| 光谱学与光谱分析 |
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| Determination of Rhenium in Raffinate and Residue from Synthesis of Methyltrioxorhenium by ICP-AES |
| LIU Ning1,ZHANG Shi-tao2,LI Jun1,YUE Shuang3,ZANG Shu-liang3* |
1. College of Chemistry，Liaoning University，Shenyang 110036，China
2. The Geology and Mineral Institute of Liaoning Province，Shenyang 110032，China
3. Institute of Rare-Scattered Elements of Liaoning University, Shenyang 110036, China |
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Abstract Methyltrioxorhenium is a novel and efficient organometallic catalyst. It has exhibited amazingly high activities in a variety of organic reactions, and can form compounds with Lewis base. Thus, the improvement of its synthesis rate has become a pop topic all over the world. The content of rhenium in raffinate and residue from the synthesis of methyltrioxorhenium is an important standard for the evaluation of synthesis rate and a foundation for the optimization of synthesis condition. UV spectrophotometry is the standard technique for the determination of rhenium. However, this method presents several disadvantanges such as low sensitivity, high interferences, and hard handling. Inductive coupled plasma-atomic emission spectrometry has many advantages such as high precision, rapid analysis speed and good stability, and can determine multi-elements simultaneously. It is widely used in determination in every walk of life. An ICP-AES method for determination of the content of rhenium in raffinate and residue from the synthesis of methyltrioxorhenium was used. The working parameters were optimized. The detection limit was 0.01 mg·L-1. RSD was in the range of 0.48%-1.12% and recoveries in the range from 97.2%-104% were obtained. The spectrum interference can be neglected. Compared with spectrophotometer, the proposed method was proved to be simple, rapid and accurate, and the result was satisfactory.
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Received: 2007-10-18
Accepted: 2008-01-08
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Corresponding Authors:
ZANG Shu-liang
E-mail: slzang@lnu.edu.cn
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