电感耦合等离子体原子发射光谱法测定铍中11种杂质元素

铍中铝、钴、铬、铜、铁、镁、锰、镍、铅、硅和锌等11种杂质元素含量的准确测定,是判定铍材是否合格的重要指标。目前,上述杂质元素的测定标准为GJB 2513A—2008《铍化学分析方法》,方法分别采用光度法和原子吸收光谱法对各元素逐一测定,测定周期很长。试验采用盐酸-硝酸溶解样品,选择Al 308.215nm、Co 230.786nm、Cr 284.325nm、Cu 324.754nm、Fe 261.187nm、Mg 285.213nm、Mn 260.569nm、Ni 221.647nm、Pb 182.205nm、Si 250.690nm、Zn 213.856nm为分析谱线,采用标准加入法(MSA)配制标准溶液系列消除基体效应的影响,使用电感耦合等离子体原子发射光谱法(ICP-AES)测定铝、钴、铬、铜、铁、镁、锰、镍、铅、硅和锌,从而建立了铍中11种元素的测定方法。各待测元素校准曲线的线性相关系数均大于0.9995;各元素的定量限为0.001%~0.002%。实验方法用于测定铍样中铝、钴、铬、铜、铁、镁、锰、镍、铅、硅和锌,结果的相对标准偏差(RSD,n=10)为0.63%~8.6%,回收率为90%~110%。按照实验方法测定铍样中上述11种元素,测定结果与采用GJB 2513A—2008测定的结果吻合。

Determination of eleven impurity elements in beryllium by inductively coupled plasma atomic emission spectrometry

The accurate determination of 11 impurity elements (including aluminum, cobalt, chromium, copper, iron, magnesium, manganese, nickel, lead, silicon and zinc) in beryllium is an important index to judge whether the beryllium material is qualified. At present, the standard for the determination of above impurity elements is GJB 2513A-2008 . The elements are determined one-by-one by photometry and atomic absorption spectrometry with very long measurement period. The sample was dissolved in hydrochloric acid-nitric acid system. Al 308.215nm, Co 230.786nm, Cr 284.325nm, Cu 324.754nm, Fe 261.187nm, Mg 285.213nm, Mn 260.569nm, Ni 221.647nm, Pb 182.205nm, Si 250.690nm and Zn 213.856nm were selected as the analytical lines. The standard solution series were prepared by the method of standard addition (MSA) to eliminate the influence of matrix effect. The determination method of 11 elements (including aluminum, cobalt, chromium, copper, iron, magnesium, manganese, nickel, lead, silicon and zinc) in beryllium by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established. The linear correlation coefficients of calibration curves for elements were all higher than 0.9995. The limit of quantification was in range of 0.001%-0.002%. The experimental method was applied for the determination of aluminum, cobalt, chromium, copper, iron, magnesium, manganese, nickel, lead, silicon and zinc in beryllium sample. The relative standard deviations (RSD, n=10) of results were between 0.63% and 8.6%. The recoveries were between 90% and 110%. The contents of 11 elements in beryllium sample were determined according to the experimental method, and the found results were consistent with those obtained by GJB 2513A-2008.