研究了高纯铅中微量锑的氢化物-原子荧光光谱方法.考察了最佳测定条件、干扰的消除方法及酸度影响.结果表明,采用硝酸溶解样品,蒸至有硝酸铅析出后,加入盐酸酸度达20%时,基体铅以氯化铅形式沉淀,消除基体铅的影响,其它共存离子不干扰锑的测定.检出限(3σ)为0.37 μg·L-1,样品加标回收率在95.0%-101.4%之间,RSD为1.73%.

A method of hydride-generation atomic fluorescence spectrometry for the determination of trace amounts of antimony in high-purity lead was described.Instrumental and analytical conditions were optimized.The lead sample was dissolved in dilute nitric acid,and the sample solution was evaporated until the salt of lead nitrate separated.Conc.hydrochloric acid was added until its ratio to water in the solution attained to 1 to 4,to precipitate majority of lead(Ⅱ) as lead chloride form the solution in order to eliminate the matrix interference.No interferences were observed by the other co-existing ions.Detection limit (3σ) of this method was found to be 0.37 μg·L-1.RSD found by 6 repeated determinations was 1.73%.Recoveries tested by standard addition method gave values in the range from 95.0% to 101.4%.