Characterization of metal components in white-based polyester single fibers by X-ray fluorescence spectrometry and X-ray absorption fine structure analysis utilizing synchrotron radiation for forensic discrimination

Abstract

Discrimination of single fibers is important in forensic investigation. Conventional microscopic observation and analytical methods such as micro-Fourier transform-infrared spectroscopy, a suitable technique for polymer component identification, can discriminate single white fibers made from different polymers. Polyesters contain metal compounds derived from polymerization catalysts, transesterification catalysts, and matting agents. Here we propose a forensic method for discriminating white-based polyester single fibers. The X-ray intensity ratios, distribution of metal elements, and chemical states are identified by semi-microbeam X-ray fluorescence (XRF) spot analysis, nanobeam XRF imaging, and X-ray absorption fine structure analysis (XAFS) utilizing synchrotron radiation, respectively. The analytical specimens were white-based polyester single fibers from the standard forensic fiber collection (Microtrace LLC, USA) and commercially available polyester products. Semi-microbeam XRF spot analysis detected metallic elements such as Ti, Mn, Co, Ge, and Sb derived from polymerization catalysts, transesterification catalysts, and matting agents. The X-ray intensity ratios of Ti/Mn, Ti/Ge, Ti/Sb, and Mn/Sb were obtained with good reproducibility but those of Ti/Co, Mn/Co, and Co/Sb, which are related to cobalt, were lowly reproducible in some samples. The poor reproducibility of the cobalt-related X-ray intensity ratios was attributed to uneven distributions of the metallic elements in the polyester single fibers, as visualized by nanobeam XRF imaging. The images showing elemental heterogeneity have proven to be good markers for identification. The XAFS results showed that three types of Ti compounds and two types of cobalt compounds are utilized in different applications of polyester single fibers; moreover, the chemical states are useful indices of single-fiber discrimination.