混合吸附剂分离富集-电感耦合等离子体质谱法测定地质样品中铂钯金  

Determination of Platinum,Palladium and Gold in Geological Samples by Bomb-inductively Coupled Plasma-Mass Spectrometry with Concentrate and Extraction by Mixed Adsorbent

作　　者：王琳[1,2] 唐志中[1,2] 来新泽[1,2] 连文莉[1,2] 胡家祯[1,2] 周岚[3] 

机构地区：[1]河南省岩石矿物测试中心,河南郑州450012 [2]国土资源部贵金属分析与勘查技术重点实验室,河南郑州450012 [3]青海省地质矿产测试应用中心,青海西宁810008

出　　处：《岩矿测试》2013年第3期420-426,共7页Rock and Mineral Analysis

基　　金：国土资源部公益性行业科研专项(201211016-3)

摘　　要：贵金属分析应用火试金法分离富集时,试金配料复杂、耗时较长,分析成本相对较高,空白较难控制。本文建立了采用过氧化氢-盐酸湿法分解样品,电感耦合等离子体质谱同时测定地质样品中Pt、Pd、Au的分析方法。在10%的盐酸介质中,以LSC-400巯基树脂和活性炭为混合吸附剂,采用动态吸附方式对样品中的Pt、Pd、Au分离富集,用Lu作内标元素,195Pt、197Au、108Pd为待测同位素消除了非谱线干扰和谱线干扰,三元素的回收率均大于96.4%。方法检出限(3σ):Pt为0.06 ng/g,Pd为0.08 ng/g,Au为0.12 ng/g,优于火试金等其他分离富集方法的检出限。应用于测定国家标准物质,Pt、Pd、Au的测定结果与标准值相符,12次测定的相对标准偏差均小于16.1%,满足区域地球化学调查样品的分析要求。该方法操作简便、成本低廉,提高了分析速度,有效地降低了测试过程的空白值。Fire assay separation enrichment technology has been applied to precious metals analysis, however, its ingredients are complex, time-consuming, analysis costs are relatively high and blank controls are more difficult. A new method was set up such as the samples were dissolved with H2O2-HCl before Pt, Pd and Au were determined by Inductively Coupled Plasma-Mass Spectrometry （ICP-MS）. In 10% hydrochloric acid solution, LSC-400 mercapto resin and activated carbon were mixed as the adsorbent. Pt, Pd and Au in the sample solution were separated and enriched by using dynamic adsorption. Lu was selected as the internal standard element to eliminate non-spectral interference and spectrum interference along with tracers of ^195pt, ^197Au and ^108pd. The recovery rates of each elemenl were more than 96.4%. The detection limits were 0.06 ng/g for Pt, 0.08 ng/g for Pd and 0.12 ng/g for Au. Compared with the detection limits, this established method was better than the fire assaying method and other separation and enrichment methods. The method has been applied to the determination of these elements in Nalional Standard Materials for PGEs and results were in agreement with the certified values. The relative standard deviations （RSD, n = 12） was less than 16.1%. The method is simple, low cost and greatly improves the speed of analysis, and effectively reduces the blanks of the chemical processing.

关 键 词：地质样品 铂 钯 金 LCS-400巯基树脂 混合吸附剂 电感耦合等离子体质谱法 

分 类 号：O614.826[理学—无机化学] O614.823[理学—化学]