ICP-AES法测定合成甲基三氧化Re过程中馏出液和残渣中的Re  

Determination of Rhenium in Raffinate and Residue from Synthesis of Methyltrioxorhenium by ICP-AES

作　　者：刘宁[1] 张世涛 李俊[1] 岳爽[3] 臧树良[3] 

机构地区：[1]辽宁大学化学学院,辽宁沈阳110036 [2]辽宁省地质矿产研究院,辽宁沈阳110032 [3]辽宁大学稀散元素化学研究所,辽宁沈阳110036

出　　处：《光谱学与光谱分析》2008年第7期1650-1652,共3页Spectroscopy and Spectral Analysis

基　　金：国家自然科学基金项目(20271024)资助

摘　　要：甲基三氧化Re是一种新型高效的过渡金属有机催化剂，它具有许多优良的催化性能，也可与路易斯碱形成多种配合物，因此，提高其合成产率已成为国内外研究的热点。合成过程中馏出液和残渣中Re的含量是衡量合成产率的重要标准，也是改进合成条件的基础。Re的测定通常采用分光光度法，但该法存在灵敏度较低、干扰多、操作不便等因素。电感耦合等离子体发射光谱法，具有灵敏度高，分析速度快，稳定性好且能同时测定多种元素等特点，被广泛应用于各行业的分析测试中。文章研究了用ICP-AES测定合成甲基三氧化Re过程中馏出液和残渣中Re的方法，选取了最佳工作条件，检出限为0．01mg·L^-1，方法的精密度在0．48％～1．12％之间，加标回收实验的回收率在97．2％～104％之间，体系中存在的光谱干扰可以不计，并将实验数据与分光光度法进行比较，该法简便、快速、准确，结果令人满意。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.

关 键 词：电感耦合等离子体发射光谱法 甲基三氧化Re 馏出液 残渣 RE 

分 类 号：O657.3[理学—分析化学]