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Abstract
ECHA classified TiO2 particles with an aerodynamic diameter ≤10 μm as carcinogen. Although the OELV for TiO2 is still related to inhalable particles in many jurisdictions, NIOSH recommended a REL of 2.4 mg/m3 for fine TiO2, and 0.3 mg/m3 for ultrafine TiO2. The latter implies the development of a more robust method for measuring TiO2 in workplace air. X-ray diffraction (XRD) is a powerful laboratory method for quantifying crystalline matter and is frequently used to measure respirable crystalline silica in workplaces. Rutile and anatase powders were obtained from a commercial vendor and a size fraction smaller than 10 µm was separated from these powders and used to prepare a calibration series in a calm-air dust chamber. The methodology for quantifying the rutile or anatase is performed as described in ISO 16258-1:2015 for measuring respirable crystalline silica. The limit of detection and quantification (LOD/LOQ) were for rutile 0.8/1.4 µg and anatase 0.6/1.1 µg, respectively. From these measurements, we conclude that direct on filter XRD is a powerful method for analyzing respirable TiO2 samples. Further validation of the XRD method was performed by comparing the results of 177 respirable personal samples collected on 25 mm MCE filters using Casella-HD cyclone samplers at nine TiO2 production plants with ICP-MS data gained from the same samples. Excellent correlations were obtained between the XRD and ICP-MS data for each sampling site but observed consistent site-dependent deviations explained by differences in crystallinity of the TiO2 phases and the presence of titanium-containing minerals other than rutile and anatase.