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This study examined a sample-preparation procedure in the glow-discharge mass analysis of yttria-stabilized zirconia (YSZ). We investigated a procedure for mixing it with high-purity gallium to guarantee the electrical conductivity. Several chips of single-crystal specimens were placed in the center of a homemade PTFE mold, embedded with 6 g of molten gallium (Ga), and then cooled and solidified. Three samples were subjected to an evaluation of the reproducibility in repetitive IBR measurements. Although the IBR of Ga to Zr varied with a difference in the respective occupation rate in the discharge area, the variation was less than 2% in RSD. Furthermore, the relative errors among three samples were less than 2% in Y and Hf, the main components, and less than 10% in trace impurities. Therefore, this method was proved to be applicable as a sample-preparation procedure. Moreover, we studied spectrum interference caused by the matrix and discharge gas, conducted a detailed analysis of composite molecular ions, and determined the optimal isotope for the measurement.

Sample-Preparation Method for the Analysis of Yttria-Stabilized Zirconia by Glow-Discharge Mass Spectrometry