A P P L I C AT I O N N O T E

Fully Automated Gunshot Residue Analysis

For Quanta series SEM

Any sample, all data

When a gun is fired, small particles are generated The elements constituting GSR can originate from the
during the explosion of the gunpowder. The particles, primer, the bullet, a coating or jacket on the bullet,
referred to as gunshot residue (GSR), exit the gun cartridge components, and previous residues in the
backwards and are deposited on the hand and clothes barrel. Residue particles are arbitrarily divided into two
of the person firing the gun. Because GSR particles have types, depending on their primary source: primer
distinctive characteristics, their presence contributes particles and bullet particles. Particles containing Pb,
evidence that suspect persons have been close to Ba and Sb, and those containing Ba and Sb (also referred
a gun being fired. This kind of evidence is often used to as three- and two-component particles) are typical
in criminal cases involving the use of firearms. inorganic components from the primer and are
classified as primer particles (Figure 2). Large numbers
GSR contains elements that result from the propellant of particles composed mainly of Pb originate from the
and primer decomposing, as well as from the bullet and bullet and are termed bullet particles.
cartridge case. Samples of GSR are taken by pressing
adhesive material to areas of interest, such as the
fingers, the top part of the hand and the clothes, to
remove any particles. The particles are transferred from
the area of interest onto a small sample for examination
in a scanning electron microscope (SEM) linked to an
X-ray micro-analytical system equipped with a GSR
software package. This software package allows
automated, unattended classification of GSR particles
(Figure 1).

Finding 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 0.5-10µm. In a scanning
electron microscope, these particles can be found,
magnified and analysed chemically, and the presence
of GSR on a sample confirmed.
Figure 1. Graphical User interface of the GSR software, showing the
results of a typical GSR run. All data is available within one field.
The microscope control page is on the right..
 A P P L I C AT I O N N O T E

In normal GSR suspect tapings, the particles on the

adhesive tape are typically <10µm in size (usually
0.5-2µm) and are relatively few divided over a fairly
large area. Earlier studies(1) have been shown that the
majority of the GSR particles have a small diameter
(<2µm). As a consequence, large surfaces have to be
analysed in order to yield results of sufficient statistical
validity.

For this reason, interactive location and analysis of GSR

by the SEM operator is impractical. The task is tedious
and very time-consuming, and the risk of introducing
errors is high. However, an automatic routine has been
Figure 2. Typical Pb, Ba, Sb particle
developed that allows unattended analysis, followed by
operator-assisted validation and summarising of results.

The automatic routine

The analysis of GSR by dedicated software ensures
reliable, fast and fully unattended analysis. The software
also identifies other indicative particles similar to those
originating from the bullet and containing a large
amount of Lead (Pb). Other particles of interest can be
Titanium (Ti) and Zinc (Zn), as found in lead-free
ammunition. Environment-related particles can also
provide additional information about the suspect.

Performing an analysis
The steps involved in performing 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 atomic number
Z-window back-scattered electron imaging (BSEI)
• The position and size of the candidate particles are
recorded
• The particles are revisited by the electron beam to
perform an X-ray analysis
• The emitted X-ray spectrum from each individual
particle is compared to a classification scheme
Figure 3. BSD image at low magnification, used to separate and
locate particles.
• All results are stored (on disk)
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 and by applying a threshold to the
signal the particles are distinguished and located by the
software (figure 3). After system calibration, up to 20
samples can be analysed.

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Software description
The dedicated GSR analysis package is a fully embedded
software package for the analytical FEI Quanta series of
scanning electron microscopes. The system makes
optimum use of the Quanta stage and beam
possibilities. An integral part of the package is an
advanced, automatic calibration procedure, which
allows complete set-up and dynamic readjustment of
the microscope column, motorised stage, backscattered
electron detector and X-ray analysis system without
the need for operator intervention.
If the intensity of the electron beam varies during a
run, GSR particles may no longer fall within the pre
selected threshold level. In order to prevent that the
search criteria would no longer be met it has been
made possible to perform a calibration in between
each sample. This is very helpful during long runs to
guarantee reliability of long run analysis. Through
calibration, the SEM column as well as the BSED can
be dynamically adjusted to yield reproducible results.
Because samples taken from the suspect are often not
completely flat, the system supports full z-movement.
The operator can choose between using the traditional
focusing method on the sample (mostly used for very
flat samples), including the possibility of using auto-
focus or the z-movement. The software reads the
z position (optimum X-rays around 10 mm) of all
individual samples and during the automated run it will
bring the specimen in focus by using stage movement.
Using the z-movement will speed up the analysis
enormously, because the use of autofocus adds a certain
amount of time to the overall analysis time.
Set-up and Calibration.
X-ray excitation conditions (counts per second) are
calibrated first, using a standard to ensure reproducible
results. Before a run is started, the SEM column
parameters (kV, spot size, etc.) are automatically
adjusted. After each sample stub is completed, the
stage can return to the standard and perform a new
calibration.
A P P L I C AT I O N N O T E
Following X-ray count rate adjustment, the
backscattered detector is calibrated in 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 only
rely on their video intensity, as in most other systems.
This is a key feature, because GSR particles tend
intrinsically to have high average Z, so searching for
‘bright particles only’ is eliminated. Particles are
detected on the basis of their average atomic number
falling within a user-defined Z-window.
The FEI Quanta SEM motorized stage is automatically
driven to each standard and the video levels are
measured without changing any column conditions.
The BSED response curve is then used to set upper and
lower threshold criteria for particle detection by the
BSED, based on the average atomic number. This serves
as input for the preliminary search on particles in the
automatic routine.
Because samples taken from a suspect are often not
completely flat, the height between samples may vary.
The system therefore supports full z movement. The
operator can choose between the traditional method
of focusing on the sample, including using auto-focus
(mostly used for very flat samples), or z-movement.
The software reads the z position (optimum X-rays
around 10mm) of all samples and, during the
automated run, brings the specimen into focus using
stage movement, instead of lens focussing.
The calibration procedure is one of the key functions
of the software.
Analysis.
After calibration of the Quanta SEM-EDX system, GSR
sample batches are configured to begin a run. Samples
are arranged on the stage in a regular array, or in an
irregular array of up to 20 samples. In both cases, the
pre-defined substage layout can be used. This allows
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 A P P L I C AT I O N N O T E

Figure 4. Substage layout page to store the 20 sample positions.. Figure 5. Sample configuration se- up page.

fast and accurate recording of the sample positions speed of the automatic analysis depending on how
without moving the stage (Figure 4). much of the sample can be captured in a single frame.
Information such as sample size, search area, sample
array, number of samples, minimum size of searched The following ‘no-find’ time can be quoted:
particles, and percentage of stub to be analysed, are
defined. Search “stop” criteria and “run-time” options Surface area = 100 mm2
such as maximum number of particles per sample and Search criteria = 0.5 micron particle (1 pixel)
‘pause’ are available (Figure 5). Magnification = 63x
No. of fields = 30
GSR Analysis Throughput Specification Time = 25 minutes
The throughput of GSR software solutions can be
described by the number of detected and measured Surface area = 100 mm2
(classified by EDX) particles per unit of time. However, Search criteria = 0.5 micron particle (2 pixels)
particle density typically is very low and the throughput Magnification = 130x
of GSR solutions is typically expressed as ‘no found’ No. of fields = 130
time, i.e. the time needed to scan empty fields (without Time = 100 minutes
finding particles). “No found” time critically depends on
search criteria. The search criteria include minimum On real-life samples, the GSR sw will measure 10 – 20
particle size (diameter) and the minimum number of particles per minute. This includes scanning of the field,
pixels per particle. These criteria will determine the detecting the particles, measuring and classifying of the
search magnification and therefore will influence the particles and moving the stage to the next field.

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 A P P L I C AT I O N N O T E

Classification.
The position and size of the candidate particles is
recorded automatically and a revisit of the electron
beam is used to analyse the particle. The emitted X-ray
spectrum of each individual particle is recorded and
compared to a classification scheme. The software is
equipped with a spectrum stripping routine, which will
result in a more accurate classification in case of severe
overlap between elements eg, Sb and Ca and/or Sn).
It is possible to create your own classes or configure the
selected class with a maximum of 8 elements. User-
definable classes can include quantification thresholds.
Stop criteria can be set for each class. Up to 4000 user
definable classes can be defined for each run (Figure 6). Figure 6. User definable classification scheme to set up the
individual classes.
A set of classes can be saved in order to create multiple
classes for multiple disciplines.

Automatic reclassification of the complete data set

without performing a real re-run is also possible. New
classes can be added, or existing ones can be changed
according to match the found spectra. After the start
of the run, it takes several minutes before all data are
recalculated. A new result file is stored. And the original
data set will not be overwritten

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
Figure 7. GSR Stub Particle Map to show the specific classified
by particle, directly after the run has been completed or particles on the stub.
at a later date. A single page, easy to read report is
automatically generated after each sample has been
analysed. A complete GSR Parameter List or Stub Particle
Map can also be printed. The Stub Particle Map will
show an overview of all detected particles, classified by
type (Figure 7).

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 A P P L I C AT I O N N O T E

The GSR spectrum utility is used to investigate all

detected, classified or reclassified particles and print the
results in a handy format, including particle data. This
fast spectrum-viewing utility helps to save time
reviewing the many individual spectra generated during
an unattended run (Figure 8). Fast single-page report
generation is possible, and can include the image of the
particle, its spectrum and text.

Relocation.
Relocation and reclassification are often required.
Particles can be revisited easily for further imaging and
verification by simple double-click on the particle
number. The high precision motorised stage of the FEI Figure 8. GSR Spectra Utility for fast investigation of the multiple
stored spectra
Quanta SEM will center and zoom the particle
automatically to be relocated very easily (Figure 9).
The EDX analysis can be started and reclassification
carried out using the default GSR condition.
Alternatively, the EDX analysis can be started within
the GSR application to acquire a spectrum over longer
time and save it to disk for use in the final report
(Figures 10 and 11).

The accuracy of the relocation is very important because

of the small size of many GSR particles (approximately
0.5 - 2 micron). After relocation, the analysis for
confirmation is made at a magnification of 1000x.
Automatic analysis and certain relocation demand
a low scan hysteresis and a motorised stage that is not Figure 9. Revisiting an individual particle is very easy. The system
susceptible to wear. Low scan hysteresis is important will automatically move to and center the particle.

because the electron beam will be brought back to the

particle for verification. If still some magnetism is left
in the scan coils, the beam will simply miss the particle.
The motorised stage of the SEM in a busy crime lab will
make a few million movements on yearly base. A high
precision motorised stage is therefore a must. Searching
at low magnification will only help to reduce the
number of stage movements. FEI’s Quanta series SEMs
fulfill these typical forensic requirements.

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Figure 10. After the particle has been centered, an image is creat-
ed automatically and manual classification of the particle is possi-
ble. Easy report generation can also be done from this location.
Figure 11. After manual spectrum acquisition the spectrum can be
classified. A quantitative analysis is performed on the spectrum.
A P P L I C AT I O N N O T E
Sample holders
A dedicated holder for 8 and 20 stubs is available,
designed for ease of use. The base-plate of the holder
will stay in the SEM and the top part of the holder can
be removed for easy loading and unloading. Multiple
sample holders are available, therefore one can store,
temporarily, several cases.
GSR standalone software (GSR emulator)
The GSR software is also available as a standalone
program. This software module runs on every
standalone PC (under Windows 2000). Reclassification
therefore can be done easily off-line, leaving the SEM
free to start a new run. The new emulator program
holds the same features as the embedded GSR software.
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A P P L I C AT I O N N O T E

Forensic SEM
The FEI Quanta SEM offers, beside conventional
imaging under high vacuum conditions using the
traditional SE detector, the possibility to image the
specimen surface in a gaseous environment at chamber
pressures in the range of 0.1 to 1.3 mbar (130 Pa) by
employing backscatter detection (as needed for GSR)
for elemental contrast or the dedicated GSED (Gaseous
Secondary Electron Detector) for topographic contrast.
The presence of the gas inside the chamber is two fold:
it will eliminate the charging effects of the uncoated
sample and the gas is used for imaging by use of
dedicated detectors (Figure 12).
Figure 12. Forensic SEM

The Quanta, operating in the “low vacuum” range is

Key benefits
the ideal scanning electron microscope for all forensic
investigations. This type of SEM is very suitable for
• Fast automatic searching and characterising particles
imaging non-conducting materials without preparation.
• Minimum detectable particle size 0.3 micron
For many materials such as plastics, polymers, glass,
• Automatic optimisation of SEM
wood, paints, fibres, hairs, fingerprints, insects, etc., the
• Automatic calibration of the BSED
Quanta allows these types of specimen to be viewed in
• Automated multi-field run
the natural uncoated state with the possibility of
• Pre defined substage layout
performing microanalysis.
• Up to 20 samples in one run
• Fast and accurate re-visiting possibilities
Using GSR at low vacuum conditions offers a tremendous
• Fast report generation
benefit for samples that do not allow any conductive
• User definable classes
coating, thus no destruction of the evidence will occur.
• Results fully compatible with MS Excel format

The choice between different chamber atmosphere

conditions makes the Quanta the perfect solution for a
References
wide variety of applications.
1. M.H. Peeters, J. Antoine, V. Lamothe, A. Viala.
Automation of gunshot-residue analysis by functional
integration of a scanning electron microscope and an
energy dispersive microanalysis system.
Microbeam Analysis, 1990, 369 - 371.

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