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样品按生铁系统快速分析法溶解后,用1:1硫酸调节酸度至10N,加抗坏血酸及碘化钾,用苯萃取,水反萃取后,调节酸度至1.0~1.2N的硫酸溶液中加入钼酸铵,硫酸肼,以砷钼蓝法测定砷。试剂: 硝硫混合酸:硫酸50毫升,硝酸8毫升加入水至1升;过硫酸铵溶液:30%,当天配制;碘化钾溶液:5M,称取碘化钾83克溶于水中,稀至100毫升。盐酸——碘化钾洗液:吸2毫升5M碘化钾,用10N盐酸稀至100毫升(用时配制)。 2.5%钼酸铵——10N硫酸溶液:称取2.5克钼酸铵溶于少量的水中,过滤于100毫升量瓶中,加入56毫升1:1硫酸,冷却后稀至刻度。
After the sample was dissolved by the rapid analysis method of the pig iron system, the acidity was adjusted to 10N with 1: 1 sulfuric acid, ascorbic acid and potassium iodide, extracted with benzene, and after the water was stripped, the ammonium sulfate was added to the sulfuric acid solution of which the acidity was adjusted to 1.0 to 1.2N, Hydrazine sulfate, arsenic determination by arsenic molybdenum blue method. Reagents: sulfur and sulfur mixed acid: 50 ml of sulfuric acid, 8 ml of nitric acid was added to 1 liter of water; ammonium persulfate solution: 30%, the day preparation; potassium iodide solution: 5M, weighed 83 grams of potassium iodide dissolved in water, dilute to 100 ml. Hydrochloric acid-potassium iodide lotion: Aspirate 2 ml of 5 M potassium iodide and dilute to 100 ml with 10 N hydrochloric acid (in preparation). 2.5% Ammonium molybdate - 10N sulfuric acid solution: Dissolve 2.5g of ammonium molybdate in a small amount of water, filter in a 100ml volumetric flask, add 56ml of 1: 1 sulfuric acid, dilute to the mark after cooling.