高纯铝样品经盐酸(1+1)溶液微波消解,采用电感耦合等离子体质谱法测定所得样品溶液中钛、铁、铜、锌、镓、银、镉、铟和铅等杂质元素的含量。选择适当的待测元素的同位素克服了质谱干扰,定量加入50 μg·L-1铯和锗内标元素有效地校正了基体效应。选用碰撞室技术消除了多原子离子对部分被测元素的干扰。结果表明:方法的检出限(3s)在0.003~0.042 μg·L-1之间。高纯铝样品中9种元素测定结果的相对标准偏差(n=10)在2.9%~9.5%之间。方法用于精铝标准样品(R11C)的测定,结果与认定值基本相符。

The sample of high-purity aluminum was treated with HCl (1+1) solution by microwave assisted digestion, and the contents of Ti, Fe, Cu, Zn, Ga, Ag, Cd, In and Pb in the sample solution were determined by ICP-MS. Appropriate isotopes of the elements determined were selected to overcome the mass spectrometric interferences and definite amount (50 μg·L-1) of mixed internal standard of Cs and Ge was added to compensate the matrix effect. Interference of polyatomic ion effect to part of the determined elements was eliminated by adoption of the collision cell technique. Values of detection limits (3s) for the 9 elements were found in the range of 0.003-0.042 μg·L-1. Precision of the method was tested by analyzing a high-purity aluminum, values of RSD′s (n=10) found were ranged from 2.9% to 9.5%. The proposed method was applied to the determination of standard sample of pure aluminum, the results obtained were in consistency with the certified values.