Analysis of crystalline phases in airborne particulates by grazing incidence X-ray diffractometry

Abstract

Amounts of crystalline phases of airborne particulates collected on a silicon wafer (10 × 10 mm) using a high-volume air sampler were analyzed by grazing incidence X-ray diffractometry (GIXD). Airborne particulates were classified into five size ranges (1.09–10.5 µm) with a cascade impactor attached on the sampling ports of the high-volume air sampler. GIXD was used throughout this analysis to obtain better sensitivity for small amounts of airborne particulates on the silicon wafer. Calibration standards on the silicon wafer for the diffractometric determination were prepared by the suspension droplet method of the crystalline standards dispersed in cyclohexane. Analytical lines were (020) for gypsum, (101) for quartz, (104) for calcite, (200) for halite, and (110) for sal ammoniac. The sample and the calibrating standards were heated at 350 °C for 2 h to avoid mutual interference with gypsum (041 and 21) when calcite and halite were determined. The GIXD method enables us to determine 0.23–13.2 µg of gypsum, quartz, calcite, halite and sal ammoniac in 0.110–0.233 mg of airborne particulates on the silicon wafer.