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出 处:《分析试验室》2014年第7期787-790,共4页Chinese Journal of Analysis Laboratory
基 金:国家质检总局项目(2012IK043);宁波市自然科学基金项目(2012A610150)资助
摘 要: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。In cool plasma mode,^63Cu was used as an internal standard,and a method for the determination of elements in pure copper and its wire with single point laser ablation inductively coupled plasma mass spectrometry was investigated.Experimental parameters were optimized.The results from different diameter samples were provided,the zinc signal became smaller with decrease of the diameter,and the selenium signal became bigger with reduction of the diameter.The fractionation factors of Cd,Sb,Pb and Bi were about 0.80,so there was fractionation effect.Matrix effect was investigated through element calibration curves fitted by different matrix CRMs,and the correlation coefficients of Mn,Ni,Zn,Pb and Bi were largerthan 0.95,matrix effect was not obvious,but for other elements there was matrix effect.A method was proposed for the direct determination of elements P,Mn,Fe,Ni,Zn,As,Se,Ag,Cd,Sn,Sb,Pb and Bi in pure copper and its wire,but sulfur could not be analyzed,and iron could not be analyzed with m/z 56,either.Good agreement was achieved between the found levels and the certified values.Except low content manganese,RSDs(n = 5) were between 2.1 and 15.5 percent.
关 键 词:激光剥蚀 电感耦合等离子体质谱法 纯铜 铜丝
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