氯化钡沉淀+ICP-OES法测定工业硫酸中砷含量

Determination of arsenic in industrial sulphuric acid by barium chloride precipitation and ICP-OES

研究了利用氯化钡饱和溶液除去硫酸溶液中的硫酸根,再用电感耦合等离子体发射光谱仪测定工业硫酸中砷含量的方法。探讨了砷元素常用分析谱线的干扰情况及酸度效应对砷含量测定结果的影响,通过试验验证了方法的可靠性。试验结果表明,向制备的硫酸溶液中加入饱和氯化钡溶液沉淀除去硫酸根,有利于消除硫酸基体对ICP-OES测定结果的影响,砷的加标回收率为99.6%~101.5%,平行测定的相对标准偏差小于5%,与原子荧光光度法、砷斑法的测定结果无明显差异。

A method for the determination of arsenic in industrial sulphuric acid by inductively coupled plasma emission spectrometry after the removal of sulfate radical from sulphuric acid solution with barium chloride saturated solution is studied.The interference of commonly used analytical spectral lines of arsenic element and the influence of acidity effect on the determination results of arsenic content are discussed,and the reliability of the method is verified through tests.The test results show that adding saturated barium chloride solution to the prepared sulphuric acid solution to precipitate and remove sulfate radical is conducive to eliminating the influence of sulphuric acid matrix on the ICP-OES determination results.The recovery rate of arsenic spiking is 99.6%-101.5%,the relative standard deviation of parallel determination is less than 5%,and there is no significant difference between the determination results of atomic fluorescence spectrometry and arsenic spot method.