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在动力学法测钯时硒有干扰。我们研究了在活化剂汞(Ⅱ)存在下,硒(Ⅳ)对次磷酸钠还原磷钼酸成钼蓝的反应的强烈催化作用,建立了动力学法测定痕量硒(Ⅳ)的方法,经人发标样对照,结果令人满意。在文中所选条件下,检出限为8.3×10~(-6)μg·ml~(-1),为目前催化动力学法测定硒(Ⅳ)最灵敏的一种。 1 试验部分 1.1 仪器与试剂超级恒温器(重庆试验设备厂) 721型分光光度计(上海第三分析仪器厂) 硒(Ⅳ)标准溶液:称取Na_2SeO_3 0.22g溶于1L水中,此溶液含硒(Ⅳ)0.10mg·ml~(-1),用时再用水稀释至含硒(Ⅳ)0.10μg·ml~(-1)。
Selenium has interference in the kinetic method for the determination of palladium. We have studied the strong catalytic effect of selenium (Ⅳ) on the reaction of sodium hypophosphite to phosphomolybdic acid to molybdenum blue in the presence of activator mercury (Ⅱ), and established a method for the determination of trace selenium (Ⅳ) by kinetic method. By the standard sample control, the results are satisfactory. Under the conditions selected in this paper, the detection limit is 8.3 × 10 -6 μg · ml -1, which is the most sensitive one for the determination of selenium (Ⅳ) by catalytic kinetic method. 1 Experimental 1.1 Instruments and reagents Super thermostat (Chongqing Experimental Equipment Factory) 721 spectrophotometer (Shanghai Third Analytical Instrument Factory) Selenium (Ⅳ) standard solution: Weigh 0.22g Na_2SeO_3 dissolved in 1L of water, the solution containing selenium (Ⅳ) 0.10mg · ml ~ (-1), dilute with water to selenium (Ⅳ) 0.10μg · ml ~ (-1).