Enrichment of Trace Iron with Activated Carbon in Bi-Based Superconductor Powder and Determination by Inductively Coupled Plasma Atomic Emission Spectroscopy
HUANG Wen-jie1, LI Jian-qiang1*, FAN Hui-li1, FAN Li-xin1, BAO Rui2, ZHANG Xia1, WANG Jie1, LU Qing1
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 determination of trace iron 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 was serious when the amount of matrix increased, and the repeatability was poor, so it was necessary that separation and preconcentration were used to improve the accuracy and precision. In the experiment, complex was formed with Fe and phenanthroline after the matrix elements Bi and Cu were masked by triethanolamine in an appropriate acidity condition. Then the complex was quantitatively adsorbed by activated carbon, and desorbed by 1∶1 HNO3. The enrichment conditions were investigated in detail. Under the optimal condition, an artificial sample was analysed, and the result was identical with reference values, with the RSD and detection limit being 2.42% and 0.033 μg·g-1, respectively. The method was applied for the determination of trace iron in Bi-based superconductor powder samples with satisfactory results, in which the recoveries experiment was performed with the recovery coefficient falling in the range of 95.6% to 98.0%.
Key words：Iron;Enrichment with activated carbon;ICP-AES;Superconductor powder
黄文杰1，李建强1*，范慧俐1，范丽新1，包 蕊2，张 霞1，王 杰1，陆 青1 . 活性炭富集电感耦合等离子体原子发射光谱测定铋系超导粉中痕量铁[J]. 光谱学与光谱分析, 2012, 32(02): 514-518.
HUANG Wen-jie1, LI Jian-qiang1*, FAN Hui-li1, FAN Li-xin1, BAO Rui2, ZHANG Xia1, WANG Jie1, LU Qing1 . Enrichment of Trace Iron with Activated Carbon in Bi-Based Superconductor Powder and Determination by Inductively Coupled Plasma Atomic Emission Spectroscopy . SPECTROSCOPY AND SPECTRAL ANALYSIS, 2012, 32(02): 514-518.
