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1.邻-硝基苯亚磺酸在0.4N盐酸溶液中与锆离子生成淡黄色絮状沉淀。沉淀不溶于水或0.1N的盐酸,具有恒定的组成ZrO(C_6H_4NO_2SO_2)_2。在110—120℃烘干后可直接 称重,也可以灼烧成ZrO_2后称重。 2.在实验条件下,除锆外只有钍离子与试剂生成沉淀,四价钛、锡离子含量低(<5毫克)时不干扰,含量大时有共沉淀现象。 3.有钍存在时,可以先用草酸分离钍,用高锰酸钾破坏滤液中的草酸,再用邻-硝基苯亚磺酸测定锆。 4.与苯亚磺酸一样,Fe~(+3)、Ce~(+3)、Mn~(+2)、UO_2~(+2)、Al_(+3)等存在无干扰。 5.邻-硝基苯亚磺酸的分析性能比苯亚磺酸好,邻位硝基的存在起了决定性的作用。
1. O-nitrobenzenesulfinic acid in 0.4N hydrochloric acid solution with zirconium ions generated yellowish flocculent precipitate. The precipitate is insoluble in water or 0.1 N hydrochloric acid and has a constant composition of ZrO (C_6H_4NO_2SO_2) _2. After drying at 110-120 ℃ can be directly weighed, can also be weighted into ZrO_2 after burning. 2. Under experimental conditions, except zirconium, only thorium ion and reagent generate precipitation, tetravalent titanium, tin ion content is low (<5 mg) does not interfere with the large amount of co-precipitation phenomenon. 3. Thorium exists, you can first use of oxalic acid separation of thorium, with potassium permanganate destruction of oxalic acid in the filtrate, and then o-nitrobenzene sulfinic acid determination of zirconium. The same as benzene sulfinic acid, Fe ~ (+3), Ce ~ (+3), Mn ~ (+2), UO_2 ~ (+2), Al _ (+3) and so there is no interference. The o-nitrobenzenesulfinic acid has better analytical performance than benzenesulfinic acid, and the presence of o-nitro group plays a decisive role.