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我们试验了以KCl-HAc-NaAc为底液时,用玻碳汞膜电极和“79-1”伏安分析仪连续测定Bi,Cu、Pb、Cd离子的条件,该法分辨力好,灵敏度高,测定的最低浓度为Bi 0.4ppb,Cu 0.5ppb,Pb 0.6ppb,Cd 0.2ppb。方法应用于纯银和河水的测定,回收率在92～112%范围内。一仪器和试剂 79-1型伏安分析仪(附旋转电解池); 工作电极:盘状玻碳电极;参比电极:Ag-AgCl电极;对电极:pt丝电极; LZ3-104型x-y函数记录仪。铜,铅,镉混合标准液:称取高纯铜,铅和镉各0.25克,于50毫升烧杯中加5毫升硝酸(1+1)溶解并加热除尽氧化氮,移入250毫升量瓶中,用重蒸馏水稀释至刻度摇匀。其浓度为1mg ml~(-1),用时稀释至10μg ml~(-1);铋标准溶液:称取高纯铋0.25克于100毫升烧杯中加入硝酸(1+2)15毫升,加热溶解后,每次用5毫升浓盐酸反复蒸干2～3次,除尽氧化氮,移入250毫升量瓶中以盐酸(1+1)稀释至刻度,其浓度为1 mgml~(-1),用时以盐酸(1+1)稀释至10μg ml~(-1)。
We tested the continuous determination of Bi, Cu, Pb and Cd ions using glassy carbon-mercury membrane electrode and “79-1” voltammetry analyzer with KCl-HAc-NaAc as the bottom solution. , The sensitivity is high. The lowest concentrations measured are Bi 0.4ppb, Cu 0.5ppb, Pb 0.6ppb, Cd 0.2ppb. The method was applied to the determination of pure silver and river water and the recoveries ranged from 92% to 112%. An instrument and reagent 79-1 type voltammetry analyzer (with rotating electrolytic cell); working electrode: plate glassy carbon electrode; reference electrode: Ag-AgCl electrode; counter electrode: pt wire electrode; LZ3-104 type xy function Logger. Copper, lead and cadmium mixed standard solution: Weigh each high-purity copper, lead and cadmium 0.25 grams, in a 50 ml beaker plus 5 ml of nitric acid (1 +1) dissolved and heated to remove nitrogen oxide, into a 250 ml volumetric flask , Dilute with distilled water to the mark. The concentration of 1mg ml -1, when diluted to 10μg ml -1; bismuth standard solution: Weigh high purity bismuth 0.25 g in 100 ml beaker was added nitric acid (1 +2) 15 ml, heated to dissolve After each time with 5 ml of concentrated hydrochloric acid repeatedly evaporated 2 or 3 times, except for the nitrogen oxide, into a 250 ml volumetric flask diluted with hydrochloric acid (1 + 1) to the mark, the concentration of 1 mgml -1, When used with hydrochloric acid (1 + 1) diluted to 10μg ml ~ (-1).