Microscopical recognition and characterization of solution dyed fibers.

Solution dyed fibers are synthetic fibers colored through the addition of insoluble pigmentation to the polymer prior to extrusion. This is in contrast to most textile fibers, which are traditionally colored via immersion in liquid dyebaths following extrusion. Solution dyed fibers are increasing in market share in numerous applications (e.g., apparel, carpet, upholstery), and thus, the microscopic characteristics and variety of pigments used to color them represent unexploited properties in forensic fiber comparisons. This paper presents the development of a microscopical process to first recognize a fiber as solution dyed and subsequently characterize the color and optical properties of each type of pigment found in a given fiber. To this end, a set of 76 fibers, representing polypropylene, nylon, polyester, and rayon, spanning all nominal colors and several consumer applications were analyzed longitudinally and in cross section using a combination of polarized light, fluorescence, and oil immersion microscopy. A given fiber contained between one and six different pigments, and a total of 260 pigments (not all unique) were recognized within this set of fibers. Pigment morphologies were categorized as angular, elongated, rounded, finely divided, or streaky, and about 40% of the pigments fluoresced. Ultimately, this body of data is intended to provide trace evidence examiners with a specific approach to recognize and begin to exploit pigmented fibers encountered in casework.

Locating, Identifying, and Comparing Sub-visible Paint Particles.

Forensic paint comparisons are generally conducted on samples which, while small relative to their source, are still visible to the unaided eye and are thus located and analyzed without great difficulty. Here we demonstrate that a more detailed examination of candidate transfer surfaces can capture materials (questioned samples), even when such traces are invisible to the unaided eye. While certain analytical details (such as layer sequence or a pure FTIR spectrum) may not be obtainable from such traces due to their size and condition, a detailed analysis of the sample characteristics that are analytically accessible may still provide sufficient analytical data to arrive at a probative result. Here we present the application of this approach to a suspected paint transfer case, involving particles of paint as small as 40 µm in size. Using a combination of stereomicroscopy, polarized light microscopy, infrared microspectroscopy, Raman microspectroscopy, and SEM/EDS, all performed on a single, subsample of the original minute particle, it was possible to demonstrate evidence of a two-way transfer between the suspected sources. Furthermore, the transferred paint particle in one direction could be classified as automotive in nature based on a combination of polymer composition, microscopic texture, and pigment package (which included three specifically identified pigments). This work demonstrates (i) the potential for improving detection limits when searching for a questioned sample, (ii) the potential benefits of higher resolution analyses on samples that would be traditionally labeled as "sample-size limited," and (iii) the value of case-specific interpretation over standardized, one-size fits all report templates.

A Generalized Approach to Forensic Dye Identification: Development and Utility of Reference Libraries.

While color is arguably the most important optical property of evidential fibers, the actual dyestuffs responsible for its expression in them are, in forensic trace evidence examinations, rarely analyzed and still less often identified. This is due, primarily, to the exceedingly small quantities of dye present in a single fiber as well as to the fact that dye identification is a challenging analytical problem, even when large quantities are available for analysis. Among the practical reasons for this are the wide range of dyestuffs available (and the even larger number of trade names), the low total concentration of dyes in the finished product, the limited amount of sample typically available for analysis in forensic cases, and the complexity of the dye mixtures that may exist within a single fiber. Literature on the topic of dye analysis is often limited to a specific method, subset of dyestuffs, or an approach that is not applicable given the constraints of a forensic analysis. Here, we present a generalized approach to dye identification that (1) combines several robust analytical methods, (2) is broadly applicable to a wide range of dye chemistries, application classes, and fiber types, and (3) can be scaled down to forensic casework-sized samples. The approach is based on the development of a reference collection of 300 commercially relevant textile dyes that have been characterized by a variety of microanalytical methods (HPTLC, Raman microspectroscopy, infrared microspectroscopy, UV-Vis spectroscopy, and visible microspectrophotometry). Although there is no single approach that is applicable to all dyes on every type of fiber, a combination of these analytical methods has been applied using a reproducible approach that permits the use of reference libraries to constrain the identity of and, in many cases, identify the dye (or dyes) present in a textile fiber sample.

A survey of extraction solvents in the forensic analysis of textile dyes.

The characterization and identification of dyes in fibers can be used to provide investigative leads and strengthen associations between known and questioned items of evidence. The isolation of a dye from its matrix (e.g., a textile fiber) permits detailed characterization, comparison and, in some cases, identification using methods such as thin layer chromatography in conjunction with infrared and Raman spectroscopy. A survey of dye extraction publications reveals that pyridine:water (4:3) is among the most commonly cited extraction solvent across a range of fiber and dye chemistries. Here, the efficacy of this solvent system has been evaluated for the extraction of dyes from 172 commercially prevalent North American textile dyes. The evaluated population represents seven dye application classes, 18 chemical classes, and spans nine types of commercial textile fibers. The results of this survey indicate that ∼82% of the dyestuffs studied are extractable using this solvent system. The results presented here summarize the extraction efficacy by class and fiber type and illustrate that this solvent system is applicable to a wider variety of classes and fibers than previously indicated in the literature. While there is no universal solvent for fiber extraction, these results demonstrate that pyridine:water represents an excellent first step for extracting unknown dyes from questioned fibers in forensic casework.

Applications of Blue Light-curing Acrylic Resin to Forensic Sample Preparation and Microtomy.

This study discusses the results of an evaluation of a one-part blue light-curing acrylic resin for embedding trace evidence prior to the preparation of thin sections with a microtome. Through a comparison to several epoxy resins, the physical properties relevant to both trace evidence examination and analytical microscopy in general, including as viscosity, clarity, color, hardness, and cure speed, were explored. Finally, thin sections from paint samples embedded in this acrylic resin were evaluated to determine if, through smearing or impregnation, the resin contributed to the infrared spectra. The results of this study show that blue light-curing acrylic resins provide the desired properties of an embedding medium, generate high-quality thin sections, and can significantly simplify the preparation of paint chips, fibers and a multitude of other types of microscopic samples in the forensic trace evidence laboratory.