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测定高锰试样(如高锰炉渣、焊剂、锰矿等)中铝、钙、镁时,锰的干扰特别严重。必须进行彻底的分离。常用的方法有氨-过硫酸铵法,氨-溴水法,硝酸-氯酸钾法及离子交换法等等。但是这些方法对于锰的分离除非反复进行多次,否则总难完全,近年来用铜试剂(DDTC)分离锰比较盛行,但是,它在pH3时不能沉淀锰,在pH5～6也只能使少于1毫克的锰得到分离。此时铝亦水解沉淀,不能联测。本文提出在pH3的微酸性试液中加入邻菲罗啉-硫氰酸钠混合溶液(以下简写为Phen-NaCNS),与锰生成Mn·Phen_2·CNS_2沉淀。试验说明:高至100毫克锰也能完全分离。且不吸附铝、钙、镁。同时,
The determination of high manganese samples (such as high manganese slag, flux, manganese ore, etc.) of aluminum, calcium, magnesium, manganese interference is particularly serious. Must be completely separated. Ammonia - ammonium persulfate method, ammonia - bromine water method, nitric acid - potassium chlorate method and ion exchange method and so on. However, the separation of manganese from these methods is not always complete unless manganese is repeatedly separated many times. In recent years, the separation of manganese by copper reagent (DDTC) is relatively prevalent. However, manganese can not precipitate manganese at pH 3, 1 mg of manganese was separated. At this time, aluminum also hydrolyzed sediment, can not be combined test. In this paper, a solution of phenanthroline-sodium thiocyanate (abbreviated as Phen-NaCNS) was added into slightly acidic test solution of pH3 to generate Mn · Phen2 · CNS2 precipitate with manganese. Test description: Up to 100 mg of manganese can also be completely separated. And does not absorb aluminum, calcium, magnesium. Simultaneously,