电感耦合等离子体质谱法测定高纯镍板中砷锡锑铅铋

摘要

采用10 mL硝酸(1+1)低温加热至沸溶解0.1000 g试样,在优化仪器参数的基础上,通过选择合适的同位素以避免质谱干扰和采用标准加入法绘制校准曲线以消除基体效应,建立了电感耦合等离子体质谱法( ICP-MS)测定高纯镍板中砷、锡、锑、铅、铋的方法。各元素校准曲线的相关系数为0.9992~0.9999,方法检出限为0.009~0.047μg/g。方法应用于高纯镍板实际样品分析,测得结果的相对标准偏差( RSD, n=9)为2.4%~5.4%,加标回收率为95%~106%。方法测定高纯镍板实际样品的结果与原子吸收光谱法( AAS)相吻合。%0. 100 0 g of sample was dissolved with 10 mL of nitric acid (1+1) by heating from low temperature to boiling. Based on the optimization of instrumental parameters, the mass spectrometry interference was avoided by selecting proper isotope, and the calibration curve was plotted by standard addition method to eliminate the matrix effect. Consequently, a determination method of arsenic, tin, antimony, lead and bismuth in high-purity nickel plate was established by inductively coupled plasma mass spectrometry ( ICP-MS ) . The correlation coefficient of calibration curve for each element was between 0. 999 2 and 0. 999 9 . The detection limit of method was 0. 009-0. 047 μg/g. The proposed method was applied to the analysis of high purity nickel plate actual sample. The rela-tive standard deviation (RSD, n=9) was 2. 4%-5. 4%, and the recoveries were between 95% and 106%. The determination results of high purity nickel plate actual sample were consistent with those obtained by atomic absorp-tion spectrometry ( AAS) .