对甲酰氨基乙酸偶氮氯膦的纯化和结构的研究

Studies on purification and structure of new chromogenic reagent p-hippuric acid chlorophosphonazo for the determination of total rare earths

以正戊醇为萃取剂去杂质,用盐酸酸化水相,得沉淀。用稀酸洗涤,干燥,得纯对甲酰氨基乙酸偶氨氯膦。用无水乙醇:三乙醇胺:氨水=10:4:5为展开剂,于硅胶 H 板上薄层色谱提纯对甲酰氨基乙酸偶氮氯膦(p-HACPA)。比移值(R_f)等于0.771。还对 p-HACPA 进行了元素分析、红外光谱测定、核磁共振光谱及热失重分析测定,据此推断了试剂的结构。

n-Amyl alcohol was used as an extractive agentto remove impurities in p-hippuric acid chloro-phosphonazo(p-HACPA),when the aqueousphase was acidified,p-HACPA was precipitatedwhich was then filtered,washed with dilute HClsolution and dried under infra-red lamp.Usingethyl alcohol/triethanolamine/ammonia(28%)(V/V,10:4:5)as the developing solvent chromatogra-phic separation of pure p-HACPA was achievedon silica gel H plate.The R_f value is 0.771.Elemental analysis,IR,NMR and thermal gravi-merry were used for p-HACPA to determine itsstructure.