高流速辉光放电质谱法测定镍基单晶高温合金中43种痕量元素

Determination of 43 Trace Elements in Nickel-Based Single Crystal Superalloy by Fast Flow-Glow Discharge Mass Spectrometry

基于高流速辉光放电质谱法(GDMS)的质谱干扰消除技术,对镍基单晶高温合金中43种痕量元素的质谱干扰与同位素选择进行了研究,用于高性能镍基单晶高温合金的纯净化水平评价。固体样品采用直接进样,通过复杂基体质谱干扰计算判定、共存元素干扰消除等方式,确定了待测元素的同位素和分辨率模式,通过相应标准物质对待测元素的相对灵敏度因子进行校正,采用高流速GDMS测定镍基单晶高温合金中43种痕量元素。结果表明,痕量元素的检出限(3s)为1.04×10^(-7)%~6.60×10^(-3)%,大部分元素的检出限达到0.1μg·g^(-1)级别;对内控标准物质DD6-6#测定6次,测定值的相对标准偏差为0.59%~13%。方法分析结果与不同分析方法对照、标准物质比对,结果吻合度高。

Mass spectrometry interference and isotope selection of 43 trace elements in nickel-based single crystal superalloy were studied based on fast flow-glow discharge mass spectrometry. This method was used to evaluate the purification level of high-performance nickel-based single crystal superalloy. The solid samples were injected directly. The isotopes and resolution modes of the analytical elements were determined by the calculation judgement of mass spectrum interference in complex matrix, and the interference elimination of the coexisting elements. The corresponding standard materials were used to correct the relative sensitivity factors of the analytical elements. The 43 trace elements of nickel-based single crystal superalloy were then determined by fast flow-glow discharge mass spectrometry. As shown by the results, the detection limits(3s) of the trace elements were in the range of 1.04×10^(-7)%-6.60×10^(-3)%, most of which reached 0.1 μg·g^(-1)level. The internal control standard material DD6-6# was determined 6 times, with RSDs of the determined values in the range of 0.59%-13%. The analytical results of this method were consistent with those of different analytical methods and standard materials.