Determination of Zirconium Dioxide in Zirconium Dioxide Material by X-Ray Fluorescence Spectrometry after Sample Preparation with Powder Tableting

Zirconium dioxide in zirconium dioxide material was determined by the title method, and effects of sample amount and spectral line overlapping interference on the determination of zirconium dioxide were studied. The samples were ground into powder with particle size less than 75 μm, and heated at 105 ℃ for 2 h. Boric acid (2 g) was placed into the pressure chamber of tabletting machine as the substrate, flattened, and covered evenly with not less than 2.00 g of sample powder, and the sample tablet with outer diameter of 40 mm was pressed under 410 kN for 20 s, and detected according to the working conditions of the instrument. As found by results, when the sample amount was 1.00 g, the sample thickness was lower than the critical thickness (167 nm), and the radiation surface thickness of the sample was uneven, and the determined value of zirconium dioxide was low; when the sample amount was not less than 2.00 g, the density of the analytical layer was decreased, and the determined value of zirconium dioxide was decreased, and the effect could be corrected by the normalization method. Zirconium in the zirconium dioxide sample could produce strong spectral line overlapping interference at the analytical spectral lines of molybdenum, cerium and neodymium, and the interference could be eliminated by adjusting the spectral line overlapping correction coefficients of molybdenum, cerium and neodymium. The proposed method was used for the analysis of 4 actual samples and zirconium dioxide standard substance GBW 06602, and RSDs (n=5) of the determined values were not more than 0.15%. Compared with the results found by X-ray fluorescence spectrometry with fusion sample preparation, the determined values of the 2 methods were basically consistent, and the determined values of the standard substance were within the uncertainty range of the certified value.