Elemental analysis by energy dispersive x-ray: a significant factor in the forensic analysis of glass.

Eighty-one glass samples were analyzed by EDX; two were indistinguishable. However, when the physical properties of the glass samples were considered, all glass samples were distinguishable from each other. The need to examine glass with respect not only to physical properties but also to elemental composition has been demonstrated. The authors believe that if glass is examined only by density and refractive indexes it is quite possible to conclude incorrectly that glass samples with the same physical qualities could have originated from the same source. To confirm that the glass specimens may have in fact originated from the same source their elemental compositions in addition to density and refractive indexes must be determined. The analysis by EDX of glass samples can selectively eliminate most specimens on the basis of elemental differences. If this step is performed prior to refractive index or density measurements considerable time savings can be realized in casework situations.     

Application of false discovery rate procedure to pairwise comparisons of refractive index of glass fragments

This study was undertaken to apply a new method of controlling type I error when performing pairwise comparisons. The Benjamini and Hochberg false discovery rate (FDR) controlling procedures have proved to be very powerful tools in solving many practical problems but have not yet been applied to pairwise comparisons of refractive index of glass samples. Students t-test and Welch test (unequal variance Student's t-test) were applied to all possible pairwise comparisons. The comparisons were made on the basis of refractive index values of 72 glass fragments from different car windows and 69 different fragments from one windscreen. The type I error was controlled by the use of Benjamini and Hochberg false discovery rate (FDR) controlling procedure. To illustrate the importance of controlling type I error when using pairwise comparisons, results of pairwise comparisons with the FDR controlling procedure were compared to those comparisons made without any controlling procedure. Significantly fewer false negative results (false rejection of H0) were found during the use of FDR procedure in the comparison of refractive indices from the same windscreen than when comparing without controlling type I error. The results of application of FDR method were also compared to the results of other post-hoc tests, such as Tukey HSD test and Bonfferoni test. The FDR method has higher power than Bonferroni method and Tukey HSD method and control errors better than comparing without controlling type I error. The method of choice, for pairwise comparison of glass fragments on the basis of refractive index is Welch test with FDR adjustment. The method gave type I errors at level about 5.3% and type II error at about 3.7%.     

Factors affecting the forensic examination of automotive lubricating oils

Lubricating oil comparisons impact a variety of forensic investigations, including cases where oil was transferred from a suspect vehicle to the crime scene or victim. In this study, high-temperature gas chromatography/mass spectrometry was used to examine the influence of oil mixtures and oil changes over time on the comparison of known and questioned lubricating oils. Varying concentrations of oil mixtures were prepared and showed the potential for identifying individual components. Motor oils from 18 automobiles monitored over a 2-month period did not demonstrate significant changes in the chromatographic data. Chemometric analysis of motor oil mass spectral data provided little information regarding differentiation of, or changes in, the samples. Power steering fluid (PSF) from a naturally occurring leak collected from several locations was consistent with the PSF in the automobile's reservoir, and the PSF composition did not change over time.     

玻璃折射率数据处理方法初探

目的探讨玻璃折射率数据处理方法。方法将案件中收集到的45个玻璃样品和同一个车灯不同部位的45块玻璃样品进行折射率测定。用独立样本Student’st检验、welch检验以及方差分析（ANOVA）对数据进行成对检验。结果方差分析法中Dunnett’s C法处理玻璃折射率数据,有效控制了第一类和第二类错误。当α=0．05时,犯第一类错误的概率约为4．44％,犯第二类错误的概率约为3．54％。     

Mixed effects modelling for glass category estimation from glass refractive indices

520 Glass fragments were taken from 105 glass items. Each item was either a container, a window, or glass from an automobile. Each of these three classes of use are defined as glass categories. Refractive indexes were measured both before, and after a programme of re-annealing. Because the refractive index of each fragment could not in itself be observed before and after re-annealing, a model based approach was used to estimate the change in refractive index for each glass category. It was found that less complex estimation methods would be equivalent to the full model, and were subsequently used. The change in refractive index was then used to calculate a measure of the evidential value for each item belonging to each glass category. The distributions of refractive index change were considered for each glass category, and it was found that, possibly due to small samples, members of the normal family would not adequately model the refractive index changes within two of the use types considered here. Two alternative approaches to modelling the change in refractive index were used, one employed more established kernel density estimates, the other a newer approach called log-concave estimation. Either method when applied to the change in refractive index was found to give good estimates of glass category, however, on all performance metrics kernel density estimates were found to be slightly better than log-concave estimates, although the estimates from log-concave estimation prossessed properties which had some qualitative appeal not encapsulated in the selected measures of performance. These results and implications of these two methods of estimating probability densities for glass refractive indexes are discussed.     

The consequences of potentially differing distributions of the refractive indices of glass fragments from control and recovered sources

In forensic cases involving glass evidence, the variance of the recovered glass refractive index (RI) has been observed to be larger than the variance of the control glass RI. This has consequences for subsequent interpretation. To investigate this phenomenon, a study was made of the probable distributions of refractive indices of the recovered glass given a range of casework type scenarios involving breakage and backscatter. An investigation of the consequences of any distribution differences with regard to casework was also made. It was discovered that the inclusion of surface fragments from the float surface of the glass can have a profound effect on the comparison of recovered and control glass samples. The effect was largest when a breaker was striking the float surface of a window. In particular, it was found that the inclusion of a few surface fragments even post grouping is sufficient by itself to explain the observed differences in variance of RI between control and recovered groups. Surface fragments, if present, are very likely to be treated as outliers and to be deemed as non-matching. The findings of this paper challenge routine glass examination procedure and suggest that knowledge of which surface is facing the striker is valuable information in interpretation.     

Bayesian mixture modelling for glass refractive index measurement

Glass is a common type of physical evidence in forensic science. Broken glass recovered from a suspect may have similar physical characteristics to glass collected at a crime scene and therefore can be used as evidence. Statistical treatment of this evidence involves computing a measure of the weight of evidence. This may be done in a Bayesian framework that incorporates information from the circumstances of the crime. One of the most crucial quantities in this calculation is the assessment of the relative rarity of the characteristics of the glass, essentially the probability distribution used to model the physical characteristics of recovered glass. Typical characteristics used in casework are the elemental composition of glass and the refractive index measurement. There is a considerable body of scientific literature devoted to the modelling of this information. For example a kernel density estimation has been used to model the background population of glass based on the refractive index measurement and a multivariate Gaussian finite mixture model has been used to model the elemental composition of glass. In this paper, we present an alternative approach, the Dirichlet Process Mixture Model, to model the glass refractive index measurement in a Bayesian methodology. A key advantage is that using this method allows us to model the probability density distribution of refractive index measurements in a more flexible way.     

Microscopical discrimination of twins' head hair

Twin populations are ideal for studying human variation; a study of twin's hair, therefore, provided a better understanding of the value of hair comparisons. Duplicate head hair samples from 17 pairs of twins and one set of identical triplets were compared in a verified blind study. In addition to the direct comparison of all twins, random samples of two or three hairs were compared with randomly selected groups of known samples in a second blind study, to better simulate an ordinary forensic science case. Features commonly used by forensic hair examiners were adequate to distinguish hair samples from each twin from all other samples, illustrating the power of microscopical comparison when numerous questioned hairs are available in evidence. When two or three hairs were compared with randomly selected known samples, several were indistinguishable from hair samples other than the true source, proving once again that a human hair can never be associated with one person to the exclusion of all others.     

Elemental analysis of glass by laser ablation inductively coupled plasma optical emission spectrometry (LA-ICP-OES)

The elemental analysis of glass evidence has been established as a powerful discrimination tool for forensic analysts. Laser ablation inductively coupled plasma optical emission spectrometry (LA-ICP-OES) has been compared to laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) and energy dispersive micro X-ray fluorescence spectroscopy (μXRF/EDS) as competing instrumentation for the elemental analysis of glass. The development of a method for the forensic analysis of glass coupling laser ablation to ICP-OES is presented for the first time. LA-ICP-OES has demonstrated comparable analytical performance to LA-ICP-MS based on the use of the element menu, Al (Al I 396.15 nm), Ba (Ba II 455.40 nm), Ca (Ca II 315.88 nm), Fe (Fe II 238.20 nm), Li (Li I 670.78 nm), Mg (Mg I 285.21 nm), Sr (Sr II 407.77 nm), Ti (Ti II 368.51 nm), and Zr (Zr II 343.82 nm). The relevant figures of merit, such as precision, accuracy and sensitivity, are presented and compared to LA-ICP-MS. A set of 41 glass samples was used to assess the discrimination power of the LA-ICP-OES method in comparison to other elemental analysis techniques. This sample set consisted of several vehicle glass samples that originated from the same source (inside and outside windshield panes) and several glass samples that originated from different vehicles. Different match criteria were used and compared to determine the potential for Type I and Type II errors. It was determined that broader match criteria is more applicable to the forensic comparison of glass analysis because it can reduce the affect that micro-heterogeneity inherent in the glass fragments and a less than ideal sampling strategy can have on the interpretation of the results. Based on the test set reported here, a plus or minus four standard deviation (± 4s) match criterion yielded the lowest possibility of Type I and Type II errors. The developed LA-ICP-OES method has been shown to perform similarly to LA-ICP-MS in the discrimination among different sources of glass while offering the advantages of a lower cost of acquisition and operation of analytical instrumentation making ICP-OES a possible alternative elemental analysis method for the forensic laboratory.     

Identification and comparison of electrical tapes using instrumental and statistical techniques: I. Microscopic surface texture and elemental composition

Comparisons of polyvinyl chloride electrical tape typically rely upon evaluating class characteristics such as physical dimensions, surface texture, and chemical composition. Given the various techniques that are available for this purpose, a comprehensive study has been undertaken to establish an optimal analytical scheme for electrical tape comparisons. Of equal importance is the development of a quantitative means for sample discrimination. In this study, 67 rolls of black electrical tape representing 34 different nominal brands were analyzed via scanning electron microscopy and energy dispersive spectroscopy. Differences in surface roughness, calendering marks, and filler particle size were readily apparent, including between some rolls of the same nominal brand. The relative amounts of magnesium, aluminum, silicon, sulfur, lead, chlorine, antimony, calcium, titanium, and zinc varied greatly between brands and, in some cases, could be linked to the year of manufacture. For the first time, quantitative differentiation of electrical tapes was achieved through multivariate statistical techniques, with 36 classes identified within the sample population. A single-blind study was also completed where questioned tape samples were correctly associated with known exemplars. Finally, two case studies are presented where tape recovered from an improvised explosive device is compared with tape recovered from a suspect.     

The interpretation of refractive index measurements. III

The question of whether or not to group recovered glass fragments before comparison with a control sample is fundamental to the interpretation of refractive index measurements. A computer program has been written to perform the grouping and explore the consequences. Grouping the fragments is shown to increase the chances of finding all recovered fragments similar when they have in fact come from the same source as the control, and to give enhanced discrimination when the recovered glass has come from a different source. When the recovered fragments have come from two different sources the consequences of the grouping procedure are preferable to non-grouping.     

Observer determination of the make,model, and year of questioned vehicles

Often, criminal acts involving a vehicle are caught on digital video surveillance systems. While potentially useful for an investigation, the recording conditions are typically less than optimal for the extraction of key information for the identification of the perpetrator, such as a license plate. Providing the make, model and year of a questioned vehicle is a common request for examiners, to narrow the field of potential suspect vehicles. This study seeks to compare the performance of a nonpeer-reviewed make, model, and year determination between two separate groups, specifically, trained forensic image examiners and nontrained individuals. Results show that even with varied image capture conditions and quality, the trained forensic image examiners more correctly and completely identified the test group of questioned vehicles make, model, and year.     

Identification of Acer rubrum using amplified fragment length polymorphism

Amplified fragment length polymorphism (AFLP) analysis of botanical forensic evidence provides a means of obtaining a reproducible DNA profile in a relatively short period of time in species for which no sequence information is available. AFLP profiles were obtained for 40 Acer rubrum trees. Leaf material from five additional species was also typed. Genomic DNA was isolated using the DNeasy Plant Miniprep Kit (Qiagen, Valencia, CA), double-digested by two restriction endonucleases (EcoRI and MseI) and ligated to oligonucleotide adapters. Two consecutive PCR reactions (pre-amplification and selective amplification) were performed using a modification of the AFLP protocol described by Gibco (Invitrogen, Rockville, MD). The DNA fragments were separated by capillary electrophoresis using the CEQ 8000 DNA Fragment Analyzer. A number of Acer rubrum species-specific peaks were identified. In addition, within this closed set of samples, 15 of 16 (93.8%) blind samples were correctly identified. AFLP data can be used to determine the species of botanical evidence or to associate a sample to a source. This information can be used in forensic investigations to link a piece of evidence with a particular location or suspect.     

Characterization and differentiation of aluminum powders used in improvised explosive devices – Part 1: Proof of concept of the utility of particle micromorphometry

Aluminum (Al) powders are commonly used in improvised explosive devices as metallic fuels, a component of explosive mixtures. These powders can be obtained readily from industrial‐scale and consumer products, and produced using unsophisticated “kitchen chemistry” techniques. This research demonstrates the potential of automated particle micromorphometry for comparisons between known source and questioned Al powders recovered from IEDs, as well as for insight into the method of Al powder manufacture. Al powder samples were obtained from legitimate manufacturers, and 56 samples were produced “in‐house” from Al‐containing spray paints and ball‐milled Al foils. Transmitted light microscope images of Al powder particles were acquired using an automated stage with automated z‐focus; 17 size and shape parameters were measured for all particles. Approximately 37,000–2,500,000 particles/sample were analyzed using an open‐source statistical package with customized code. Dimensionality reduction was required for processing the large datasets: eight of the 17 measured variables were selected based on inspection of the correlation matrix. Data from four subsamples from each of the 56 samples produced using “in‐house” methods were analyzed using ANOVA to assess the within‐ and between‐sample variation. High within‐sample variation was noted; however, ANOVA and post‐hoc Tukey's honestly significant difference (HSD) tests demonstrated that the between‐sample variation was substantially larger than the within‐sample variation. Each sample could be differentiated from all other samples in the test set. Future experiments will focus on ways to reduce the within‐sample variation, and additional statistical and microanalytical methods to classify sources and confidently constrain the method of Al powder manufacture.     

Immunohistochemical analysis of forensic evidence from a double homicide

We report the use of immunohistochemical staining for analysis of forensic evidence from a double homicide. A 38-year-old woman and her 7-year-old daughter were murdered by multiple blows to the head and face with a tomahawk, resulting in multiple fragments of brain tissue scattered about the murder scene. The victims' husband and father was the main suspect, who maintained that he was out of town on business during the evening of the murders. However, a shirt taken from the suspect's car on the morning after the murders (secured by the police before the suspect visited the murder scene) was found to have two small stains. DNA analysis on the stains showed the presence of the deceased wife's DNA, and immunohistochemical stains on shirt fragments conclusively documented the presence of deep central nervous system tissue, providing the critical piece of evidence needed to arrest and prosecute the suspect. This report demonstrates that shirt or similar cloth fragments can be processed into paraffin blocks and subsequently immunostained to search for and classify types of tissue fragments that may be present on the fabric.     

Analysis of glass fragments by laser ablation-inductively coupled plasma-mass spectrometry and principal component analysis

Laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) is used to differentiate glass samples with similar optical and physical properties based on trace elemental composition. Laser ablation increases the number of elements that can be used for differentiation by eliminating problems commonly associated with dissolution and contamination. In this study, standard residential window and tempered glass samples that could not be differentiated by refractive index or density were successfully differentiated by LA-ICP-MS. The primary analysis approach used is Principal Component Analysis (PCA) of the complete mass spectrum. PCA, a multivariate analysis technique, provides rapid analysis of samples without time-consuming pair-wise comparison of calibrated analyses or prior knowledge of the elements present in the samples. Probabilities for positive association of the individual samples are derived from PCA. Utilization of the Q-statistic with PCA allowed us to distinguish all samples within the set to a certainty greater than the 99% confidence interval.     

玻璃雨飞溅高度及分布的实验研究

目的研究平板玻璃打碎后玻璃雨的飞溅高度及空间分布,从而为玻璃物证提取和现场分析提供依据。方法应用自制的实验装置,模拟嫌疑人手持硬物击碎窗户玻璃,收集窗户下地面上和打击者处飞溅的玻璃微粒,对颗粒大小、散布区域进行统计分析,并与通过动力学计算得出的分布进行比较。结果在距离窗户0.5m处,玻璃颗粒的飞溅高度可高于玻璃上相应来源点的高度;较小颗粒有较大的飞溅范围。结论玻璃雨颗粒大小分布和空间分布规律对于嫌疑人身上、头部玻璃物证的提取以及案件的现场分析有十分重要的意义。     

强奸致孕形成部分性葡萄胎的检验分析

目的探讨强奸致孕案葡萄胎组织的DNA检验和STR结果分析。方法用DNA Typer TM15试剂盒对犯罪嫌疑人、受害人血样和流产胚胎组织进行荧光复合STR基因座扩增检测。结果检测的一例流产胚胎组织DNA的STR峰谱表现出部分3条带,且3条带中有两个等位基因来源于犯罪嫌疑人,另外一个来源于受害人,推断为单卵双精子受精的部分性葡萄胎。结论应用STR分型技术可以推断葡萄胎的DNA来源和受精类型,为亲缘关系鉴定提供依据。     

Particle size analysis of soils under simulated scene of crime conditions: the interest of multivariate analyses

Two simulated scenes of crime have been studied. Soil traces adhering to boots, sport shoes and tissues have been compared with control samples using particle size analysis. Comparisons of percentage of particles per class interval and multivariate analyses were used to determine how the size distribution of each suspect sample varied compared to the original distribution. A loss of coarse fractions characterized most of the suspect samples even though they were derived from soils having different distributional patterns. However, the differences between control and suspect samples were found to be more important for soils dominated by extreme size classes than for soils rich in medium size particles. The differences among soil samples from the same source were found to be restricted to the extreme size classes. The finding of significant differences within size classes ranging from 1 to 0.063 mm should be then considered as a dissimilarity sign between trace sample and hypothetic control soil.     

Particle size analysis of soils under simulated scene of crime conditions: the interest of multivariate analyses

Two simulated scenes of crime have been studied. Soil traces adhering to boots, sport shoes and tissues have been compared with control samples using particle size analysis. Comparisons of percentage of particles per class interval and multivariate analyses were used to determine how the size distribution of each suspect sample varied compared to the original distribution. A loss of coarse fractions characterized most of the suspect samples even though they were derived from soils having different distributional patterns. However, the differences between control and suspect samples were found to be more important for soils dominated by extreme size classes than for soils rich in medium size particles. The differences among soil samples from the same source were found to be restricted to the extreme size classes. The finding of significant differences within size classes ranging from 1 to 0.063 mm should be then considered as a dissimilarity sign between trace sample and hypothetic control soil.