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方法基于3.8——4.3NH_2SO_4介质中,用乙酸乙酯萃取硅钼黄与主体铂和钯分离,经还原为硅钼蓝后的有机相颜色不稳定,部分进入水相,加入正丁醇做稳定剂,以含有抗坏血酸的硫酸联胺和二氧化锡还原,颜色很稳定。 1.主要试剂:钼酸钠溶液(5％):5g钼酸钠溶于23ml水中,滴加1:3H_2SO_4至pH2-3,放置15分钟,加20ml 1:3H_2SO_4,用乙酸乙酯萃取提纯后水相放入聚四氟乙烯烧杯中,蒸发除去乙酸乙酯,用水稀至100ml;硫酸联胺溶液:取100ml硫酸联胺饱和溶液(用0.5NH_2SO_4配制),加1—1.5g
Method Based on the 3.8--4.3NH_2SO_4 medium, the molybdenum silicate yellow was extracted with ethyl acetate and separated from the host platinum and palladium. The organic phase after being reduced to molybdenum blue was unstable in color, partially into the aqueous phase, adding n-butanol to stabilize The agent, reduced with ascorbic acid, hydrazine sulfate and tin dioxide, the color is very stable. 1. The main reagent: sodium molybdate solution (5%): 5g sodium molybdate dissolved in 23ml of water, the dropwise addition of 1: 3H_2SO_4 to pH2-3, for 15 minutes, add 20ml 1: 3H_2SO_4, extracted with ethyl acetate purification The aqueous phase was placed in a Teflon beaker, evaporated to remove ethyl acetate, dilute to 100ml with water; Hydrazine sulfate solution: Take 100ml saturated solution of hydrazine sulfate (formulated with 0.5NH 2 SO 4), add 1-1.5g