Evaluation of the detectability and quantification of respirable crystalline silica by X-ray powder diffraction methods

Abstract

X-ray powder diffraction is one of the most sensitive methods for the analysis of crystalline forms of silica. In addition to detection and quantification, it can determine the specific crystalline species in the sample. The principal limitations of the method depend on the effective volume of the sample in the X-ray beam and the number of crystallites in the proper orientation to diffract. Detection limits are usually reported as 2 μg in thin-film filter mounts and 0.1% in bulk samples that are free of interference from associated minerals. Filter methods are most often used for air quality monitoring and several standardized procedures have been certified. Standard procedures for bulk samples are difficult to certify because of the variability of the matrices and their potential interferences. All of the methods of quantification require calibration with known samples of quartz or cristobalite. Certification of standard samples involves characterization of the particle and crystallite size and size distribution and amorphous content as well as determining the X-ray diffraction response. Although quartz is readily available and cristobalite is easy to synthesize, preparation of quantities of sufficient uniformity and stability is a limiting factor in certifying such samples for reasonable costs. Conventional diffraction equipment can be used for crystalline silica analysis at the present detection limits required by safety standards. Relatively simple modifications of the diffractometer will increase its sensitivity to small amounts of silica and improve the lower limits of quantification.