Is there a real danger of concealing gunshot residue (GSR) particles by skin debris using the tape-lift method for sampling GSR from hands?

Experiments were carried out to assess the danger of concealing GSR particles by skin debris using the tape-lift method for sampling GSR from hands. Thirty discrete spherical particles (from GSR and from the debris of oxygen cutting of steel) sized from 8 to 30 microns were mounted on a double-side adhesive coated stubs in known locations using a stereomicroscope. These stubs were then used for dabbing hands 50 times. Some of the particles or parts thereof were covered by skin flakes, however, all particles could be detected using the backscattered electron image (BEI) in the scanning electron microscope (SEM). Also, all could be identified by the energy dispersive X-ray spectroscopy (EDX).     

Preparation of a Ytterbium‐tagged Gunshot Residue Standard for Quality Control in the Forensic Analysis of GSR

Preparation of a ytterbium‐tagged gunshot residue (GSR) reference standard for scanning electron microscopy and energy dispersive X‐ray spectroscopic (SEM‐EDS) microanalysis is reported. Two different chemical markers, ytterbium and neodymium, were evaluated by spiking the primers of 38 Special ammunition cartridges (no propellant, no projectile) and discharging them onto 12.7 mm diameter aluminum SEM pin stubs. Following SEM‐EDS microanalysis, the majority of tri‐component particles containing lead, barium, and antimony (PbBaSb) were successfully tagged with the chemical marker. Results demonstrate a primer spiked with 0.75% weight percent of ytterbium nitrate affords PbBaSb particles characteristic of GSR with a ytterbium inclusion efficiency of between 77% and 100%. Reproducibility of the method was verified, and durability of the ytterbium‐tagged tri‐component particles under repeated SEM‐EDS analysis was also tested. The ytterbium‐tagged PbBaSb particles impart synthetic traceability to a GSR reference standard and are suitable for analysis alongside case work samples, as a positive control for quality assurance purposes.     

Image analysis of gunshot residue on entry wounds: I – The technique and preliminary study

An automated image analysis (IA) technique has been developed to obtain a measure of the amount (i.e. number and area) of gunshot residue (GSR) particles within and around a gunshot wound. Sample preparation and IA procedures were standardised to improve the reproducibility of the IA measurements of GSR. Measurements of GSR from test firings into goat hide were enhanced by staining the barium and lead components present on the skin sections with Alizarin Red S. The amount of GSR detected on the stained skin sections was compared with backscatter electron micrographs of the same sections. The differences were deemed to be insignificant when the variability in the repeated test firings were taken into consideration. Preliminary results indicated that the decreasing relationship between firing range and the amount of GSR deposited was non-linear, and that for firing ranges of up to 20 cm the amount of GSR deposited from repeated shots fired from the same distance was highly variable.     

A simple method for detection of gunshot residue particles from hands, hair, face, and clothing using scanning electron microscopy/wavelength dispersive X-ray (SEM/WDX).

We devised a simple and rapid method for detection of gunshot residue (GSR) particles, using scanning electron microscopy/wavelength dispersive X-ray (SEM/WDX) analysis. Experiments were done on samples containing GSR particles obtained from hands, hair, face, and clothing, using double-sided adhesive coated aluminum stubs (tape-lift method). SEM/WDX analyses for GSR were carried out in three steps: the first step was map analysis for barium (Ba) to search for GSR particles from lead styphnate primed ammunition, or tin (Sn) to search for GSR particles from mercury fulminate primed ammunition. The second step was determination of the location of GSR particles by X-ray imaging of Ba or Sn at a magnification of x 1000-2000 in the SEM, using data of map analysis, and the third step was identification of GSR particles, using WDX spectrometers. Analysis of samples from each primer of a stub took about 3 h. Practical applications were shown for utility of this method.     

Detecting Gunshot Residue from Sellier & Bellot Nontox Heavy Metal‐free Primer by in situ Cathodoluminescence

Gunshot residue (GSR) from the discharge of ammunition can provide crucial information in reconstructing criminal cases. Traditional primers create particles of heavy metals such as lead, barium, and antimony. In forensic laboratories, automatic inorganic particle detection is performed by scanning electron microscopy (SEM), using the backscattered electron signal to search for bright residues among the many darker environmental particles, due to higher electron density of the former. Some innovative primers, indicated as heavy metal‐free (HMF), produce a residue of elements with atomic numbers below 21, urgently demanding new detecting solutions. For the first time, residues from Sellier & Bellot Nontox HMF primer are demonstrated to emit visible light under electron beam stimulation in a SEM. Cathodoluminescence is then proposed as a promising tool to both detect and characterize residues in forensic cases involving HMF primers, with minor changes to traditional analytical apparatus used for inorganic GSR analysis.     

GSR2005—Continuity of the ENFSI Proficiency Test on Identification of GSR by SEM/EDX

Abstract:  Within the framework of the ENFSI Expert Working Group "Firearms" a proficiency test on the detection and identification of GSR by energy-dispersive scanning electron microanalysis (SEM/EDX) is carried out in a 2 years term. The latest test was performed in 2005/2006 and was denoted as GSR2005 . Seventy-five laboratories from 28 countries participated in this proficiency test and submitted in total 83 independent data-sets. The participating laboratories were requested to determine the total number of PbSbBa containing particles on a synthetic test sample following their own laboratory specific methods of automated GSR particle search and detection by SEM/EDX. Furthermore size and position of the detected particles had to be reported by the laboratories and were evaluated statistically. The results were compiled by means of z -scores according to the IUPAC and EURACHEM guidelines—assessing individual laboratory achievements (inter-laboratory) as well as intra-laboratory performance—and were compared to the results of the previous proficiency test run GSR2003 ( 1 ). The comparison shows that there is a noticeable improvement in the method's detection capability.     

Automated SEM/EDS Analysis of Airbag Residue. II: Airbag Residue as a Source of Percussion Primer Residue Particles

Abstract:  Automated scanning electron microscopy with energy dispersive spectroscopy has been used to analyze airbag residue particles. Analysis of airbag residue from some passenger side airbags revealed some residue particles which are consistent with gunshot residue (GSR) samples. The source of these particles was determined to be percussion primers used to initiate the chemical reaction for deployment. This article identifies some vehicles which contain this type of airbag and demonstrates the types of particles which could be misidentified as being GSR. The low numbers of GSR particles in among the large particle populations of zirconium and/or copper–cobalt particles, which are clearly airbag residue, allow the trained analysts to distinguish the correct source of this residue. Particles containing high aluminum levels, elevated levels of allowable elements in GSR particles, or the presence of elements that are rare in GSR particles stand out as indications that the particles are not GSR in origin. This study serves as a guide to analysts who perform particle analysis in forensic investigations.     

Image analysis of gunshot residue on entry wounds. I--The technique and preliminary study.

An automated image analysis (IA) technique has been developed to obtain a measure of the amount (i.e. number and area) of gunshot residue (GSR) particles within and around a gunshot wound. Sample preparation and IA procedures were standardised to improve the reproducibility of the IA measurements of GSR. Measurements of GSR from test firings into goat hide were enhanced by staining the barium and lead components present on the skin sections with Alizarin Red S. The amount of GSR detected on the stained skin sections was compared with backscatter electron micrographs of the same sections. The differences were deemed to be insignificant when the variability in the repeated test firings were taken into consideration. Preliminary results indicated that the decreasing relationship between firing range and the amount of GSR deposited was non-linear, and that for firing ranges of up to 20 cm the amount of GSR deposited from repeated shots fired from the same distance was highly variable.     

Image analysis of gunshot residue on entry wounds: II – A statistical estimation of firing range

A statistical investigation of the relationship between firing range and the amount and distribution of gunshot residue (GSR), used automated image analysis (IA) to quantify GSR deposit resulting from firings into pig skin, from distances ranging between contact and 45 cm. Overall, for a Ruger .22 semi-automatic rifle using CCI solid point, high velocity ammunition, the total area of GSR deposit on the skin sections decreased in a non-linear fashion with firing range. More specifically there were significant differences in the amount of GSR deposited from shots fired at contact compared with shots fired from distances between 2.5 and 45 cm; and between shots fired from a distance of 20 cm or less, with shots fired at a distance of 30 cm or more. In addition, GSR particles were heavily concentrated in the wound tract only for contact and close range shots at 2.5 cm, while the particle distribution was more uniform between the wound tract and the skin surfaces for shots fired from distances greater than 2.5 cm. Consequently, for future scientific investigations of gunshot fatalities, once standards have been established for the weapon and ammunition type in question, image analysis quantification of GSR deposited in and around the gunshot wound may be capable of providing a reliable, statistical basis for estimating firing range.     

Distribution of GSR particles in the surroundings of shooting pistol

Several series of experiments were performed to study the distribution of GSR particles in seven directions in the surroundings of shooting firearm (pistol CZ 85 caliber 9 mm Luger). External and internal conditions and two different primer types were used for the shooting experiments. The results showed that maximum number of GSR particles could be found in the right front quadrant at a distance of 2–4 m with respect to the shooting firearm position and shooting direction. GSR particles were even found in distance 10 m from shooting firearm. A significant influence of climatic conditions on GSR distribution was confirmed.     

Image analysis of gunshot residue on entry wounds. II--A statistical estimation of firing range.

A statistical investigation of the relationship between firing range and the amount and distribution of gunshot residue (GSR), used automated image analysis (IA) to quantify GSR deposit resulting from firings into pig skin, from distances ranging between contact and 45 cm. Overall, for a Ruger .22 semi-automatic rifle using CCI solid point, high velocity ammunition, the total area of GSR deposit on the skin sections decreased in a non-linear fashion with firing range. More specifically there were significant differences in the amount of GSR deposited from shots fired at contact compared with shots fired from distances between 2.5 and 45 cm; and between shots fired from a distance of 20 cm or less, with shots fired at a distance of 30 cm or more. In addition, GSR particles were heavily concentrated in the wound tract only for contact and close range shots at 2.5 cm, while the particle distribution was more uniform between the wound tract and the skin surfaces for shots fired from distances greater than 2.5 cm. Consequently, for future scientific investigations of gunshot fatalities, once standards have been established for the weapon and ammunition type in question, image analysis quantification of GSR deposited in and around the gunshot wound may be capable of providing a reliable, statistical basis for estimating firing range.     

Gunshot residue in Chicago police vehicles and facilities: an empirical study

Suspects in shooting investigations in Chicago are routinely transported in department vehicles and detained in department facilities prior to gunshot residue (GSR) evidence collection. The GSR test results are used to associate the suspect with primary exposure to GSR. The potential for these vehicles and facilities being sources of secondary GSR contamination needed to be determined. A total of 201 samples were collected from randomly selected vehicles and detention facilities. The sampling collected trace materials from surfaces that suspects' hands may contact during the arrest process. These samples were examined for the presence of GSR particles using scanning electron microscopy. Upon completion of the automated analysis, those particles that met an initial GSR screening criterion were relocated and reanalyzed. The locations where GSR particles were recovered allowed us to make recommendations to the Chicago Police Department with regard to transporting and detaining these suspects. The low number of GSR particles recovered suggests that the potential for secondary contamination, although present, is relatively low.     

GSR2005--continuity of the ENFSI proficiency test on identification of GSR by SEM/EDX.

Within the framework of the ENFSI Expert Working Group "Firearms" a proficiency test on the detection and identification of GSR by energy-dispersive scanning electron microanalysis (SEM/EDX) is carried out in a 2 years term. The latest test was performed in 2005/2006 and was denoted as GSR2005. Seventy-five laboratories from 28 countries participated in this proficiency test and submitted in total 83 independent data-sets. The participating laboratories were requested to determine the total number of PbSbBa containing particles on a synthetic test sample following their own laboratory specific methods of automated GSR particle search and detection by SEM/EDX. Furthermore size and position of the detected particles had to be reported by the laboratories and were evaluated statistically. The results were compiled by means of z-scores according to the IUPAC and EURACHEM guidelines-assessing individual laboratory achievements (inter-laboratory) as well as intra-laboratory performance-and were compared to the results of the previous proficiency test run GSR2003 (1). The comparison shows that there is a noticeable improvement in the method's detection capability.     

A Study of Background Levels of Antimony,Barium, and Lead on Vehicle Surface Samples by Graphite Furnace Atomic Absorption

Law enforcement agencies routinely sample for gunshot residue (GSR) by bulk techniques and often submit swabs taken from other surfaces besides the hands of the suspect shooter. This study aims to establish the prevalence of antimony, barium, and lead on normally handled automobile surfaces by graphite furnace atomic absorption analysis. No positives were determined on 50 sampled automobile surfaces above cutoff (positive) from background levels. Transfers of GSR particles from shooter hands to automobile surfaces were found to potentially allow for positive GSR determinations, but such transfers seem to be dependent on the shooting conditions and length of GSR exposure. We determined that our bulk analysis method yields an overall 87.94 ± 5.52% extraction efficiency from cotton swabs, while the LOQ determinations strengthening the fact that bulk analysis methods are valid and valuable tools for GSR investigations.     

Characterisation of 0.22 caliber rimfire gunshot residues by time-of-flight secondary ion mass spectrometry (TOF-SIMS): a preliminary study

The application of time-of-flight secondary ion mass spectrometry (TOF-SIMS) for the characterisation of gunshot residue (GSR) from 0.22 caliber rimfire ammunition is reported. Results obtained by TOF-SIMS were compared with conventional scanning electron microscopy (SEM) studies. As could be expected, TOF-SIMS exhibited greater elemental sensitivity than SEM equipped with energy dispersive X-ray detection (SEM-EDX), and was also capable of detecting fragments characteristic of inorganic compounds. This preliminary study indicates that TOF-SIMS offers substantial potential for forensic GSR examinations as a complementary technique to SEM-EDX. In addition TOF-SIMS is applicable to the analysis of individual particles in the typical size range encountered in GSR casework.     

Automated gunshot residue particle search and characterization

The main disadvantage to gunshot residue (GSR) particle analysis utilizing scanning electron microscope/energy dispersive X-ray (SEM/EDX) instrumentation has been the excessive operator time required for search and identification. This study uses an automated particle search and characterization program for unattended GSR search and identification. This system allows for automatic matrix search, particle sizing, chemical typing, and spectral aquisition with subsequent storage of data to disk for later operator review and verification. This work describes various aspects of the program, determines appropriate parameters adequate for both unique and characteristic GSR particle identification, and evaluates the reliability of data obtained. Samples are collected via the tape lift method from test-firings of .38, .32, .25, and .22 caliber handguns at time after firing intervals of 0 to 6 h. Unique GSR particles are consistently and correctly identified by this method on tape lift samples taken up to 4 h after firing. False positive results of unique GSR particles are not encountered on control handblank samples. This technique appears to provide the forensic science community with an operator-free method of reliable GSR particle search and an improved analyst-time-per-case ratio.     

A study of dispersion of gunshot residue from a frequently used Serbian ammunition cal. 7.65 mm to support selected aspects of casework in North Macedonia

The subject of this research was the inorganic gunshot residue component collected from shooting patterns obtained on woven cotton cloth using a Pietro Beretta model 70 pistol, cal. 7.65 mm and Serbian ammunition for the following muzzle-to-target distances: 25, 50, 75, 100 and 125 cm. For each distance, three rounds of shooting were performed. Particles were lifted within a 10 cm radius of the projectile entrance and automatically analyzed using a scanning electron microscope coupled with an energy dispersion X-ray spectrometry. The obtained data on the populations of particles were analyzed taking into account their numbers, chemical classes and sizes. The results showed an apparent maximum incidence within all particles containing barium at about 50 cm distance. Also, lead particles revealed a distinct behaviour, being dominant at a 25 cm distance, falling below the other chemical classes, and finally becoming dominant again at 125 cm. The analysis of the frequency of occurrence of particles sorted according to their sizes confirmed that the small particle population is the largest, and their distribution in function of the equivalent circle diameter is exponential-like. The obtained results provided knowledge on the distribution of particles in the vicinity of the tested firearm and ammunition cal. 7.65 mm which generally corroborates with similarly studied GSR distributions obtained for the use of pistols cal. 9 mm. This information, together with the examinations of gunshot damages and other types of residues such as soot or unburned propellant grains may support qualitative inferences on shooting distance estimation, especially in cases, when the firearm and cartridges are not available to perform test shooting. In such cases even roughly estimated shooting distance can be helpful, e.g. for confirming or excluding the possibility of self-inflicted injuries or suicide and infer on the mutual position of the shooting stage actors. An example of casework that illustrates intermediate shooting distance estimation is presented.     

电流斑的光镜和扫描电镜观察以及能谱测定

为了找出电流斑在扫描电镜下的特征性改变,作者用扫描电镜和能谱测定,配合光镜观察,对电击死者的22个皮肤电流斑和尸体上造成的18个皮肤电流斑和金属灼伤,进行了对比观察。结果表明,光镜下电流斑的形态改变与过去学者所述基本一致。非典型的电流斑难与热灼伤相鉴别。扫描电镜下电流斑的形态特征为:(1)损伤底部和壁上可见散在的小孔穴,直径为30～100μm,深浅不一,边缘不规则;(2)损伤组织表面大量细胞碎屑和颗粒;(3)组织和脱落细胞表面有裂纹;(4)损伤区内有散在的异物颗粒沉积,其形态为球形、方形或不规则形,电子密度较大。作者认为这些改变是电流作用造成,热灼伤不具备这些改变,故在扫描电镜下极易区别电流斑和热灼伤。所有电流斑均可测出与导体化学组成相同的金属元素。作者提出,扫描电镜下的上述形态改变和能谱测定结果可以作为诊断电流斑的依据。     

Maintenance of the ENFSI proficiency test program on identification of GSR by SEM/EDX (GSR2003)

Within the framework of the ENFSI Expert Working Group "Firearms," every second year, a proficiency test on the detection and identification of GSR by SEM/EDX is carried out. This proficiency test is a development and extension of the previous proficiency test GSR2001. The test material was again designed by the organization panel and manufactured by an external company for SEM accessories. This time the participating laboratories were requested to determine the total number of PbSbBa containing particles on a test sample following their own laboratory specific methods of automated GSR particle search and detection by SEM/EDX. One synthetic particle sample (SPS) with artificial GSR particles was dispatched to all participants. This paper summarizes the results of the study and assesses the overall performance of the participating laboratories. Furthermore an extended statistical evaluation and a comparison with previous studies was carried out.