Consideration of Kaolinite Interference Correction for Quartz Measurements in Coal Mine Dust

Abstract

Kaolinite interferes with the infrared analysis of quartz. Improper correction can cause over- or underestimation of silica concentration. The standard sampling method for quartz in coal mine dust is size selective, and, since infrared spectrometry is sensitive to particle size, it is intuitively better to use the same size fractions for quantification of quartz and kaolinite. Standard infrared spectrometric methods for quartz measurement in coal mine dust correct interference from the kaolinite, but they do not specify a particle size for the material used for correction. This study compares calibration curves using as-received and respirable size fractions of nine different examples of kaolinite in the different correction methods from the National Institute for Occupational Safety and Health Manual of Analytical Methods (NMAM) 7603 and the Mine Safety and Health Administration (MSHA) P-7. Four kaolinites showed significant differences between calibration curves with as-received and respirable size fractions for NMAM 7603 and seven for MSHA P-7. The quartz mass measured in 48 samples spiked with respirable fraction silica and kaolinite ranged between 0.28 and 23% (NMAM 7603) and 0.18 and 26% (MSHA P-7) of the expected applied mass when the kaolinite interference was corrected with respirable size fraction kaolinite. This is termed “deviation,” not bias, because the applied mass is also subject to unknown variance. Generally, the deviations in the spiked samples are larger when corrected with the as-received size fraction of kaolinite than with the respirable size fraction. Results indicate that if a kaolinite correction with reference material of respirable size fraction is applied in current standard methods for quartz measurement in coal mine dust, the quartz result would be somewhat closer to the true exposure, although the actual mass difference would be small. Most kinds of kaolinite can be used for laboratory calibration, but preferably, the size fraction should be the same as the coal dust being collected.

Keywords:

• coal dust
• FTIR
• kaolinite
• NMAM 7603
• P-7
• quartz
• silica

ACKNOWLEDGMENT

Many thanks to Daniel Crane from the Occupational Safety and Health Administration and Mark Wesolow- ski from the MSHA for reviewing this work, and to an anonymous reviewer for several helpful suggestions.

The findings and conclusions in this report are those of the authors and do not necessarily represent the official position of the Centers for Disease Control and Prevention/the Agency for Toxic Substances and Disease Registry. This article not subject to U.S. copyright law.