Abstract:
Gadolinium fluoride is the main raw material for the production of metallic gadolinium and gadolinium iron. The content of impurities in gadolinium fluoride will directly affect performance of products. Therefore, it is important to determine the content of impurity elements efficiently and accurately. In this study, an analysis method for the determination of trace impurity elements in gadolinium fluoride by direct current glow discharge mass spectrometry(DC-GDMS) was developed. Tantalum strip and graphite powder were selected as the conductive medium and binder. The powder sample was filled in a square space with a side length of 5 mm surrounded by tantalum strip and embedded in graphite powder, realizing the direct solid analysis of gadolinium fluoride powder. The key parameters were obtained through systematical optimization: the discharge current was 30 mA; the discharge voltage was 1 200 V; the argon flow rate was 400 mL/min; the pre-sputtering time was 10 min. The contents of 70 impurity elements in high purity gadolinium fluoride were determined in seven replicates according to the experimental method. The relative standard deviations(RSD, n=7) of determination results of all detected elements were not more than 30%(when the content of impurities in the sample was greater than 1 μg/g, the RSD was not more than 10%). The results were verified and compared with inductively coupled plasma tandem mass spectrometry(ICP-MS/MS). The t-test results indicated that there was statistical consistency between two methods for the elements specified in product standard except for Ca and Si. The specimens obtained in this sample preparation method had good appearance regularity and high mechanical strength. The proposed method provided a reliable solution for the detection of impurity elements in rare earth fluorides.