumental Detection Technology: SPME & PSPME 54 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS
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Contact Information Professor José R. Almirall, Ph.D.
Department of Chemistry and Biochemistry
International Forensic Research Institute
Florida International University
11200 SW 8th Street, OE116
Miami, FL USA
305348.3917
Note: All images and graphics are courtesy of the Dr. José R. Almirall Laboratory unless otherwise indicated.
Introduction to Instrumental Detection Technology: SPME & PSPME 55 Field Detection of Drug and Explosive Odor Signatures Using PSPME-IMS