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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。
Methyltrioxide is a new and efficient transition metal organic catalyst, it has many excellent catalytic properties, but also with the Lewis base to form a variety of complexes, therefore, to improve the synthesis yield has become a hot research at home and abroad. The content of Re in the distillate and the residue during the synthesis is an important criterion for measuring the yield of synthesis and also the basis for improving the synthesis conditions. The determination of Re usually spectrophotometry, but the method has low sensitivity, interference, inconvenient operation and other factors. Inductively coupled plasma-atomic emission spectrometry has the characteristics of high sensitivity, fast analysis, good stability and simultaneous determination of various elements. It is widely used in the analysis and testing of various industries. In this paper, the method of determination of Re in distillate and residue in the process of synthesizing methyl trioxide by ICP-AES was studied. The optimum working conditions were selected with the detection limit of 0.01 mg · L-1 and the precision of the method was 0.48 % To 1.12%. The recoveries of spiked recovery experiments ranged from 97.2% to 104%. The spectral interference existed in the system could be neglected, and the experimental data were compared with spectrophotometry. The method was simple, rapid and accurate , The result is satisfactory.