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Arsenic and antimony speciation analysis in copper electrolyte by liquid chromatography coupled to hydride generation atomic fluorescence spectrometry (HPLC-HG-AFS)
Analytical Methods ( IF 3.1 ) Pub Date : 2020-03-21 , DOI: 10.1039/d0ay00148a
Ana Isabel González de las Torres 1, 2, 3, 4 , Michael S. Moats 5, 6, 7, 8 , Guillermo Ríos 4, 9, 10 , Ana Rodríguez Almansa 4, 9, 10 , Daniel Sánchez-Rodas 1, 2, 3, 4, 11
Affiliation  

A novel method based on high performance liquid chromatography (HPLC) coupled to hydride generation-atomic fluorescence spectrometry (HG-AFS) is proposed for the determination of arsenic and antimony redox couples (As(III), As(V), Sb(III) and Sb(V)) in copper electrolyte samples, which are characterized by extreme acidity and high metallic content (Cu and Ni in the g L−1 range). The determination of the oxidation states of As and Sb in sulfuric acid based electrolyte is of critical importance as these elements can form slimes that affect copper quality. The proposed speciation method was successfully applied to industrial electrolyte samples, indicating that As(V) and Sb(III) were the predominant species in the electrolyte. The results were validated by comparison with total arsenic and antimony content determined with ICP-OES. The stability of arsenic and antimony species in the samples prior to analysis was also studied during a period of 28 days considering aqueous dilution, acidification with HCl and different storage temperature (4 °C, 25 °C or 65 °C). The dilution and the acidification with HCl caused partial oxidation of Sb(III) to Sb(V), while the As species were not affected. Undiluted copper electrolyte samples showed stability periods of 14 and 28 days for Sb and As, respectively, independently of the storage temperature.

中文翻译:

液相色谱-氢化物发生原子荧光光谱法(HPLC-HG-AFS)分析铜电解液中的砷和锑形态

提出了一种基于高效液相色谱(HPLC)结合氢化物发生原子荧光光谱法(HG-AFS)的新方法,用于测定砷和锑氧化还原对(As(III),As(V),Sb(III))和Sb(V))在铜电解液样品中,其特征在于极高的酸度和高金属含量(Cu和Ni在g L -1范围内)。确定硫酸基电解质中As和Sb的氧化态至关重要,因为这些元素会形成影响铜质的粘泥。所提出的形态分析方法已成功应用于工业电解质样品,表明As(V)和Sb(III)是电解质中的主要物质。通过与ICP-OES测定的总砷和锑含量的比较,验证了结果。还考虑了水稀释,盐酸酸化和不同的存储温度(4°C,25°C或65°C),在28天的时间内对样品中砷和锑物种的稳定性进行了研究。稀释和用HCl酸化导致Sb(III)部分氧化为Sb(V),而As种类不受影响。未稀释的铜电解质样品显示出Sb和As的稳定期分别为14天和28天,与存储温度无关。
更新日期:2020-04-24
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