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建立了电解分离-电感耦合等离子体质谱法测定纯铜中17种杂质元素(Be,Mg,Al,P,Ti,Cr,Mn,Co,Ni,As,Se,Zr,Cd,Sn,Sb,Te和Pb)的方法。通过控制电流分离基体铜,大于99%的铜沉积至阴极,各杂质元素的回收率大于90%。研究了电解后电解液的酸效应、残余铜的影响和基体效应。结果表明,选用合适的内标能有效的控制信号漂移和降低基体效应,采用八极杆碰撞池技术消除多原子离子对部分元素的干扰。除P和Al外,各元素的检出限在1.0×10-3～1.0×10-2mg/kg之间。运用该方法测定纯铜标准物质GBW02141,测定值与参考值吻合,回收率在85%～110%之间,精密度在1.8%～8.5%之间。
A total of 17 impurity elements (Be, Mg, Al, P, Ti, Cr, Mn, Co, Ni, As, Se, Zr, Cd, Sn and Sb) in pure copper were determined by electrolytic separation and inductively coupled plasma mass spectrometry Te and Pb). By controlling the galvanic separation of the matrix copper, more than 99% of the copper is deposited to the cathode with a recovery of more than 90% for each impurity element. The acid effect, residual copper effect and matrix effect of the electrolyzed electrolyte were studied. The results show that the selection of suitable internal standard can effectively control the signal drift and reduce the matrix effect, and the octopole collision cell technology can eliminate the interference of some elements from polyatomic ions. In addition to P and Al, the detection limit of each element is between 1.0 × 10-3 ~ 1.0 × 10-2mg / kg. The pure copper standard GBW02141 was determined by this method. The measured values were in good agreement with the reference values. The recoveries ranged from 85% to 110% and the precision was between 1.8% and 8.5%.