Spectroscopy and Spectral Analysis, Volume. 31, Issue 12, 3375(2011)
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
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.
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FAN Li-xin, LI Jian-qiang, FAN Hui-li, SUN Jian-ling, ZHANG Xia, BAO Rui, LU Qing, WANG Jie. 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[J]. Spectroscopy and Spectral Analysis, 2011, 31(12): 3375
Received: Jan. 27, 2011
Accepted: --
Published Online: Jan. 5, 2012
The Author Email: Li-xin FAN (fanlx306@163.com)