电感耦合等离子体原子发射光谱(ICP-AES)法测定硅锆合金中的铝和钙

Determination of Aluminum and Calcium in Silicon Zirconium Alloy by Inductively Coupled Plasma Atomic Emission Spectrometry

通过硝酸、氢氟酸和盐酸分解试样，高氯酸冒烟驱走硅和氟，最后用盐酸溶解盐类，选择Al（396．152nm）、Ca（315．887nm）作为分析谱线，电感耦合等离子体原子发射光谱（ICP—AES）法测定硅锆合金中的铝和钙。研究了锆离子（0．3mg／mL）和铁离子（0．2mg／mL）共存体系中基体效应和光谱干扰对待测元素测定的影响。结果表明，该质量浓度的锆离子和铁离子对待测元素的测定结果不产生影响。铝和钙的质量浓度在10～50／ag／mL，其线性相关系数均不小于0．999，方法中铝和钙的检出限分别为0．009μg／mL和0．006μg／mL。按照实验方法测定硅锆合金中的铝和钙，结果的相对标准偏差（RSD，n=10）分别为0．85％和1．4％。方法适用，结果令人满意。

The samples were firstly digested with nitric acid, hydrofluoric acid and hydrochloric acid, and then fumed with perchloric acid so as to remove silicon and fluorine, and finally the salts were dissolved by hydrochloric acid. The analytical lines were selected as A1 396. 152 nm and Ca 315. 887 nm. The contents of aluminum and calcium in silicon zirconium alloy were determined by inductively coupled plasma atomic emission spectrometry （ICP-AES）. The influence of matrix interference and spectral interference on the determination were investigated in the coexistence system containing 0.3 mg/mL zirconium ion and 0.2 mg/mL iron ion. The results showed that the determination of A1 and Ca by zirconium ion and iron ion were not affected under the experimental conditions. The linear correlation coefficients were both less than 0. 999 when the concentrations of A1 and Ca were 10-50 μg/mL. The detection limits for A1 and Ca were 0. 009 μg/mL and 0. 006 μg/mL, respectively. The relative standard deviations （RSDs, n=10） for A1 and Ca were 0.85% and 1.4 %, respectively. The method is applicable with satisfactory results.