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硫酸镍样品不经分离和予处理,用水溶解制成含NiSO_4·6H_2O80毫克/毫升的溶液,用钙离子选择电极直接测定钙含量。本方法测定Ca~(2+)浓度范围为10~(-1)～10~(-4)M的硫酸镍溶液,相对标准偏差为1.1%,方法简便快速、易于掌握。硫酸镍是碱性蓄电池的主要成份之一,硫酸镍中钙含量直接影响蓄电池的性能,所以,测定硫酸镍中钙含量有重要意义。常量钙的测定用滴定法和重量法可得满意结果。微量钙的测定可用光度法、阳极溶出伏安法和原子吸收分光光度法。用离子选择电极测定钙已有报导。陈超五用钙电极测定了岩石中的钙,薛效贤等用钙电极测定了血清中总钙量,但用钙电极直接测定硫酸镍中的钙未见报导。硫酸镍中钙含量在0.02～0.03%时,一般化工厂用硫化铵沉淀基体元素镍,用氰化物作掩蔽剂排除干扰元素,再用络合滴定法测定钙,这样,不仅由于使用氰化物毒性大、污染环境,且手续繁杂,再现性差。我们把硫酸镍用水溶解后,制成高浓度(含NiSO_4·6H_2O80毫克/毫升)溶液,不经分离,不作任何处理,用钙电极直接测定钙,得到了满意的结果。
Nickel sulfate samples without isolation and pretreatment, dissolved in water to make a solution containing NiSO 4 · 6H 2 O 80 mg / ml, with calcium ion selective electrode direct determination of calcium content. The method was applied to the determination of nickel sulfate solution with Ca ~ (2+) in the range of 10 ~ (-1) ~ 10 ~ (-4) M with the relative standard deviation of 1.1%. The method is simple, rapid and easy to master. Nickel sulfate is one of the main components of alkaline batteries. The content of calcium in nickel sulfate directly affects the performance of the battery. Therefore, it is important to determine the content of calcium in nickel sulfate. Determination of constant calcium Titration and gravimetric methods give satisfactory results. Determination of trace calcium spectrophotometry, anodic stripping voltammetry and atomic absorption spectrophotometry. Calcium has been reported using ion-selective electrodes. Chen Chaowu calcium electrode determination of calcium in the rock, Xuexian Yin and other calcium electrode determination of serum total calcium, but direct determination of calcium in calcium sulfate with calcium has not been reported. Nickel sulphate calcium content of 0.02 to 0.03%, the general chemical plant with ammonium sulfide precipitation of nickel as the matrix element, with cyanide as a masking agent to exclude interference elements, and then the complexometric titration of calcium, so not only because of the use of cyanide toxicity Large, pollute the environment, and complicated procedures, poor reproducibility. After dissolving the nickel sulfate in water, we made a solution with high concentration (containing NiSO 4 · 6H 2 O 80 mg / ml) without any treatment and directly measured the calcium with the calcium electrode. We got satisfactory results.