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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。
A new method for the determination of trace amounts of palladium, iridium, platinum and gold in high iced nickel by solid-phase extraction and total reflection X-ray fluorescence analysis (TXRF) was established for the solid phase extraction column with Dowex1-X10 anion exchange resin as filler. , To solve the complex system before the detection of trace precious metals separation and enrichment difficult. The relative standard deviations (RSDs) of palladium, iridium, platinum and gold in high ice nickel were all less than 3.4% in the 0.5 mol / L hydrochloric acid system. The detection limits were 0.015, 0.011, 0.013 μg / mL and 0.015 μg / mL, the detection limits were 0.050, 0.036, 0.043μg / g and 0.050μg / g, respectively. The actual results of the determination of the sample and ICP-MS are basically the same. With TXRF, the precious metals in high iced nickel can be measured simultaneously and quickly, and the results of the sample determination are reliable.