湿法炼锌过程溶液中镍的微分脉冲极谱法测定

在氨-氯化铵缓冲液(pH=10.0)+150g/L柠檬酸钠+2g/L丁二酮肟(DMG)底液体系中,采用微分脉冲极谱法测定湿法炼锌中间溶液中镍的浓度。结果表明:在-0.98V左右产生灵敏的微分脉冲极谱波,镍浓度在8.52×10-7～8.52×10-5 mol/L范围内与相应峰电流有良好的线性关系,检测限为1.7×10-7 mol/L。该方法成功用于湿法炼锌中上清液、一段净化后液、二段净化后液、电积新液、电积废液中镍的测定,RSD分别小于等于0.43%、1.33%、1.92%、2.87%、4.87%,加标回收率为98.4%～102.2%,方法灵敏、简单、快速。

Determination of Nickel in Intermediate Liquid From Zinc Hydrometallurgy by Differential Pulse Polarography

In the substrate solution(ammonia-ammonium chloride buffer solution(pH=10.0)+150 g/L sodium citrate+2 g/L dimethylglyoxime(DMG)),nickel(Ⅱ) in intermediate liquid from the process of zinc hydrometallurgy can be determinated by differential pulse polarography.A sensitive adsorptive complex wave forms at about-0.98 V.There is a good linear relationship between the nickel(Ⅱ) concentration and corresponding peak current when the nickel(Ⅱ) concentration is between 8.52×10-7to 8.52×10-5 mol/L,the detection limit is 1.7×10-7 mol/L.This method has been successfully used to determine nickel concentration in the middle-supernatant,first stage cleaning liquid,second stage cleaning liquid,electrolyte and spent electrolyte in zinc hydrometallurgy.Relative standard deviation are less than or equal to 0.43%、1.33%、1.92%、2.87%、4.87%,and the recovery of nickel(Ⅱ) is between 98.4% to 102.2%.The method is sensitive,simple and fast.