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Determination of Trace Amount of Cobalt in a Steel Sample by Two-dimensional On-line Redox Derivatization Liquid Chromatography

机译:二维在线氧化还原衍生化色谱法测定钢样中痕量钴

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A two-dimensional on-line redox derivatization HPLC system was developed where “heart-cutting” chromatography, in conjunction with on-line redox derivatizaion, was used to isolate specific analytes in complex matrix samples. Cobalt in a stainless steel sample was used as a model analyte to evaluate the performance of the HPLC system developed. We adopted a small column packed with porous graphitic carbon (PGC) treated with hydrogen peroxide as an oxidation derivatization unit and two C_(18) silica columns which had adsorbed hexadecyltrimethylammonium ion as the first and second separation columns. After complexation of metal components with ethylenediaminetetraacetate (edta), the sample was directly submitted to the analysis by the HPLC system without any preseparation steps. In the first dimension separation cobalt was eluted as Co(II)-edta and was separated from trivalent metal complexes such as Fe(III) and Cr(III), while it was selectively oxidized to Co(III)-edta in the PGC column and then completely separated from the divalent metal complexes such as Ni(II) on the second column. A successful application of this method to accurate and precise determination of trace amount of cobalt in a stainless steel is demonstrated.
机译:开发了二维在线氧化还原衍生化HPLC系统,其中“心脏切割”色谱与在线氧化还原衍生化一起用于分离复杂基质样品中的特定分析物。不锈钢样品中的钴用作模型分析物,以评估开发的HPLC系统的性能。我们采用一个装有用过氧化氢处理过的多孔石墨碳(PGC)作为氧化衍生单元的小柱和两个吸附了十六烷基三甲基铵离子的C_(18)硅胶柱作为第一和第二分离柱。金属成分与乙二胺四乙酸盐(edta)络合后,样品无需任何分离步骤即可直接通过HPLC系统进行分析。在第一维分离中,钴被洗脱为Co(II)-edta,并从三价金属络合物(例如Fe(III)和Cr(III))中分离出来,而在PGC柱中它被选择性氧化为Co(III)-edta。然后在第二列上与二价金属络合物(例如Ni(II))完全分离。演示了该方法成功地用于精确,精确地确定不锈钢中痕量钴的应用。

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