Bone Mineral Change During Experimental Calcination: An X‐ray Diffraction Study

The effects of calcination (400–1200°C) on pig bones have been studied using powder X‐ray diffraction (XRD) and secondary modifications, such as color change and weight loss. The characterisation by powder XRD confirmed the presence of the crystalline phase of hydroxyapatite, and comparison of the results obtained at different temperatures suggested that at 650°C, all the organic components and carbonate substitutions were completely removed. Accordingly, these samples were white. In addition, the crystallinity degree and the crystallite size progressively increased with the calcination temperature until 650°C, remaining stable until 1200°C. Below 650°C, bone samples presented organic compounds, resulting in background noise in the diffractogram and gray or black color. In addition, impurities in the lattice correspond to low crystallite sizes.     

X‐ray Powder Diffraction for Characterization of Raw Materials in Banknotes

We report about the X‐ray powder diffraction characterization of crystalline materials used to produce genuine and counterfeit banknotes, performed with a single‐crystal diffractometer that permits fast and nondestructive measurements in different 0.5‐mm sized areas; 20‐euro denomination genuine banknotes were analyzed, and results were compared with counterfeit banknotes. The analysis shows that the papers used to print real banknotes are composed, as expected, of cotton‐based cellulose and titanium dioxide as crystalline additive, but different polymorphs of TiO₂ for different emission countries are evidenced. The counterfeit banknotes are composed of cellulose based on wood pulp; moreover, an unexpected significant quantity of TiO₂ was found to be mixed with calcite, indicating that the paper employed by forgers is not simply a common low‐cost type. The crystalline index and intensity ratios between the peaks attributable to cellulose and fillers can provide additional information to trace back paper suppliers for forensic purposes.     

Quantitative Phase Analysis by the Rietveld Method for Forensic Science

Quantitative phase analysis (QPA) is helpful to determine the type attribute of the object because it could present the content of the constituents. QPA by Rietveld method requires neither measurement of calibration data nor the use of an internal standard; however, the approximate crystal structure of each phase in a mixture is necessary. In this study, 8 synthetic mixtures composed of potassium nitrate and sulfur were analyzed by Rietveld QPA method. The Rietveld refinement was accomplished with a material analysis using diffraction program and evaluated by three agreement indices. Results showed that Rietveld QPA yielded precise results, with errors generally less than 2.0% absolute. In addition, a criminal case which was broken successfully with the help of Rietveld QPA method was also introduced. This method will allow forensic investigators to acquire detailed information of the material evidence, which could point out the direction for case detection and court proceedings.     

The Potential of X‐Ray Diffraction in the Analysis of Burned Remains from Forensic Contexts*

Abstract: In view of the difficulties in extracting quantitative information from burned bone, we suggest a new and accurate method of determining the temperature and duration of burning of human remains in forensic contexts. Application of the powder X‐ray diffraction approach to a sample of human bone and teeth allowed their microstructural behavior, as a function of temperature (200–1000°C) and duration of burning (0, 18, 36, and 60 min), to be predicted. The experimental results from the 57 human bone sections and 12 molar teeth determined that the growth of hydroxylapatite crystallites is a direct and predictable function of the applied temperature, which follows a nonlinear logistic relationship. This will allow the forensic investigator to acquire useful information about the equilibrium temperature brought about by the burning process and to suggest a reasonable duration of fire exposure.     

Calcium and Phosphorus Detection Using Benchtop Versus Handheld X‐ray Fluorescence Spectrometers

Elemental analysis of calcium (Ca) and phosphorus (P) has been shown to be useful in differentiating skeletal and nonskeletal material. X‐ray fluorescence spectrometry (XRF) is an attractive, nondestructive technique for forensic anthropologists, and the development of portable XRF instrumentation is promising for field applications. This study examines the performance of handheld XRF instrumentation operated in air compared to a traditional benchtop XRF device that has the ability to control the analysis atmosphere. Both instruments can be used to effectively distinguish skeletal from nonskeletal remains. However, as the measurement atmosphere affects detection levels for calcium and phosphorus, Ca/P ratios obtained from the instruments and analysis conditions were found to differ significantly, with analyses conducted in air showing significantly lower phosphorus detection. Consequently, comparison of Ca/P ratios to conclude skeletal versus nonskeletal origin must be based on data collected under similar analysis conditions.     

Elemental Analysis of Variably Contaminated Cremains Using X‐ray Fluorescence Spectrometry

Analyzing and identifying skeletal remains becomes increasingly difficult when remains have been cremated, especially in cases where the cremated material may have been intentionally contaminated with nonskeletal material. This study examined the potential of X‐ray fluorescence spectrometry (XRF) to detect the presence of nonskeletal contaminants in samples of cremains. Eleven samples of cremains were variably combined with concrete mix and analyzed using XRF. Photon counts of elements in each sample were analyzed, and the coefficient of determination (R²) using unweighted linear regression as a function of percent cremains was calculated. Results showed that with changes in the proportion of skeletal material and contaminant, there were significant (R² > 0.90) changes in detected levels of phosphorus, potassium, zinc, aluminum, and sulfur. The use of XRF is concluded to be a valid approach in the identification of the presence of nonskeletal material in potentially contaminated cremains.     

Forensic Comparison of Automotive Aluminum Wheel Fragments Using Synchrotron Radiation X‐ray Fluorescence with 18‐ and 116‐keV Excitation X‐rays

The performance of synchrotron radiation X‐ray fluorescence (SR‐XRF) spectrometry for nondestructive discrimination of small fragments of automotive aluminum wheels was studied. Fragments (< 500 × 500 μm²) of 45 kinds of wheels were first analyzed by scanning electron microscopy–energy dispersive spectroscopy (SEM‐EDS) and then by SR‐XRF. Despite the Mg/Al intensity ratio being a useful identification index, SEM‐EDS was not efficient enough because of the absence of other meaningful indicators of comparison. Conversely, pairwise comparison was conducted and a 92.9% identification was achieved via SR‐XRF using 18‐keV X‐rays. Trace heavy elements in the high‐energy region were detected by SR‐XRF using 116‐keV X‐rays, and an 82.9% identification was obtained. Combined use of 18‐ and 116‐keV X‐rays allowed 98.2% identification. Hence, SR‐XRF is a powerful tool for nondestructive discrimination of automotive aluminum wheels with high precision using trace elements in a wide energy region.     

Practical Considerations in Trace Element Analysis of Bone by Portable X‐ray Fluorescence

Forensic anthropologists are more often turning to nondestructive methods to assist with skeletal analyses, specifically for trace elemental analyses. Portable XRF (pXRF) instruments are versatile and are able to be used in diverse settings or for specimens of a shape and size that cannot be accommodated by laboratory‐based instruments. Use of XRF requires knowledge of analysis parameters such as X‐ray penetration and exit depth. Analysis depth was determined by examining pure elements through known thicknesses of equine bone slices. Correlation between the element's X‐ray emission energy and the depth of reading was observed. Bone surfaces from a small unknown historic cemetery were analyzed before and after sanding of the periosteal surface to observe possible changes in XRF readings based on potential diagenesis. Results validate the pXRF device as a powerful and convenient instrument for nondestructive analysis, while highlighting limitations and considerations for the analysis of osseous materials.     

Single‐Image Rectification Technique in Forensic Science

Many researchers have been working in Spain to document the communal graves of those assassinated during the Spanish Civil War. This article shows the results obtained with two low‐cost photogrammetric techniques for the basic documentation of forensic studies. These low‐cost techniques are based on single‐image rectification and the correction of the original photo displacement due to the projection and perspective distortions introduced by the lens of the camera. The capability of image rectification is tested in an excavation in the village of Loma de Montija (Burgos, Spain). The results of both techniques are compared with the more accurate data obtained from a laser scanner system RIEGL LMS‐Z390i to evaluate the error in the lengths. The first technique uses a camera situated on a triangle‐shaped pole at a height of 5 m and the second positions the camera over the grave using a linearly actuated device. The first technique shows measurement errors less than 6%, whereas the second shows greater errors (between 8% and 14%) owing to the positioning of the carbon‐fiber cross on an uneven surface.     

Forensic Epidemiologic and Biomechanical Analysis of a Pelvic Cavity Blowout Injury Associated with Ejection from a Personal Watercraft (Jet‐Ski)

Jet‐propelled personal watercraft (PWC) or jet‐skis have become increasingly popular. The means of propulsion of PWC, which is a jet of water forced out of small nozzle at the rear of the craft, combined with a high risk of falling off of the seat and into close proximity with the water jet stream, raise the potential for a unique type of injury mechanism. The most serious injuries associated with PWC falls are those that occur when the perineum passes in close proximity to the jet nozzle and the high‐pressure water stream enters the vaginal or rectal orifice. We describe the forensic investigation into a case of an anovaginal “blowout” injury in a passenger who was ejected from the rear seat position of a PWC and subsequently suffered life‐threatening injuries to the pelvic organs. The investigation included a biomechanical analysis of the injury mechanism, a summary of prior published reports of internal pelvic injuries resulting from PWC falls as well as other water sports and activities, and a comparison of the severity of the injuries resulting from differing mechanisms using the New Injury Severity Score (NISS). The mean (±standard deviation [SD]) NISS values for reported PWC injuries [not including the NISS of 38 in this case study] were 11.2 (±9.5), while the mean value for reported water‐skiing falls was half that of the PWC group at 5.6 (±5.2). It was concluded that the analyzed injuries were unique to a PWC ejection versus other previously described non‐PWC‐associated water sport injuries. It is recommended that PWC manufacturers help consumers understand the potential risks to passengers with highly visible warnings and reduce injury risk with revised seat design, and/or passenger seat “deadman” switches.     

Influence of Velocity on Variability in Gait Kinematics: Implications for Recognition in Forensic Science

Closed circuit television (CCTV) footage is often available from crime scenes and may be used to compare perpetrators with suspects. Usually, the footage comprises incomplete gait cycles at different velocities, making gait pattern identification from crimes difficult. This study investigated the concurrence of joint angles throughout a gait cycle at three different velocities (3.0, 4.5, 6.0 km/h). Six datasets at each velocity were collected from 16 men. A variability range VR throughout the gait cycle at each velocity for each joint angle for each person was calculated. The joint angles at each velocity were compared pairwise, and whenever this showed values within the VR of this velocity, the case was positive. By adding the positives throughout the gait cycle, phases with high and low concurrences were located; peak concurrence was observed at mid‐stance phase. Striving for the same velocity for the suspect and perpetrator is recommended.     

X‐ray Scattering Evaluation of Ultrastructural Changes in Human Dental Tissues with Thermal Treatment

Micro‐ and ultrastructural analysis of burned skeletal remains is crucial for obtaining a reliable estimation of cremation temperature. Earlier studies mainly focused on heat‐induced changes in bone tissue, while this study extends this research to human dental tissues using a novel quantitative analytical approach. Twelve tooth sections were burned at 400–900°C (30‐min exposure, increments of 100°C). Subsequent combined small‐ and wide‐angle X‐ray scattering (SAXS/WAXS) experiments were performed at the Diamond Light Source synchrotron facility, where 28 scattering patterns were collected within each tooth section. In comparison with the control sample, an increase in mean crystal thickness was found in burned dentine (2.8‐fold) and enamel (1.4‐fold), however at a smaller rate than reported earlier for bone tissue (5–10.7‐fold). The results provide a structural reference for traditional X‐ray scattering methods and emphasize the need to investigate bone and dental tissues separately to obtain a reliable estimation of cremation temperature.     

Development of a Simple and Low‐Cost Enzymatic Methodology for Quantitative Analysis of Carbamates in Meat Samples of Forensic Interest

Abstract: Foods contaminated with a granulated material similar to Temik (a commercial pesticide formulation containing the carbamate insecticide aldicarb) are often involved in accidental ingestion, suicides, and homicides in Brazil. We developed a simple technique to detect aldicarb. This technique is based on the inhibition of a stable preparation of the enzyme acetylcholinesterase, and it is specially adapted for forensic purposes. It comprises an initial extraction step with the solvent methylene chloride followed by a colorimetric acetylcholinesterase assay. We propose that results of testing contaminated forensic samples be expressed in aldicarb equivalents because, even though all other carbamates are also potent enzyme inhibitors, aldicarb is the contaminant most frequently found in forensic samples. This method is rapid (several samples can be run in a period of 2 h) and low cost. This method also proved to be precise and accurate, detecting concentrations as low as 40 μg/kg of aldicarb in meat samples.     

Optimization of Headspace Solid‐Phase Microextraction Technique for Extraction of Volatile Smokeless Powder Compounds in Forensic Applications

Smokeless powders are low explosives and are potentially found in cases involving firearms and improvised explosive devices. Apart from inorganic compound analysis, forensic determination of organic components of these materials appears as a promising alternative, especially the chromatographic techniques. This work describes the optimization of a solid‐phase microextraction technique using an 85 μm polyacrylate fiber followed by gas chromatography‐flame ionization detection for smokeless powder. A multivariate experimental design was performed to optimize extraction‐influencing parameters. A 2⁴ factorial first‐order design revealed that sample temperature and extraction time were the major influencing parameters. Doehlert matrix design has subsequently selected 66°C and 21 min as the compromised conditions for the two predetermined parameters. This extraction technique has successfully detected the headspace compounds of smokeless powders from different ammunition types and allowed for their differentiation. The novel technique allows more rapid sample preparation for chromatographic detection of smokeless powders.     

The Utility of the Samworth and Gowland Age‐at‐Death “Look‐up” Tables in Forensic Anthropology*

Abstract: Accurate age‐at‐death estimates are crucial to forensic anthropologists when onstructing biological profiles aimed at narrowing a missing‐persons list and to allow for timely and efficient identification of an unknown victim. The present contribution evaluates the utility of three new age‐at‐death estimation techniques recently proposed by Samworth and Gowland (2007). Results indicate that, in the samples under study, the Samworth and Gowland estimates from the pubic symphysis and auricular surface perform similar to alternate phase methods. The combined method does not appear to further enhance either the precision or the accuracy of the single pubic symphysis age‐at‐death estimate. In conclusion, these new methods seem to be more robust to distribution deviations than originally proposed by Samworth and Gowland (2007). They are therefore suitable for immediate and reliable forensic usage in the United States and worthy of further research for their use in North American forensic contexts.     

Utilization of X‐ray Computed Tomography for the Exclusion of a Specific Caliber and Bullet Type in a Living Shooting Victim

A bystander claimed to have been shot by a police officer, and CT scans were used to match qualitative and quantitative aspects of the unremoved bullet with police issued 9 mm Luger ammunition. CT scan methodology proved a valid approach for the measurement of bullets based on calculated measurement capability and correlation with “gold standard” physical measurement by vernier caliper. Measurements regarding length and base diameter, as well as length/diameter ratio, were insufficient to unambiguously identify a specific caliber, or a bullet of specific mass within a caliber class. It was, however, possible to exclude a bullet of specific design and mass with well‐characterized precision and accuracy values under selected CT scan conditions. A 9 mm Luger bullet (115 gr FMJ RN) was excluded from involvement in a shooting based on qualitative bullet shape combined with length, base, and ratio measurements of the bullet in‐situ for the victim.     

The Optimization of Electrophoresis on a Glass Microfluidic Chip and its Application in Forensic Science

Microfluidic chips offer significant speed, cost, and sensitivity advantages, but numerous parameters must be optimized to provide microchip electrophoresis detection. Experiments were conducted to study the factors, including sieving matrices (the concentration and type), surface modification, analysis temperature, and electric field strengths, which all impact the effectiveness of microchip electrophoresis detection of DNA samples. Our results showed that the best resolution for ssDNA was observed using 4.5% w/v (7 M urea) lab‐fabricated LPA gel, dynamic wall coating of the microchannel, electrophoresis temperatures between 55 and 60°C, and electrical fields between 350 and 450 V/cm on the microchip‐based capillary electrophoresis (μCE) system. One base‐pair resolution could be achieved in the 19‐cm‐length microchannel. Furthermore, both 9947A standard genomic DNA and DNA extracted from blood spots were demonstrated to be successfully separated with well‐resolved DNA peaks in 8 min. Therefore, the microchip electrophoresis system demonstrated good potential for rapid forensic DNA analysis.     

A Review of Forensic Science Higher Education Programs in the United States: Bachelor’s and Master’s Degrees*

Abstract: As the number of forensic science programs offered at higher education institutions rises, and more students express an interest in them, it is important to gain information regarding the offerings in terms of courses, equipment available to students, degree requirements, and other important aspects of the programs. A survey was conducted examining the existing bachelor’s and master’s forensic science programs in the U.S. Of the responding institutions, relatively few were, at the time of the survey, accredited by the forensic science Education Programs Accreditation Commission (FEPAC). In general, the standards of the responding programs vary considerably primarily in terms of their size and subjects coverage. While it is clear that the standards for the forensic science programs investigated are not homogeneous, the majority of the programs provide a strong science curriculum, faculties with advanced degrees, and interesting forensic‐oriented courses.