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本试验证明用 CHCl_3萃取 Ni-丁二酮肟,镍量高达100毫克也能萃取完全.萃取前采用2克酒石酸钾钠络合铁铝等元素,0.2～0.4克盐酸羟胺将锰还原成低价以消除其干扰,0.5克硫代硫酸钠还原隐蔽铜,钻消耗丁二酮肟但不被三氯甲烷萃取,方法易于掌握,适用于矿样、合金中镍的测定.一试剂丁二酮肟饱和的酒精溶液.氢氧化铵-氯化铵缓冲溶液:pH10,称取氯化铵13.5克溶解于100毫升水中,加氢氧化铵87.5毫升,用水稀至250毫升,摇匀。镍标准溶液:称取纯镍5.000克于400毫升烧杯中,用硝酸溶解,蒸干,用盐酸赶硝酸后,加盐酸使盐类溶解,冷却后移入500毫升量瓶中,用水准确稀至刻度,摇匀.1毫升约等于10毫克镍。EDTA 标准液:称取 EDTA 二钠盐6.5克于
This experiment proved that the extraction of Ni-dimethylglyoxime with CHCl_3, the amount of up to 100 mg of nickel can also be extracted completely before extraction using 2 grams of potassium sodium tartrate complex iron and aluminum and other elements, 0.2 to 0.4 grams of hydroxylamine hydrochloride to reduce the manganese To eliminate its interference, 0.5 grams of sodium thiosulfate reduction of concealed copper, but not consumption of diacetyldichloroxydimethylsiloxane consumption, the method is easy to grasp, suitable for the determination of nickel in the mineral samples, alloys.A reagent dimethylglyoxime Saturated alcohol solution ammonium hydroxide - ammonium chloride buffer solution: pH10, weighed 13.5 g of ammonium chloride dissolved in 100 ml of water, add 87.5 ml of ammonium hydroxide, diluted with water to 250 ml, shake. Nickel standard solution: Weigh pure nickel 5.000 g in 400 ml beaker, dissolved with nitric acid, evaporated to dryness, hydrochloric acid to catch nitric acid, add hydrochloric acid to dissolve salts, cooled and moved into 500 ml volumetric flask, dilute to the mark with water Shake well, and 1 ml equals about 10 mg of nickel. EDTA standard solution: Weigh EDTA disodium salt 6.5 g at