氧化铝负载二苯基硫脲分离富集ICP-AES测定贵金属的研究

Determination of Trace Platinum, Palladium, Gold and Rhodium in Geological Samples by ICP-AES after Preconcentration by Diphenlthiourea Immobilized on Aluminum Oxide

报道了氧化铝负载二苯基硫脲分离富集ICP-AES法同时测定痕量Pt,Pd,Au和Rh的新方法,研究了影响分离富集的各种条件(溶液酸度、流速、试样体积、洗脱剂的种类和体积及其共存离子的影响等)对测定上述痕量元素回收率的影响。在优化的实验条件下本方法的检出限分别为Au 0.0085,Pd 0.022,Pt 0.015和Rh 0.022μg·g^(-1),相对标准偏差小于5.0％,样品加标回收率在95％～105％之间。本方法已成功地应用于地质样品中痕量Pt,Pd,Au和Rh的测定。

A method for the determination of Au, Pt, Pd and Rh by ICP-AES after preooncentration on a column containing diphenylthiourea immobilized on aluminum oxide was developed. The optimum acidity of solution, amount of adsorbent, elution solution, flow rate and volume of the samples were obtained for the elements studied. The effect of interfering ions on the recovery of the analytes was also investigated. Under the optimum measuring conditions, the recoveries were found to be between 95%-105%. The detection limits of Au, Pd, Pt and Rh was 0.008 5, 0.022, 0.015 and 0.022 mug.g(-1), respectively, and the relative standard deviation was lower than 5%. This procedure was applied to the determination of Au, Pd, Pt and Rh in geological samples.