固相萃取-TXRF测定高冰镍中的贵金属  

Determination of Noble Metals in High Grade Matte Nickel by TXRF with Solid Phase Extraction

作　　者：韩晓锋[1] 王丽[1] 吕建刚[1] 陈伟[1] 徐淑华 田宇紘[1] 邬旭然[1] 

机构地区：[1]烟台大学化学化工学院

出　　处：《光谱实验室》2012年第5期3181-3184,共4页Chinese Journal of Spectroscopy Laboratory

基　　金：国家自然科学基金(21045005)

摘　　要：制备了以Dowex1-X10阴离子交换树脂为填料的固相萃取小柱,建立了固相萃取、全反射X射线荧光分析法(TXRF)测定高冰镍中微量贵金属钯、铱、铂和金含量的新方法,解决了复杂体系中微量贵金属检测前的分离富集难的问题。在0.5mol/L盐酸体系中,TXRF测定高冰镍中钯、铱、铂和金的相对标准偏差(RSD)均小于3.4%,其仪器检出限分别为0.015、0.011、0.013μg/mL和0.015μg/mL,方法检出限分别为0.050、0.036、0.043μg/g和0.050μg/g。实际样品的测定结果与ICP-MS基本一致。用TXRF可以同时、快速地测定高冰镍中的贵金属,样品测定结果可靠。The solid phase extraction cartridges were prepared with Dowex1-X10 anion exchange resin as filler,a new method for determination trace noble metals（Pd,Ir,Pt and Au） in high grade matte nickel by solid phase extraction and total reflection X-ray fluorescence spectrometry（TXRF） was established,and the problem that hard separation and enrichment before detection of trace noble metals in complex system was solved.RSDs of Pd,Ir,Pt and Au in high grade matte nickel that was determined by TRXF were all less than 3.4% in 0.5mol/L hydrochloric acid system,detection limits of instrument were respectively 0.015μg/mL（Pd）,0.011μg/mL（Ir）,0.013μg/mL（Pt）and 0.015μg/mL（Au）,and the detection limits of method were e 0.050μg/g（Pd）,0.036μg/g（Ir）,0.043 μg/g（Pt）and 0.050μg/g（Au）,respectively.The results of actual samples were essentially in agreement with the results of ICP-MS.TXRF can be applied to rapid and simultaneous determination of noble metals in high grade matte nickel with satisfactory results.

关 键 词：全反射X射线荧光分析 Dowex1-X10树脂 固相萃取 高冰镍 贵金属 

分 类 号：O657.34[理学—分析化学]