FULLY AUTOMATED GUNSHOT RESIDUE ANALYSIS

Introduction
When a gun is fired, hot gasses and small particles are generated during the explosion of the primer and the propellant in the cartridge casing. These particles, as well as those formed by the condensation of some of the hot gases, are deposited on parts of the hand and clothes of the person firing the gun, as well as on other objects in the vicinity of the weapon.


 

These small particles are called gunshot (GSR) or firearms residue. Because they have distinctive characteristics, their presence forms evidence that examined persons have been close to a gun being fired. This kind of evidence is often used in criminal court cases involving the use of firearms.The residues contain elements that result from the propellant and primer decomposing, as well as from the bullet and cartridge case. Samples of GSR are taken from people suspected of firing a gun, by pressing adhesive material to the areas of interest, for example, fingers, the top part of the hand and clothes. In this way particles are transferred from the area of interest onto a small sample for examination in a scanning electron microscope (SEM) connected to an X-ray micro-analysis system equipped with a GSR software package developed by Eastern Analytical. This software package allows automated, unattended classification of GSR particles.




Graphical user interface of the GSR software, showing a typical spectrum GSR 3-component particle in combination with the stage configuration set-up.

 

Finding the GSR particles
The characteristic particles for GSR often contain combinations of the elements Lead (Pb), Barium (Ba) and Antimony (Sb). In general these particles are very small - in the range of 0.5 -10 microns. In the scanning electron microscope, these particles can be found, magnified and analyzed chemically, and the presence of GSR on a sample confirmed.

The elements constituting GSR can originate from the primer, the bullet, a coating or jacket on the bullet, cartridge components, and previous residues in the barrel.



Typical GSR three-component particle.
 

Residue particles are arbitrarily divided into two types, depending on their primary source: primer particles and bullet particles. Particles containing Pb, Sb and Ba and those containing Sb and Ba (also referred to as two-component particles) are typical inorganic components from the primer, and are classified as primer particles. Large numbers of particles composed mainly of Pb originate from the bullet and are termed bullet particles.

In normal GSR suspect-taping, the particles on the adhesive tape are typically less than 10 microns in size (usually 0.5 - 2 microns). There are relatively few particles on the taping, divided over a relatively large area. As the majority of the GSR particles have a small diameter (less than 2 microns), a large surface has to be analyzed in order to yield results of sufficient statistical validity. Because the sample is often not smooth and contains particles which are of no particular interest, the task of locating and analyzing GSR particles manually by operator control is not practical and is a tedious and time-consuming task which runs a high risk of introducing errors. For these reasons, an automatic routine has been developed that allows unattended analysis (overnight) followed by operator-assisted validation and summarizing of results.

 

The automatic routine
The analysis of gunshot residue can be performed using dedicated software such as GSR-XT, which ensures fast, reliable and fully unattended analysis. The GSR-XT software program also identifies other indicative particles similar to the large amounts of Lead (Pb) particles from the bullet, such as Titanium (Ti) and Zinc (Zn) which are found in lead-free ammunition. Other environment-related particles could also provide additional information about the subject.

 


Low magnification image using the backscattered electron detector thresholds to seperate and locate particles.

The steps to perform an analysis are as follows:
Tape is mounted on the stubs
Stubs are placed on a multi-stub holder
Multi-stub holder is mounted on the SEM specimen stage
The stub is split into multiple fields which are scanned
one-by-one
Each area is scanned for particles using backscattered imaging
The position and size of the candidate particles are recorded
The particles are revisited by the electron beam to perform X-ray analysis
The emitted X-ray spectrum from each individual particle is compared to a classification scheme
All results are stored (on disc)
A report of all detected particles is produced after each sample.
The backscattered electron signal is used to detect the particles. Typical GSR particles appear as bright particles within the image. By applying a threshold to the signal, the particles are distinguished and located by the GSR software.

 

Description
The dedicated GSR analysis package is a fully embedded software package for analytical scanning electron microscopes of different manufacture.
An integral part of the software package is an advanced automatic calibration procedure which allows complete set-up and dynamic readjustment of the microscope column, motorized stage, backscattered electron detector (BSD), and X-ray analysis system without the need for operator intervention. The system is designed to operate successfully using either the Robinson scintillator or solid-state backscattered electron detectors.

If the intensity of the electron beam varies during a run, GSR particles may no longer fall within the pre-selected threshold level. To cope with this contingency, a calibration is performed between samples. This is also helpful during long runs to guarantee reliability of long-run analysis. Because of height differences between samples, autofocus can be applied for each stub or even for each field. Through calibration, the SEM column as well as the BSD can be dynamically adjusted to yield reproducible results.

 

Set-up and Calibration
X-ray excitation conditions (beam electron intensity measured in terms of X-ray counts per second) are calibrated first, using a standard to ensure reproducible results. Before a run starts, the SEM column parameters (kV, spot size, etc) are automatically adjusted. After each sample stub is completed, the stage can relocate to the standard and perform a new calibration. Following X-ray count-rate adjustment, the background detector is calibrated with relation to Z (atomic number), using the calibration standard delivered with the system. The purpose of this is to search for particles based on the average Z, and not to rely on their video intensity as in most other systems. This is a key feature of the GSR software. Particles are detected based on their average atomic number falling within a user-defined Z-window. The SEM motorized stage is automatically driven to each standard, and the video levels are measured without changing any column conditions. The BSD response curve is then used to set upper and lower threshold criteria for particle detection by the BSD, based on the average atomic number. This serves as input for the preliminary search on particles in the automatic routine. The calibration process may be performed unattended during the course of a run in cases where the SEM gun is unstable.



GSR Calibration Stub.

 



Substage layout page to store the 16 sample positions (regular mode).

Analysis
The calibration procedure is one of the key functions of the GSR-NT software. After calibration of the SEM system, batches of GSR samples are configured to begin a run.

Samples can be arranged on the stage in a regular array, or in an irregular array of up to 16 samples. In both cases, the operator can use the pre-defined substage layout. This allows fast and accurate recording of the sample positions without moving the stage.

 

 



Sample configuration set-up page.

Information such as sample size, search area, sample array, number of samples, minimum size of search particles, and percentage of stubs to be analyzed are defined. Search "stop" criteria and "run-time" options such as maximum number of particles per sample and "pause" are available.

 

A typical GSR run requirement is to search for particles 0.5 microns or greater in size over the 100 mm² surface of a taping. The GSR software optimizes the search by calculating the search magnification based on the minimum particle size sought. For a search of 100 mm², an array of 130 fields is needed, using a typical magnification of 120x, with a confidence level of 2x2 pixels per particle.

"A confidence level of 2x2 pixels per particle" means that in order for a group of bright neighboring particles to be classified as a particle, there must be at least two neighboring bright pixels in the X and two in the Y direction. In order to search at as low a magnification as possible, there is the option of defining a particle as one pixel (typical magnification is 60x for 0.5 micron particles or 30x for 1.0 micron particles). The latter results in a search of only 9 fields for 100 mm² taping. Using the fast scan on the SEM, the empty fields can be searched in as little as 60 minutes for a 10 mm x 10 mm field, giving a fourfold improvement over the generic scan rate. Operating at one pixel per particle as a minimum particle-definition criterion will yield the faster scan, but may not be as reliable if there are very small GSR particles present. It can, however, be used as the first fast indication of the suspect sample.

 



Classification scheme for fixed and user definable classes.

Classification
The position and size of the candidate particles is recorded automatically. A revisit by the electron beam is used to analyze the particle. The emitted X-ray spectrum of each particle is classified using the choice of either Regions of Interest (ROI) or Spectrum Stripping spectrum analysis (STRIP) classification schemes.

The ROI classification scheme uses ratios of ROI counts data to determine the elements present in the spectrum. The ROI scheme classifies each spectrum into one of 35 categories in accordance with the Metropolitan Police GSR classification scheme. It is possible to select different classes or configure the selected classes. Up to 35 user-definable classes can be defined for each run. Saving the settings as different configuration files can increase the number of definable classes.

 

 
The STRIP classification scheme performs full background subtraction and iterative peak stripping to derive intensity data for the elements present in the spectrum. This classification scheme allows classes to be constructed, by the user, according to tight or wide chemical criteria, so that both fixed stoichiometric compounds can be identified, as well as continuous-composition phases typical of GSR particles.

After a run, particles can be revisited and reanalyzed using a new, perhaps longer, acquisition-time spectrum, and then reclassified. The reclassified data are merged with the original data but preserving the original classification. In addition, whole runs can be reclassified automatically should the user decide to change or add a class definition to the classification scheme.

 

Reporting
Once the run has started, critical data on each detected particle are stored in spreadsheet format to yield a complete results file. This file can be reviewed, particle by particle, directly after the run has been completed or at a later date. A single-page, easy-to-read report is automatically generated by the GSR software after each sample has been analyzed.
 



Stub particle map to show all detected particles per sample.

A complete GSR Parameter List or Stub Particle Map can also be printed.
The Stub Particle Map shows an overview of all detected particles, classified by type. Using the special GSR Spectra Utility software, all detected and classified particles can be investigated and printed in a handy format, together with particle data. This fast spectra-viewing utility helps to save time reviewing the many individual spectra generated during the unattended run. Fast single page report generation is possible, including an image of the particle, its spectrum and text.

 

The ROI classification scheme uses ratios of ROI counts data to determine the elements present in the spectrum. The ROI scheme classifies each spectrum into one of 35 categories in accordance with the Metropolitan Police GSR classification scheme. It is possible to select different classes or configure the selected classes. Up to 35 user-definable classes can be defined for each run. Saving the settings as different configuration files can increase the number of definable classes.



GSR Spectra Utility for fast investigation of the
stored spectra.

 
Relocation
Relocation and reconfirmation of class is often required. Particles can be revisited easily for further imaging and verification by a simple double click on the particle number. The high-precision motorized stage of a motorized SEM will center and zoom the particle automatically. In this way each particle will be easily relocated. The GSR analysis can be started within the GSR application to acquire a spectrum over longer time, which can be saved on disc and used in the final report. The accuracy of the relocation is very important because of the small size of many GSR particles (approximately 0.5 - 2 microns).
After relocation, the analysis for confirmation is made at a magnification of about 2000 - 5000x. The motorized stage of the SEM in a busy crime lab will make a few million movements per year. A high-precision motorized stage is, therefore, a must. The ability to search automatically at a low magnification is a standard procedure included in the GSR software program. This will help to reduce the number of stage movements and reduce SEM maintenance costs.
 



Easy relocation of a particle is included in the GRS-NT software.

 
Please note this GSR software may not achieve full specifications on all models of SEM. For further information on specific SEMs, or details on the GSR software, please contact Eastern Analytical, EDAX, FEI or your SEM supplier.
eastern.analytical@gunshotresidue.com