BRINGING THE SCIENCE OF THE LABORATORY TO THE CRIME SCENE
WITH NEXT GENERATION ANALYSIS TOOLS
Dr. James Wylde, Vice President – 1st Detect Corporation | David Rafferty, President and CTO – 1st Detect Corporation | Deborah Burton, Managing Director – TransGlobal Distributors BV
ACKNOWLEDGEMENTS
Portions of the work presented here were funded by the US Army Defense Threat Reduction Agency - Joint Science and Technology Office and the US Army Dugway Proving Ground under Contract No. W911S6-10-C-0012. Any opinions, findings and conclusions or recommendations
expressed in this material are those of the author(s) and do not necessarily reflect the views of the DTRA JSTO or Dugway Proving Ground.
ABSTRACT
Bringing Science the science of the laboratory to the Crime Scene will create a Paradigm shift in the way investigation
teams utilize forensic capabilities to analyze, identify and formulate results in real time. It is well known that the first 48
hours after a crime is a critical period to improve the probability of solving the crime. Crucial time can be lost while
collecting samples and transporting them to a laboratory for analysis. Also, missed evidence may only be identified after
laboratory analysis is complete and the crime scene closed. The miniaturization and automation of traditional analytical
techniques opens the door to faster, more accurate analysis of data outside the traditional laboratory, thus improving
the turnaround time needed to identify forensic evidence so law enforcement can solve crimes faster. However, there is
an inevitable trade off in performance with the miniaturization of laboratory analytical tools, limiting their utility for
providing the forensic quality analysis required for law enforcement. The concept of bringing the lab to the crime scene
is only achievable when lab instrumentation can be miniaturized in a way that ensures the same level of performance,
accuracy and chemical detection expected from traditional lab instruments. The workhorse of traditional labs have is
the mass spectrometer; however traditional mass spectrometers require dedicated infrastructure to support a scientific
laboratory environment.
MINIATURE MASS SPECTROMETER
The instrument developed by the authors is a small (< 20 l volume, < 8 kg weight) mass spectrometer based on an ion
trap architecture. In short, the instrument is capable of:
• 30 – 450 amu mass range (covering most explosives, TICs, and CWAs)
• < 0.5 amu resolution (FWHM)
• Sample-to-sample time: < 1 second (30 seconds with described pre-concentrator or desorber)
• Power consumption: < 45 W (average) / < 65 W (maximum)
• Sensitivity: < 10 ppb VOCs (< 1 ppt with pre-concentrator)
Figure 1 below shows three variants of the instruments.
Figure 1 – Photographs of 3 variants of 1st Detect miniature mass spectrometer including bench-top (left), handheld (center), and sub-
component (right)
Figure 2 – representative explosives spectra showing traditional explosives PETN (top left), RDX (top center), and HMTD (top right); as well
an improvised explosives UN (bottom left), AN (bottom center); and taggant EGDN (bottom right)
THERMAL DESORBER
To enable particulate and ‘sticky’ substances to cross the vacuum barrier into the mass spectrometer, a novel thermal
desorption system is being developed. The sample inlet allows collection of explosive particulate using a swipe method
similar to those in use today. However, to allow transfer of the vaporized explosive particulate into the vacuum
chamber, the desorber is configured to evacuate the volume prior to desorption thus allowing direct injection of the
sample into the instrument without the need for external ionization or ion transport (e.g., ion funnel or quadrupole ion
guide).
Figure 5 – thermal desorber (left) and spectrum of HCE particulate post desorption
PURGE AND TRAP
The enable collection of threats agents from non-gaseous media, a novel purge and trap system has been developed
utilizing the preconcentrator presented previously. A reduced pressure headspace is created over a liquid sample, and
air bubbled through the system to release analyte. Preconcentration of the sample has been achieved with customized
adsorption matrix in a geometry optimized both for maximum adsorption collection as well as efficient high yield
desorption via direct introduction into the mass spectrometer at reduced pressure. The integrated design of the
preconcentrator with the chemical detection system is targeted at sensitive analysis of vapor samples.
Figure 4 – Photograph (left and center) of water sampler and representative data (right) showing measurement of 10 ppb
benzene and chloroform in water
m/z
50 100 150 200
Intensity
0
1000
2000
3000
4000
5000
10 ppb Concentration Mass Spectrum
Benzene peak
(78 m/z)
Chloroformpeak
(82 m/z)
PRE-CONCENTRATOR
A novel pre-concentrator has been designed that leverages the selective sorptive capabilities of advanced materials
with a novel design that significantly reduces the analysis time compared to currently deployed instruments. In the
design sorbent materials are placed in a tube with a heating element. The electrical leads of the heater is connected to
a power supply controlled by a computer system. Because the tube housing the sorbent is evacuated thus minimizing
the dead volume effect prior to thermal desorption, the overall concentration gain is a product of the adsorption and
evacuation gains yielding a typical total gain in the range of 104. Typical analysis times are less than 30 seconds.
Figure 6 – pre-concentrator (right) and location on MMS-1000 (left)
Figure 7 – increase in sensitivity of MMS-1000 showing pre-concentration gain of ~104
Figure 9 – Repeatability performance of pre-concentrator
Figure 3 – Example of MSn (MS/MS) mode of operation
1
10
100
1000
10000
100000
1000000
10000000
100000000
0.01 0.1 1 10 100 1000 10000
Intensity(AU)
Concentration (ppb)
MMS-1000 Instrument Dynamic Range
Pre-concentratorand Membrane Inlets (xylene)
MembraneInlet
Pre-concentrator
C3 C4
C5
ETHYLBENZENE
Figure 8 – Separation of C3-C5 in ethylbenzene background

Bringing the Science of the Laboratory to the Crime Scence Poster

  • 1.
    BRINGING THE SCIENCEOF THE LABORATORY TO THE CRIME SCENE WITH NEXT GENERATION ANALYSIS TOOLS Dr. James Wylde, Vice President – 1st Detect Corporation | David Rafferty, President and CTO – 1st Detect Corporation | Deborah Burton, Managing Director – TransGlobal Distributors BV ACKNOWLEDGEMENTS Portions of the work presented here were funded by the US Army Defense Threat Reduction Agency - Joint Science and Technology Office and the US Army Dugway Proving Ground under Contract No. W911S6-10-C-0012. Any opinions, findings and conclusions or recommendations expressed in this material are those of the author(s) and do not necessarily reflect the views of the DTRA JSTO or Dugway Proving Ground. ABSTRACT Bringing Science the science of the laboratory to the Crime Scene will create a Paradigm shift in the way investigation teams utilize forensic capabilities to analyze, identify and formulate results in real time. It is well known that the first 48 hours after a crime is a critical period to improve the probability of solving the crime. Crucial time can be lost while collecting samples and transporting them to a laboratory for analysis. Also, missed evidence may only be identified after laboratory analysis is complete and the crime scene closed. The miniaturization and automation of traditional analytical techniques opens the door to faster, more accurate analysis of data outside the traditional laboratory, thus improving the turnaround time needed to identify forensic evidence so law enforcement can solve crimes faster. However, there is an inevitable trade off in performance with the miniaturization of laboratory analytical tools, limiting their utility for providing the forensic quality analysis required for law enforcement. The concept of bringing the lab to the crime scene is only achievable when lab instrumentation can be miniaturized in a way that ensures the same level of performance, accuracy and chemical detection expected from traditional lab instruments. The workhorse of traditional labs have is the mass spectrometer; however traditional mass spectrometers require dedicated infrastructure to support a scientific laboratory environment. MINIATURE MASS SPECTROMETER The instrument developed by the authors is a small (< 20 l volume, < 8 kg weight) mass spectrometer based on an ion trap architecture. In short, the instrument is capable of: • 30 – 450 amu mass range (covering most explosives, TICs, and CWAs) • < 0.5 amu resolution (FWHM) • Sample-to-sample time: < 1 second (30 seconds with described pre-concentrator or desorber) • Power consumption: < 45 W (average) / < 65 W (maximum) • Sensitivity: < 10 ppb VOCs (< 1 ppt with pre-concentrator) Figure 1 below shows three variants of the instruments. Figure 1 – Photographs of 3 variants of 1st Detect miniature mass spectrometer including bench-top (left), handheld (center), and sub- component (right) Figure 2 – representative explosives spectra showing traditional explosives PETN (top left), RDX (top center), and HMTD (top right); as well an improvised explosives UN (bottom left), AN (bottom center); and taggant EGDN (bottom right) THERMAL DESORBER To enable particulate and ‘sticky’ substances to cross the vacuum barrier into the mass spectrometer, a novel thermal desorption system is being developed. The sample inlet allows collection of explosive particulate using a swipe method similar to those in use today. However, to allow transfer of the vaporized explosive particulate into the vacuum chamber, the desorber is configured to evacuate the volume prior to desorption thus allowing direct injection of the sample into the instrument without the need for external ionization or ion transport (e.g., ion funnel or quadrupole ion guide). Figure 5 – thermal desorber (left) and spectrum of HCE particulate post desorption PURGE AND TRAP The enable collection of threats agents from non-gaseous media, a novel purge and trap system has been developed utilizing the preconcentrator presented previously. A reduced pressure headspace is created over a liquid sample, and air bubbled through the system to release analyte. Preconcentration of the sample has been achieved with customized adsorption matrix in a geometry optimized both for maximum adsorption collection as well as efficient high yield desorption via direct introduction into the mass spectrometer at reduced pressure. The integrated design of the preconcentrator with the chemical detection system is targeted at sensitive analysis of vapor samples. Figure 4 – Photograph (left and center) of water sampler and representative data (right) showing measurement of 10 ppb benzene and chloroform in water m/z 50 100 150 200 Intensity 0 1000 2000 3000 4000 5000 10 ppb Concentration Mass Spectrum Benzene peak (78 m/z) Chloroformpeak (82 m/z) PRE-CONCENTRATOR A novel pre-concentrator has been designed that leverages the selective sorptive capabilities of advanced materials with a novel design that significantly reduces the analysis time compared to currently deployed instruments. In the design sorbent materials are placed in a tube with a heating element. The electrical leads of the heater is connected to a power supply controlled by a computer system. Because the tube housing the sorbent is evacuated thus minimizing the dead volume effect prior to thermal desorption, the overall concentration gain is a product of the adsorption and evacuation gains yielding a typical total gain in the range of 104. Typical analysis times are less than 30 seconds. Figure 6 – pre-concentrator (right) and location on MMS-1000 (left) Figure 7 – increase in sensitivity of MMS-1000 showing pre-concentration gain of ~104 Figure 9 – Repeatability performance of pre-concentrator Figure 3 – Example of MSn (MS/MS) mode of operation 1 10 100 1000 10000 100000 1000000 10000000 100000000 0.01 0.1 1 10 100 1000 10000 Intensity(AU) Concentration (ppb) MMS-1000 Instrument Dynamic Range Pre-concentratorand Membrane Inlets (xylene) MembraneInlet Pre-concentrator C3 C4 C5 ETHYLBENZENE Figure 8 – Separation of C3-C5 in ethylbenzene background