电感耦合等离子体原子发射光谱法测定硅锆合金中锆

以盐酸、氢氟酸、高氯酸和硝酸混合酸溶解,选择Zr 257.139nm为分析线,高纯铁基体匹配法绘制校准曲线消除基体效应的影响,采用电感耦合等离子体原子发射光谱法(ICP-AES)测定锆,从而建立了硅锆合金中高含量锆的测定方法。锆的质量分数为3.04%~30.42%时与其发射强度呈线性,校准曲线的线性相关系数为0.999 8;方法检出限为0.007%(质量分数)、测定下限为0.033%。按照实验方法测定钛合金样品和钛合金标准样品中锆,结果的相对标准偏差(RSD,n=6)不大于1.2%。实验方法用于测定3个硅锆合金样品中锆,结果与苦杏仁酸重量法测定结果一致。

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

The sample was dissolved with hydrochloric acid, hydrofluoric acid, perchloric acid and nitric acid. Zr 257.139 nm was selected as the analytical line. The influence of matrix effect was eliminated by preparing calibration curves using high purity iron matrix matching method. The determination method of high content zirconium in silicon-zirconium alloy by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established. The mass fraction of zirconium in range of 3.04%-30.42% was linear to the corresponding emission intensity. The linear correlation coefficient of calibration curve was 0.999 8. The detection limit was 0.007% (mass fraction), and the low limit of determination was 0.033%. The content of zirconium in actual sample and standard sample of silicon-zirconium alloy was determined according to the experimental method. The relative standard deviations (RSD, n=6) were less than 1.2%. The proposed method was applied to the determination of zirconium in three silicon-zirconium alloy samples, and the found results were consistent with those obtained by mandelic acid gravimetry.