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Ann. occup. Hyg., Vol. 46, No. 4, pp. 409-421, 2002
© 2002 British Occupational Hygiene Society
Published by Oxford University Press

Comparison by X-ray Diffraction and Infrared Spectroscopy of Two Samples of {alpha} Quartz with the NIST SRM 1878a {alpha} Quartz

E. KAUFFER*, J. C. MOULUT, A. MASSON, J. C. PROTOIS and M. GRZEBYK

INRS, Departement Metrologie de Polluants, Laboratoire d’Analyses Physiques, Avenue de Bourgogne, BP 27, F-54501 Vandoeuvre les Nancy, France

Received 17 May 2001; in final form 24 December 2001

The aim of this study was to compare the X-ray diffraction and infrared spectrophotometric patterns of two samples of {alpha} quartz (QUIN1 and QUIN2) with that of NIST SRM 1878a {alpha} quartz certified 100% crystalline. As it is known that the intensity diffracted and the absorbance per mass unit for a given type of {alpha} quartz depend on its particle size, this factor was taken into account. To do this, different types of {alpha} quartz were sampled on filters using a Dorr-Oliver cyclone to select particle size. Variation in the flow rate of the cyclone in the range 1.2–2.8 l/min allowed the volume median diameter of the sampled particles to be varied. For the four strongest diffraction lines it was observed that the intensity per mass unit increased with the volume median diameter of the particles. For infrared spectrophotometry for analytical band wavelengths close to 12.5 µm, it was observed that the absorbance per mass unit decreased as particle size increased. The opposite effect was noted for analytical band wavelengths >14.4 µm. Compared with SRM 1878a {alpha} quartz, certified 100% crystalline, the purity of QUIN1 {alpha} quartz was 93.1% (confidence interval 92.4–93.8%) when measured by X-ray diffraction and 91.5% (confidence interval 90.1–92.9%) when measured by infrared spectrophotometry. In the case of QUIN2 {alpha} quartz the purity was globally lower.

Keywords: crystallinity; infrared spectrophotometry; particle size; quartz; X-ray diffraction


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