Abstract
Glow discharge mass spectrometric (GDMS) analysis of zirconium-based alloys has been studied by using a VG 9000 instrument. Disk samples were dry-polished with 120-grit zirconium oxide endless-paper and preliminary exposed to glow discharge for 1.8 ks in the discharge cell. Optimum glow discharge conditions and the most suitable size of tantalum front mask were examined take the advance of analytical precision into consideration. The relative sensitivity factor (RSF) of each analyzing element was evaluated from the analytical values of thirteen standard reference materials: JAERI CRMs Z1∼Z16. As an example, the average RSF obtained were 1.612 for iron and 1.332 for hafnium. For the analysis of the zirconium-based alloys NIST SRMs 1234∼1239, relative standard deviation (RSD) of repetitive five measurements for each analyzing element was compared with those of obtained by the X-ray fluorescence spectrometry using theoretical alpha coefficients. RSD of GDMS analytical value change a little against the varying of analyzing element concentration, and it was within 10% for each trace impurity at mass ppm level. The GDMS analytical value of hafnium in those SRMs was in good agreement with the certified value and RSD of that was within 5%.
