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%.