Comparison of direct (X-ray diffraction and infrared spectrophotometry) and indirect (infrared spectrophotometry) methods for the analysis of alpha-quartz in airborne dusts.

In this study, the alpha-quartz contents measured by different analytical techniques (X-ray diffraction, direct method; and infrared spectrophotometry, direct and indirect methods) were compared. The analyses were carried out on filters sampled in an industrial setting by means of a Dorr-Oliver cyclone. To verify the methodology used, filters loaded with pure alpha-quartz were also analysed. By and large, the agreement between the two direct methods was close on average, but on the basis of a comparison of the individual results, considerable differences exist. In absolute value, the mean relative deviation between the two techniques was <25% in only 47.8% of the cases. The results obtained by the indirect method (infrared) were on average 13% lower than the results obtained by the two direct methods with a more important difference (23%) for samples where calcite was identified by X-ray diffraction in comparison with those where it was not (8%). This underestimation, which was not owing to dust losses during preparation, is probably explained by the elimination of organic compounds during dust calcinations or by the transformation of mineral compounds. The indirect method introduces additional sample handling operations with more risk of material loss. When the quantity of calcined material was <0.4 mg, the weighing operations necessary to correct any losses of material resulted in considerable variability. In terms of overall uncertainty, it would be better in this case not to carry out correction and to employ an operating mode favouring the recovery of a maximum of material while accepting a bias of about 5-7%.

Comparison by X-ray diffraction and infrared spectroscopy of two samples of alpha quartz with the NIST SRM 1878a alpha quartz.

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 micro m, 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 micro m. 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.

Exposure to metallic catalyst dust: manufacturing and handling of catalysts in the chemical industry.

The exposure of workers to metallic catalyst dust was assessed in manufacturing and reprocessing industries, and during catalyst handling in the chemical industry. The level of exposure was found to be generally low during the manufacturing and reprocessing activities taking place in permanent installations, and extremely variable during catalyst handling performed by workers of sub-contracting specialized firms. The difficulties in treating the occupational hygiene problems of these workers are pointed out.