717阴离子交换树脂富集-电感耦合等离子体质谱法测定地质样品中痕量金铂钯

来源期刊：冶金分析2011年第4期

论文作者：李丹 王锝 李彪

文章页码：14 - 19

关键词：金； 铂； 钯； 电感耦合等离子体质谱法； 阴离子交换树脂

Key words：gold； platinum； palladium； inductively coupled plasma mass spectrometry； anion exchange resin

摘    要：研究了717型阴离子交换树脂对地质样品中痕量金、铂、钯的吸附性能及分离条件。采用水浴加热,HCl+王水的方式溶解样品,溶出的干扰元素只有Mo对Pd的测定造成干扰,采用数学公式校正可消除此干扰。在5%的HCl介质中,洗脱剂流速为2 mL/min时,金、铂、钯的富集效果最佳,回收率接近100%。经对共存离子影响的校正,用电感耦合等离子体质谱法测定国家一级标准物质,其结果较认定值不超差。方法检出限为Pd 0.6 ng/mL,Pt 0.5 ng/mL,Au 0.7ng/mL。随机选取5个地质样品用本法进行分析,同时与硫镍试金-ICP-MS法进行比较,结果一致。两组结果经双样本方差F检验,无显著性差异。

Abstract: The adsorption property and separation conditions of 717 anion exchange resin to trace gold,platinum and palladium in geological samples were studied.The sample was dissolved with HCl+ aqua regia under heating in water bath.Only Mo in dissolved elements had interference with the determination of Pd,which could be eliminated using mathematical formula correction.When the flow rate of eluent was 2 mL/min,the enrichment effects of gold,platinum and palladium in 5% HCl medium reached its best,and the recoveries were close to 100%.After correcting the influence of coexisting ions,the national first-class certified reference materials were determined by inductively coupled plasma mass spectrometry,and the difference between determination results and certified values was satisfactory.The detection limit of method were 0.6 ng/mL,0.5 ng/mL and 0.7 ng/mL for Pd,Pt and Au,respectively.Five random geological samples were analyzed by this method in comparison with NiS fire assay-ICP-MS method.The determination results were consistent.The results of two methods were checked by double sample’s variance F test,and there was no significant difference.