HG-AFS DETERMINATION OF TRACE AMOUNTS OF ANTIMONY IN HIGH-PURITY LEAD

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%.