Analysis of zirconium-based alloys by glow discharge mass spectrometry

Glow discharge mass spectrometric (GDMS) analysis of zirconium-based alloys has been studied by using a VG 9000 instrument. Disk samples were dry-poli shed with 120-grit zirconium oxide endless-paper and preliminary exposed to glow discharge for 1.8 ks in the discharge cell. Optimum glow discharge co nditions and the most suitable size of tantalum front mask were examined ta ke the advance of analytical precision into consideration. The relative sen sitivity factor (RSF) of each analyzing element was evaluated from the anal ytical values of thirteen standard reference materials: JAERI CRMs Z1 simil ar to 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 similar to 1239, relative standard deviation (RSD) of repetitive five measurements for each analyzing element was compared with those of obtaine d by the X-ray fluorescence spectrometry using theoretical alpha coefficien ts. RSD of GDMS analytical value change a little against the varying of ana lyzing 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%.