基于高分辨电感耦合等离子体质谱法(HR-ICP-MS)的质谱干扰消除技术,对镍基单晶高温合金中36种痕量元素检测的质谱条件、基体干扰、质谱干扰与同位素选择进行了研究。取样品0.1000 g,用体积比为3∶1的盐酸-硝酸混合酸10 mL、氢氟酸1 mL溶解,用水定容至250 mL。通过复杂基体质谱干扰计算判定、共存元素干扰消除,确定了待测元素的同位素和分辨模式,将镍基单晶高温合金中痕量元素准确测定的元素种类确定为36种。采用标准加入法进行定量分析,36种痕量元素的检出限(3s)为0.004~6.000 μg·L^-1。方法用于分析国际标准物质,得到的测定值与认定值基本一致。方法用于镍基单晶高温合金样品分析,36种痕量元素的检出量为0.0000010%~0.018%。

Mass spectrometric conditions, matrix interference, mass spectrometric interference and isotope selection of 36 trace elements in nickel-based single crystal superalloy were studied by mass spectrometric interference elimination technique based on high-resolution inductively coupled plasma mass spectrometry (HR-ICP-MS). 0.1000 g of the sample was taken, and then dissolved in 10 mL of the mixed acid of hydrochloric acid and nitric acid at a volume ratio of 3∶1 and 1 mL of hydrofluoric acid. The volume of the solution was made up to 250 mL with water. The isotopes and resolution modes of the analysis elements were determined by the calculation and determination of the mass spectrometric interference in complex matrix, and the interference elimination of co-existing elements, and 36 trace elements in nickel-based single crystal superalloy had been accurately determined. Quantitative analysis was made by standard addition method, with detection limits (3s) of 36 trace elements in the range of 0.004-6.000 μg·L^-1. This method was applied to analysis of international reference materials, and the determined values obtained by this method were basically consistent with the certified values. This method has been applied to analysis of nickel-based single crystal superalloy samples, and the detection amounts were found in the range of 0.000 001 0%-0.018%.