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矿石中Gu、Pb、Zn的极谱测定,一般多在不同介质中分别进行。为了在同一底液中连续测定这三个元素,本文选择氨基乙酸—氯化铵为支持电解质。在此介质中,Cu、Pb、Zn的峰电位分别为-0.40V、-0.60V及-1.20V(对饱和甘汞电极)产生清晰而重现的还原波。试验表明:在20毫升体积中,Gu、Pb、Zn含量在15毫克范围内,峰高与浓度呈线性关系,三元素同时共存量高低相差100倍左右,也互不干扰测定。Fe(Ⅲ)对测定有严重的干扰,可借盐酸羟胺将其还原为Fe(Ⅱ)而消除影响;溶解于底液中的微量氧对低量铜的测定产生正干扰,可采用碳酸氢钠除氧;锡与沿波重合,可在王水溶矿后,用盐酸反复蒸干处理两次,使Sn呈SnCl_4状态而挥发;在此同时Sb也呈
Ore in Gu, Pb, Zn polarographic determination, generally more in different media separately. In order to determine the three elements in the same bottom solution continuously, we chose aminoacetic acid-ammonium chloride as supporting electrolyte. In this medium, the peak potentials of Cu, Pb and Zn were -0.40V, -0.60V and -1.20V (for saturated calomel electrode), respectively, producing a clear and reproducible reduction wave. The results showed that there was a linear relationship between the peak height and the concentration in the range of 15 mg in the volume of 20 ml, and the difference of the coexistence amount of three elements was about 100 times, which also did not interfere with each other. Fe (Ⅲ) on the determination of a serious interference by hydroxylamine hydrochloride can be reduced to Fe (Ⅱ) and eliminate the impact; dissolved in the bottom of the trace oxygen in the determination of low amount of copper have a positive interference, the use of sodium bicarbonate Deoxidation; tin and along the wave overlap, can be dissolved in the aqua regia, with hydrochloric acid repeatedly steam-cured twice, so Sn was SnCl_4 state volatile; at the same time Sb was also