Evaluation of Diffuse Reflection Infrared Spectrometry for End-of-Shift Measurement of α-quartz in Coal Dust Samples.

The inhalation of toxic substances is a major threat to the health of miners, and dust containing respirable crystalline silica (α-quartz) is of particular concern, due to the recent rise in cases of coal workers' pneumoconiosis and silicosis in some U.S. mining regions. Currently, there is no field-portable instrument that can measure airborne α-quartz and give miners timely feedback on their exposure. The U.S. National Institute for Occupational Safety and Health (NIOSH) is therefore conducting studies to investigate technologies capable of end-of-shift or real-time measurement of airborne quartz. The present study focuses on the potential application of Fourier transform infrared (FT-IR) spectrometry conducted in the diffuse reflection (DR) mode as a technique for measuring α-quartz in respirable mine dust. A DR accessory was used to analyze lab-generated respirable samples of Min-U-Sil 5 (which contains more than 90% α-quartz) and coal dust, at mass loadings in the ranges of 100-600 µg and 600-5300 µg, respectively. The dust samples were deposited onto three different types of filters, borosilicate fiberglass, nylon, and polyvinyl chloride (PVC). The reflectance, R, was calculated by the ratio of a blank filter and a filter with deposited mine dust. Results suggest that for coal and pure quartz dusts deposited on 37 mm PVC filters, measurements of -log R correlate linearly with known amounts of quartz on filters, with R(2) values of approximately 0.99 and 0.94, respectively, for samples loaded up to ∼4000 µg. Additional tests were conducted to measure quartz in coal dusts deposited onto the borosilicate fiberglass and nylon filter media used in the NIOSH-developed Personal Dust Monitor (PDM). The nylon filter was shown to be amenable to DR analysis, but quantification of quartz is more accurate when the filter is "free," as opposed to being mounted in the PDM filter holder. The borosilicate fiberglass filters were shown to produce excessive interference, making quartz quantification impossible. It was concluded that, while the DR/FT-IR method is potentially useful for on-filter measurement of quartz in dust samples, the use of PVC filters produced the most accurate results.

Deposition Uniformity of Coal Dust on Filters and Its Effect on the Accuracy of FTIR Analyses for Silica.

Miners are exposed to silica-bearing dust which can lead to silicosis, a potentially fatal lung disease. Currently, airborne silica is measured by collecting filter samples and sending them to a laboratory for analysis. Since this may take weeks, a field method is needed to inform decisions aimed at reducing exposures. This study investigates a field-portable Fourier transform infrared (FTIR) method for end-of-shift (EOS) measurement of silica on filter samples. Since the method entails localized analyses, spatial uniformity of dust deposition can affect accuracy and repeatability. The study, therefore, assesses the influence of radial deposition uniformity on the accuracy of the method. Using laboratory-generated Minusil and coal dusts and three different types of sampling systems, multiple sets of filter samples were prepared. All samples were collected in pairs to create parallel sets for training and validation. Silica was measured by FTIR at nine locations across the face of each filter and the data analyzed using a multiple regression analysis technique that compared various models for predicting silica mass on the filters using different numbers of "analysis shots." It was shown that deposition uniformity is independent of particle type (kaolin vs. silica), which suggests the role of aerodynamic separation is negligible. Results also reflected the correlation between the location and number of shots versus the predictive accuracy of the models. The coefficient of variation (CV) for the models when predicting mass of validation samples was 4%-51% depending on the number of points analyzed and the type of sampler used, which affected the uniformity of radial deposition on the filters. It was shown that using a single shot at the center of the filter yielded predictivity adequate for a field method, (93% return, CV approximately 15%) for samples collected with 3-piece cassettes.

Evaluating portable infrared spectrometers for measuring the silica content of coal dust.

Miners face a variety of respiratory hazards while on the job, including exposure to silica dust which can lead to silicosis, a potentially fatal lung disease. Currently, field-collected filter samples of silica are sent for laboratory analysis and the results take weeks to be reported. Since the mining workplace is constantly moving into new and often different geological strata with changing silica levels, more timely data on silica levels in mining workplaces could help reduce exposures. Improvements in infrared (IR) spectroscopy open the prospect for end-of-shift silica measurements at mine sites. Two field-portable IR spectrometers were evaluated for their ability to quantify the mass of silica on filter samples loaded with known amounts of either silica or silica-bearing coal dust (silica content ranging from 10-200 µg/filter). Analyses included a scheme to correct for the presence of kaolin, which is a confounder for IR analysis of silica. IR measurements of the samples were compared to parallel measurements derived using the laboratory-based U.S. Mine Safety and Health Administration P7 analytical method. Linear correlations between Fourier transform infrared (FTIR) and P7 data yielded slopes in the range of 0.90-0.97 with minimal bias. Data from a variable filter array spectrometer did not correlate as well, mainly due to poor wavelength resolution compared to the FTIR instrument. This work has shown that FTIR spectrometry has the potential to reasonably estimate the silica exposure of miners if employed in an end-of-shift method.