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本文研究了在氟化铵溶液中用二氧化锰作载体共沉淀微量稀土元素的方法,经研究确定能使10～600微克稀土氧化物定量共沉淀,并能与铁、锆、铀、铍及铝等分离。分离与测定稀土的主要步骤为:将含稀土的溶液调节为约100毫升,酸度为0.01～0.1N,加入10～40毫升4％氟化铵溶液,5毫升0.5M硫酸锰溶液,用氨水调节溶液酸度至甲基橙变为橙色,加入2～5毫升0.05M高锰酸钾溶液进行沉淀,加热至沸后趁热过滤。沉淀经灼烧后用盐酸及过氧化氢溶解并蒸干,残渣用0.01N盐酸溶液溶解,用偶氮胂Ⅲ光度测定。
In this paper, the method of coprecipitating trace rare earth elements with ammonium manganese oxide as carrier in ammonium fluoride solution was studied. It was confirmed by the research that quantitative co-precipitation of rare earth oxides (10-600 micrograms) and iron, zirconium, uranium, beryllium and Aluminum and other separation. The main steps for the separation and determination of rare earths are as follows: the rare earth-containing solution is adjusted to about 100 ml, the acidity is 0.01 to 0.1 N, 10 to 40 ml of 4% ammonium fluoride solution and 5 ml of 0.5 M manganese sulfate solution are added, The solution acidity to orange methyl orange, add 2 to 5 ml 0.05M potassium permanganate solution precipitation, heated to boiling filtered hot. The precipitate was calcined with hydrochloric acid and hydrogen peroxide dissolved and evaporated to dryness, the residue was dissolved with 0.01N hydrochloric acid solution, with arsine Ⅲ luminosity determination.