| 光谱学与光谱分析 |
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| Separation with Ion Exchange Fiber Column and Determination of La, Nd, Eu and Gd in High Purity Ytterbium Oxide by ICP-AES |
| GONG Qi, CHEN Jie, JI Ri-wen, PAN Xue-zhen, WU Juan |
| College of Chemistry and Chemical Engineering, Guangxi University, Nanning 530004, China |
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Abstract In the present paper, trace La, Nd, Eu and Gd were separated and enriched with strong acid ion exchange fiber column from high purity Yb2O3, and then determined by Optima 5 300 DV ICP-AES. The ion exchange fiber’s breakthrough capacity for Yb was 134 mg·g-1. The separation condition using 4.0 g fiber column was that after the test solution (pH=3.0) was fed into the ion exchange fiber column at 1.0 mL·min-1, the column was pre-leached by dilute nitric acid (pH=3.00) of 80 mL at 1.5 mL·min-1 at first, and then was eluted by 0.01 mol·L-1 ammonium EDTA (pH=5.00) at the same flow rate. The results showed that 10 mg Yb could reach the baseline separation with 0.100 μg of the four rare earth impurities, and after 100 mg Yb in feed solution had been separated, only 0.017 1 μg·mL-1 Yb remained in the impurities enriched effluent. When the concentration of Yb2O3 is less than 100 μg·mL-1 (87.8 μg·mL-1 Yb), the matrix interference from Yb on with determination of La, Nd, Eu and Gd can be neglected. The enrichment factors were 3.68×105 for La2O3, 4.20×105 for Nd2O3, 3.82×105 for Eu2O3, and 4.01×105 for Gd2O3, and the detection limits of the method were 0.005 0, 0.014, 0.001 8 and 0.008 2 pg·mL-1 for La2O3, Nd2O3, Eu2O3 and Gd2O3 respectively. The proposed method was applied to the analysis of 99.99% Yb2O3 with RSD (%, n=5) of 6.2, 5.9, 7.3 and 2.5 for La2O3, Nd2O3, Eu2O3 and Gd2O3 respectively, and the average recoveries of standard addition were 94.2%, 107%, 97.8% and 102% for La2O3, Nd2O3, Eu2O3 and Gd2O3 respectively. The calibration curve did not need matrix matching with Yb, and the analysis period was within 4 hour.
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Received: 2009-02-12
Accepted: 2009-05-16
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Corresponding Authors:
GONG Qi
E-mail: gongqi@gxu.edu.cn, gxugong@163.com
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