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Simultaneous determination of ultra-trace Au, Pt, Pd, Ru, Rh, Os and Ir in geochemical samples by KED-ICP-MS combined with Sb-Cu fire assay and microwave digestion
Microchemical Journal ( IF 4.9 ) Pub Date : 2020-11-01 , DOI: 10.1016/j.microc.2020.105197 Wenshan Ni , Hongli Zhang , Xiangju Mao , Lu Liu , Xiaorui Guo , Fang Xiao , Xiaofei Gao
Microchemical Journal ( IF 4.9 ) Pub Date : 2020-11-01 , DOI: 10.1016/j.microc.2020.105197 Wenshan Ni , Hongli Zhang , Xiangju Mao , Lu Liu , Xiaorui Guo , Fang Xiao , Xiaofei Gao
Abstract Simultaneous and accurate determination of ultra-trace Au and platinum group elements (Pt, Pd, Ru, Rh, Os and Ir) in geochemical samples is always a difficult task for their low abundance and uneven distribution. In this work, a new method for the simultaneous determination of ultra-trace Au, Pt, Pd, Ru, Rh, Os and Ir was proposed. Novel antimony-copper (Sb-Cu) fire assay was used as pre-concentration method and Au, Pt, Pd, Ru, Rh, Os and Ir were separated from the sample matrix and concentrated into Sb-Cu alloy particle. Details in this process were fully discussed and a coating agent was introduced to obtain the complete enrichment of noble metal elements; Then a microwave digestion method was used for the dissolution of Sb-Cu alloy particle. Both occurrence state and volatile behavior of Os element in this stage were studied. Ascorbic acid was used innovatively in this work and a fixed volatile proportion of 22.3% with RSD of 3.52% for Os element was found; Finally, based on the correction coefficient of Os standard solution and mathematical correction of 206Pb2+ on 103Rh+, kinetic energy discrimination collision cell-inductively coupled plasma mass spectrometry was successfully used for the simultaneous determination of ultra-trace Au, Pt, Pd, Ru, Rh, Os and Ir elements. The analytical performance of this method was studied and the detection limits of Au, Pt, Pd, Ru, Rh, Os and Ir were ranged from 0.005 ng g−1 to 0.031 ng g−1. The precisions that were evaluated within five replicated results of GBW07293 were ranged from 4.83% to 11.0%. Further, the feasibility and accuracy of the proposed method were verified by comparing the determination results of Chinese national reference materials with their certified values. This method is sensitive and stable. Importantly, this work provides a reliable and efficient determination method for multiple noble metal elements, which is of great significance in batches of geochemical survey samples analysis.
更新日期：2020-11-01
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