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采用冷等离子体模式,以63Cu为内标,研究了单点激光剥蚀电感耦合等离子体质谱法(LA-ICP-MS)测定纯铜及铜丝中各元素的方法。优化了仪器参数;给出了样品直径对结果的影响,锌的信号随着直径的减小而减弱,硒的信号随着直径的减小而增强;研究了分馏效应,Cd,Sb,Pb,Bi分馏因子(FI)在0.80左右有分馏效应;采用不同系列铜标准物质制作了校准曲线以考察基体效应,Mn,Ni,Zn,Pb,Bi的线性相关系数大于0.99,基体效应不明显,其它元素有基体效应。建立了测定纯铜及铜丝中P,Mn,Fe,Ni,Zn,As,Se,Ag,Cd,Sn,Sb,Pb,Bi等元素的直接测定方法,但硫不能测定,也不能用56Fe作为铁的检测同位素,标准物质的测定值与认定值基本吻合,除Mn含量低外,其它元素的RSD(n=5)在2.1%~16%之间。
Using cold plasma mode and 63Cu as internal standard, the method of single element laser ablation inductively coupled plasma mass spectrometry (LA-ICP-MS) to determine each element in pure copper and copper wire was studied. The parameters of the instrument were optimized. The effect of sample diameter on the results was also given. The signal of zinc decreased with the decrease of diameter and the signal of selenium increased with the decrease of diameter. The effects of fractionation, Cd, Sb, Pb, Bi fractionation factor (FI) fractionation effect around 0.80; using different series of copper standard material calibration curve was prepared to investigate the matrix effect, Mn, Ni, Zn, Pb, Bi linear correlation coefficient greater than 0.99, the matrix effect is not obvious, the other Elements have a matrix effect. A direct method for the determination of P, Mn, Fe, Ni, Zn, As, Se, Ag, Cd, Sn, Sb, Pb and Bi in pure copper and copper wire has been established. However, sulfur can not be measured and 56Fe As the detection isotope of iron, the measured value of the standard substance basically agrees with the certified value. The RSD (n = 5) of other elements except for the low content of Mn is between 2.1% and 16%.