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直流辉光放电质谱法测定氟化钆粉末中痕量元素

Determination of trace elements in gadolinium fluoride powder by direct current glow discharge mass spectrometry

  • 摘要: 氟化钆作为生产金属钆和钆铁的主要原料,杂质元素含量直接影响产品的性能,高效、准确地测定其杂质元素的含量至关重要。本文建立直流辉光放电质谱法(DC-GDMS)测定氟化钆中痕量杂质元素的分析方法。采用钽条结合石墨粉作为导电剂和粘结剂,将粉末样品填充于钽条围成的5 mm×5 mm方形区域并镶嵌石墨粉中,实现氟化钆粉末的直接固体分析。经系统优化获得关键参数:放电电流30 mA、放电电压1 200 V、氩气流速400 mL/min、预溅射时间10 min。按照实验方法对高纯氟化钆中70种元素进行7次重复测定,所有检出元素测定结果的相对标准偏差(RSD,n=7)不大于30%(含量大于1μg/g元素,RSD不大于10%);基于ICP-MS/MS方法比对及t检验,除Ca、Si外,产品标准中规定元素方法间具有统计学一致性。该制样法所得样片兼具形貌规整性与高机械强度,为稀土氟化物杂质检测提供可靠解决方案。

     

    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.

     

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