Quantitative Analysis of Silica in Silica-Kaolin Mixtures by Photoacoustic and Diffuse Reflectance Spectroscopies

"INTRODUCTION Silica and kaolin (a layer aluminosilicate) are among the major constituents of most coal mine dusts.' Whereas kaolin is cytotoxic in vitro but nonfibrogenic in vivo in humans and experimental animals,2-4 the cytotoxic and fibrogenic potential of silica is rather well established.5 Wallace and co-workers 6-8 have studied the cytotoxic potentials of both native and surface-modified silica and kaolin and inferred that retoxification is slow in the case of occluded silica vis-à-vis native silica. Recent epide¬miological studies indicate that silica concentration alone in a mine dust, as determined by transmission IR spec¬troscopy (TIRS), does not correlate well with the pro¬gression of coal workers' pneumoconiosis. 9 This obser¬vation has led to the suggestions that silica particles occluded by clays such as kaolin may not be fibrogenic. This proposal requires accurate estimations of kaolin, silica, and occluded silica. The current method of silica analysis in a mine dust sample employs TIRS of the 797- cm -1 band of silica, although its accuracy, as well as that of x-ray diffraction studies, is no better than 25 % , even in a laboratory-generated dust.° In this paper we have employed the techniques of diffuse reflectance spectros¬copy (DRS) and photoacoustic spectroscopy (PAS), in conjunction with an FT-IR spectrometer, for the quan¬titative determination of silica in laboratory-generated silica-kaolin mixtures.One of the main advantages of DRS and PAS is that, in these techniques, problems arising from sample prep¬aration of the KBr-based disks used in TIRS are avoided. There are, however, several other considerations (e.g., particle size effects and saturation phenomenon) which complicate the use of DRS and PAS for quantitative work. 10-25 In this paper, we have carried out a systematic comparison of the quantitative abilities of the two tech¬niques, as applied to the silica-kaolin mixtures, with par¬ticular attention to the saturation behavior of several bands with different absorption coefficients. In particular, we show that a weaker band for silica at 1875 cm-1 is suitable for quantitative purposes, and that quantitative accuracy is higher in DRS than in PAS. Details of this work are given below."