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关于钒、钼和钨的纸上层析已有不少报导,但很少涉及铼。胡之德等亦曾研究了钒、钼和钨在TBP-HNO_3体系中的反相纸上层析,也未涉及铼的分离。鉴于硫氰化铵能与上述四种离子形成络合物,并用于萃取分离和比色测定。故我们采用TBP-HNO_3-NH_4CNS体系进行反相纸上层析,得到满意结果。实验部分 (一)试剂和仪器磷酸三丁酯(TBP):E.Merck厂分析试剂。使用时按下述方法提纯: 在一升圆底烧瓶中,加入100毫升TBP及500毫升0.4％氢氧化钠水溶液,然后通入水蒸气蒸馏,直至蒸出200毫升蒸馏液为止。分出烧瓶中的TBP层,用蒸馏水洗至中性。测其折射率为1.42240~(25)。
Paper on vanadium, molybdenum and tungsten paper has been reported, but rarely involved rhenium. Hu Dede et al. Also studied the reverse phase paper chromatography of vanadium, molybdenum and tungsten in the TBP-HNO 3 system and did not deal with the separation of rhenium. Since ammonium thiocyanate can form complexes with the above four ions and is used for extraction and colorimetric determination. Therefore, we use TBP-HNO_3-NH_4CNS system for reverse phase paper chromatography to obtain satisfactory results. Experimental Part (I) Reagents and Instruments Tributyl phosphate (TBP): E. Merck plant analytical reagent. When used, purify as follows: In a one-liter round bottom flask, add 100 ml of TBP and 500 ml of a 0.4% aqueous solution of sodium hydroxide, and then steam distillation until 200 ml of distillate is distilled off. Separate the TBP layer from the flask and wash until neutral with distilled water. The refractive index measured 1.42240 ~ (25).