辉光放电质谱法测定高纯材料中痕量硫杂质

Determination of Trace Sulfur Impurity in High-purity Materials by Glow Discharge Mass Spectrometry

准确测定并控制材料中杂质元素含量是发挥高纯材料性能不可或缺的环节。辉光放电质谱法(GDMS)是准确、快速、高灵敏分析高纯材料中痕量及超痕量硫的理想方法。对GDMS分析高纯铜和镍基高温合金中痕量硫的质谱干扰进行了考察,优化了放电电流和放电电压,采用多种标准物质对硫的相对灵敏度因子(RSF)进行了校准和验证,RSF校准后的测定值与标样参考值的偏差为-2.4%和-2.6%。与二次离子质谱法(SIMS)进行实际样品的分析结果比对,两种方法测定结果的相对偏差为-3.45%和-4.67%,验证了GDMS定量分析结果的准确性和可靠性。

Accurate determination and control of impurity elements in materials is the key to ensure the performance of high-purity materials.Glow discharge mass spectrometry(GDMS)is an ideal method for accurate,rapid and sensitive analysis of trace and ultra-trace sulfur in high-purity materials.The spectral interferences of sulfur in high-purity copper and nickel base super alloy were discussed in detail.The discharge parameters of GDMS,including discharge current and discharge voltage,were optimized.The relative sensitivity factor(RSF)of sulfur was calibrated and validated by a variety of standard reference materials.The relative deviations between the determination results by the calibrated RSF and the reference values of standard reference materials were-2.4%and-2.6%.The accuracy and reliability of GDMS were verified by comparing the results with secondary ion mass spectrometry(SIMS),the relative deviations of two real samples were-3.45%and-4.67%,respectively.