An Evaluation of Total Reflection X-Ray Fluorescence as a Tool for Forensic Discrimination of Single Polyester Fibers.

Total reflection X-ray fluorescence (TXRF) spectrometry was applied to a forensic discrimination of single polyester fibers. In a non-destructive direct measurement of 5 mm long single fibers used for forensic references, trace metallic elements such as Ti, Sb, Ge, Mn, and Co, found in additives and catalyst residues, were detected using a benchtop TXRF spectrometer. The individual elemental compositions of the fibers were identified, and correlations between the compositions and manufacturers were established using principal component analysis (PCA). Black polyester fibers sampled from the car trunk mats were also analyzed. Several fibers were found to contain both Sb and Ge, elements that characterize different polymerization catalysts; this indicates that the fibers were composed of recycled materials. The TXRF and SR-µXRF spectra showed similar patterns for the fiber samples that were analyzed.

Homo- and heteronuclear two-dimensional covariance solid-state NMR spectroscopy with a dual-receiver system.

Two-dimensional (2D) covariance NMR spectroscopy, which has originally been established to extract homonuclear correlations (HOMCOR), is extended to include heteronuclear correlations (HETCOR). In a (13)C/(15)N 2D chemical shift correlation experiment, (13)C and (15)N signals of a polycrystalline sample of (13)C, (15)N-labeled amino acid are acquired simultaneously using a dual-receiver NMR system. The data sets are rearranged for the covariance data processing, and the (13)C-(15)N heteronuclear correlations are obtained together with the (13)C-(13)C and (15)N-(15)N homonuclear correlations. The present approach retains the favorable feature of the original covariance HOMCOR that the spectral resolution along the indirect dimension is given by that of the detection dimension. As a result, much fewer amounts of data are required to obtain a well-resolved 2D spectrum compared to the case of the conventional 2D Fourier-Transformation (FT) scheme. Hence, one can significantly save the experimental time, or enhance the sensitivity by increasing the number of signal averaging within a given measurement time.