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A study to assess the performance of an “X-ray powder diffraction with Rietveld” approach for measuring the crystalline and amorphous components of inhalable dust collected on aerosol sampling filters

  • P. Stacey (a1) (a2)


This work was undertaken in preparation for a survey to assess the exposure of carpenters to hazardous dust working in construction. Inhalable dust, in this industry, was expected to contain both crystalline mineral and amorphous phases (wood dust). The Rietveld method was applied to provide a simultaneous multicomponent analysis. To assess its performance, mixtures of aerosolised calcite, gypsum, quartz, kaolinite, and wood dust were collected onto quartz fibre filters (n = 41) using the Button inhalable sampler. Results obtained using Rietveld were compared with loaded mass and those from external standard calibrations. The measured content of a component in 14 samples was used as an internal standard by Rietveld to determine amorphous content (wood). The performance of the Rietveld and external standard methods was similar. The 95% confidence interval for the absolute differences between the two methods was 15%. Only one relative difference of more than 15% had a mass loading >0.5 mg. An approach for assessing the limits of detection with relative intensity ratios was applied and gave comparable values with the usual method using calibration coefficients from the external standard method. Rietveld is therefore a potentially useful multicomponent method for the measurement of dust aerosol to help better understand workers' exposures.


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Belsky, A., Hellenbrandt, M., Karen, V. L., and Luksch, P. (2002). “New developments in the Inorganic Crystal Structure Database (ICSD): accessibility in support of materials research and design,” Acta Crystallogr. B 58, 364369.
Bish, D. L., and Post, J. E. (1993). “Quantitative mineralogical analysis using the Rietveld full-pattern fitting method,” Am. Mineral., 78, 932940.
CEN (1993). EN 481 Workplace Atmospheres – Size Fraction Definitions for Measurement of Airborne Particles (European Committee for Standardisation, Brussels, Belgium).
Degen, T., Sadki, M., Bron, E., König, U., and Nénert, G. (2014). “The HighScore suite,” Powder Diffr. 29, S13S18.
Hellenbrandt, M. (2004). “The Inorganic Crystal Structure Database (ICSD) – present and future,” Crystallogr. Rev. 10, 1722.
Hill, R. J., and Howard, C. J. (1987). “Quantitative phase analysis from neutron powder diffraction data using the Rietveld method,” J. Appl. Crystallogr. 20, 467474.
Hillier, S. (2009). “Quantitative analysis of clay and other minerals in sandstones by X-Ray powder diffraction (XRPD),” in Clay Mineral Cements in Sandstones, edited by Worden, R. H. and Morad, S. (Wiley Online Library, Hoboken, NJ), pp. 213251.
HSE (2014). Methods for the Determination of Hazardous Substances, MDHS 101/2 Crystalline silica in respirable airborne dust, Direct On-Filter Analyses by Infrared Spectroscopy and X-Ray Diffraction., Health and Safety Executive (HSE), Norwich, United Kingdom, Crown.
Hubbard, C. R., and Snyder, R. L. (2013). “RIR – measurement and use in quantitative XRD,” Powder Diffr. 3, 7477.
ICDD (2018). PDF-4+ 2019 (Database), International Centre for Diffraction Data, Newtown Square, PA, USA.
ISO (2015). 16258- 1. Workplace Air – Analysis of Respirable Crystalline Silica Using X-Ray Diffraction. Part 1. Direct-on-Filter Method (British Standards Institution, Chiswick, London).
Jancsek-Turóczi, B., Hoffer, A., Nyírő-Kósa, I., and Gelencsér, A. (2013). “Sampling and characterization of resuspended and respirable road dust,” J. Aerosol Sci. 65, 6976.
Martin, J., Beauparlant, M., Lesage, J., and Van Tra, H. (2012). “Development of a quantification method for quartz in various bulk materials by X-ray diffraction and the Rietveld method,” Powder Diffr. 27, 1219.
Mecchia, M., Pretorius, C., Stacey, P., Mattenklott, M., and Incocciati, E. (2013). X-Ray Absorption Effect in Aerosol Samples Collected on Filter Media, West Conshohocken, PA, United States of America, ASTM International.
NIOSH (2003). Silica, Crystalline, by XRD (filter redeposition) Method 7500, 4th Edition. Manual of Analytical Methods. Department of Health and Human Services, National Institute for Occupational Safety and Health.
Pickard, K. J., Walker, R. F., and West, N. G. (1985). “A comparison of X-ray diffraction and infra-red spectrophotometric methods for the analysis of a-quartz in airborne dusts,” Ann. Occup. Hyg. 29, 149167.
Rietveld, H. (1969). “A profile refinement method for nuclear and magnetic structures,” J. Appl. Crystallogr. 2, 6571.
Santos, M. D., Matos, J. R., Carvalho, L. R. F., Sant'agostino, L. M., and Korn, M. (2013). “An X-ray diffraction study of filters used for atmospheric aerosol sampling,” Powder Diffr. 11, 230234.

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A study to assess the performance of an “X-ray powder diffraction with Rietveld” approach for measuring the crystalline and amorphous components of inhalable dust collected on aerosol sampling filters

  • P. Stacey (a1) (a2)


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