电感耦合等离子体原子发射光谱法测定铪合金中锆

使用硝酸和氢氟酸溶解样品,以Zr 327.305 nm为分析谱线,建立了电感耦合等离子体原子发射光谱法(ICP-AES)测定铪合金中锆含量的分析方法。结果表明:铪质量浓度在100 μg/mL以下时,对锆的测定结果影响不显著,不需要使用基体匹配法绘制校准曲线;由于酸度对锆的测定结果有影响,待测试液与标准溶液系列的酸度应该保持一致,酸度大约为1.0 mol/L。锆的质量浓度在0.2～5.0 μg/mL范围内与发射强度呈线性,校准曲线的线性回归方程为y=39 966 x+176,相关系数r=0.999 7。方法中锆的检出限为0.001 5 μg/mL。实验方法用于铪合金样品中锆的分析,测定结果的相对标准偏差(RSD,n=6)小于1%,回收率为99%;同时与X射线荧光光谱法的测定结果进行比对,两种方法测定结果基本一致。

Determination of zirconium in hafnium alloy by inductively coupled plasma atomic emission spectrometry

The sample was dissolved by nitric acid and hydrofluoric acid. The Zr 327.305 nm was selected as analytical line. The analysis method of zirconium content in hafnium alloy by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established. The results showed that the determination results of zirconium were insignificantly affected by hafnium when the mass concentration of hafnium was lower than 100 μg/mL. The matrix matching method was not required to prepare the calibration curve. Since the acidity had influence on the determination results of zirconium, the acidity of testing solution should be consistent with the standard solution series. In the experiment, the acidity was about 1.0 mol/L. When the mass concentration of zirconium was in range of 0.2-5.0 μg/mL, the linear regression equation of calibration curve was y=39 966 x+176 with correlation coefficient of r=0.999 7. The detection limit of zirconium was 0.001 5 μg/mL. The proposed method was applied to the determination of zirconium in hafnium alloy. The relative standard deviation (RSD, n=6) was less than 1%, and the recovery was 99%. Meanwhile, the proposed method was compared with X-ray fluorescence spectrometry. It was found that the determination results of two methods were basically consistent.