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硫酸工业中,钒触媒中微量砷的测定一般采用古蔡法和铜试剂银法(AgDDC法),前者灵敏度差,后者操作虽简单但需使用氯仿等有机溶剂。用二硫代二安替比林甲烷(DTPM)测定砷,灵敏度较高,不用有机溶剂,又能有效地避免有色离子的干扰,已在矿石与钢铁中测定砷获得应用,本文在盐酸介质中将其用于钒触媒中砷的测定,获得满意结果。 1 试验部分1.1 试剂与仪器砷标准溶液:100μg·ml~(-1),称取在硫酸干燥器中干燥至恒重的As_2O_30.1320g溶于NaOH(5%)溶液10ml中,用盐酸(1+1)中和至中性,移入1000ml量瓶中,定容至刻度。用时再稀释成5μg·ml~(-1)砷标准液。 DTPM溶液:0.1%,称取0.1000gDTPM(无锡高速分析仪器厂试剂研究所产品),溶于N,N′-二甲基甲酰胺25ml中,加乙醇25ml,移入100ml量瓶中,用水定容,摇匀。
Sulfuric acid industry, the determination of trace amounts of arsenic in vanadium catalyst commonly used ancient method and copper reagent Ag method (AgDDC method), the former sensitivity is poor, the latter operation is simple but need to use organic solvents such as chloroform. Determination of arsenic with dithio-diantipyrylmethane (DTPM) has the advantages of high sensitivity, no organic solvent, and effectively avoiding the interference of colored ions. The determination of arsenic in ore and steel has been applied. In this paper, It is used for the determination of arsenic in vanadium catalyst, and satisfactory results are obtained. 1 Experimental 1.1 Reagents and Instruments Arsenic standard solution: 100μg · ml -1, weighed in sulfuric acid dryer dried to constant weight As_2O_3.1320g dissolved in NaOH (5%) solution 10ml, with hydrochloric acid (1 +1) Neutralization to neutral, into 1000ml volumetric flask, set the volume to the mark. Use diluted to 5μg · ml ~ (-1) arsenic standard solution. DTPM solution: 0.1%, weighed 0.1000gDTPM (Wuxi Institute of High Speed Analytical Instrument reagent products), dissolved in N, N’- dimethylformamide 25ml, add ethanol 25ml, transferred to 100ml volumetric flask, the volume of water , Shake well.