Determination of Trace Nickel in Bi-Based Superconductor Powder by Inductively Coupled Plasma Atomic Emission Spectroscopy after Separation with Anion Exchange Resin and Extraction with Methylbenzene
FAN Li-xin1, LI Jian-qiang1*, FAN Hui-li1, SUN Jian-ling1, ZHANG Xia1, BAO Rui2, LU Qing1, WANG Jie1
1. Department of Chemistry, University of Science and Technology Beijing, Beijing 100083, China 2. Innova Superconductor Technology Co. Ltd., Beijing 100176, China
Abstract：A new method for the determination of trace nickel in superconductor powder by ICP-AES was proposed. The instrument parameters were optimized, and the matrix effects as well as the method of eliminating interferences were also studied systemically. The results showed that matrix interference in the superconductor powder was serious when the amount of matrix increased, and the repeatability as well as the accuracy was poor, so it was necessary to used separation and preconcentration to improve the accuracy and precision. In this experiment, Ni-diacetyl dioxime complexes were enriched by toluene extraction in alkaline condition after eliminating the interference of major element Bi and partial Pb, Sr, Ca and Cu by eluting with anion exchange resin, then the Ni-complexes were back extracted by diluted hydrochloric acid. The enrichment conditions were investigated in detail and the recovery rate of Ni was higher than 95%. Under the optimal condition, an artificial sample was analysed, the result showed that the found values were identical with reference values, and the RSD and detection limit were 1.9% and 0.19 μg·g-1, respectively. The method has been applied to the determination of trace nickel in Bi-based superconductor powder samples with satisfactory results.
Key words：Nickel;ICP-AES;Superconductor powder;Extraction with methylbenzene;Anion exchange resin
范丽新1，李建强1*，范慧俐1，孙建伶1，张 霞1，包 蕊2，陆 青1，王 杰1 . 阴离子交换树脂分离甲苯萃取ICP-AES测定铋系超导粉中的痕量镍[J]. 光谱学与光谱分析, 2011, 31(12): 3375-3378.
FAN Li-xin1, LI Jian-qiang1*, FAN Hui-li1, SUN Jian-ling1, ZHANG Xia1, BAO Rui2, LU Qing1, WANG Jie1 . Determination of Trace Nickel in Bi-Based Superconductor Powder by Inductively Coupled Plasma Atomic Emission Spectroscopy after Separation with Anion Exchange Resin and Extraction with Methylbenzene. SPECTROSCOPY AND SPECTRAL ANALYSIS, 2011, 31(12): 3375-3378.
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