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一、试剂 混合酸:2份硫酸与1份硝酸混合。 还原剂:在已盛有600ml水的1000ml容量瓶中,依次加入100ml浓硫酸,5g氯化钠,10g盐酸羟铵和20g二氯化锡(固体试剂先用水溶解后加入)。用水稀释至1000ml,摇匀。 汞标准溶液:准确称取0.1354g氯化高汞于0.5NH_2SO_4溶液中,并以0.5NH_2SO_4稀释至1000ml,摇匀。此液含汞100ppm。汞的工作溶液必须在当天分取配制。 二、操作手续 (1)标准曲线的绘制: 取1ml汞储备液(100ppmm)于已盛有400ml蒸馏水的500ml容量瓶中,加1∶1硫酸10ml,水稀刻度,摇匀,配制成200ppb汞的工作溶液。 在一组各盛有100ml蒸馏水的250ml容量瓶中,分别移取汞的工作溶液 0、0.5、……40ml,加混合酸10ml,5％高锰酸钾溶液2ml,在水浴上(70～
First, the reagent mixed acid: 2 parts sulfuric acid and 1 part of nitric acid mixed. Reducing agent: In a 1000 ml volumetric flask containing 600 ml of water, 100 ml of concentrated sulfuric acid, 5 g of sodium chloride, 10 g of hydroxylammonium chloride and 20 g of tin dichloride are successively added (the solid reagent is added after being dissolved with water). Dilute with water to 1000ml, shake well. Mercury standard solution: Weigh accurately 0.1354g of high chloride mercury chloride in 0.5NH_2SO_4 solution, and 0.5NH_2SO_4 diluted to 1000ml, shake. This solution contains mercury 100ppm. Mercury working solution must be prepared on the day of preparation. Second, the operating procedures (1) the standard curve drawing: Take 1ml of mercury stock solution (100ppmm) in 400ml distilled water has been filled 500ml volumetric flask, add 1: 1 sulfuric acid 10ml, dilute the water, shake, formulated into 200ppb mercury Working solution. In a set of each containing 100ml distilled water 250ml volumetric flask were removed Mercury 0,0.5 ... 40ml of the working solution, add mixed acid 10ml, 5% potassium permanganate solution 2ml, on a water bath (70 ~