摘要
用单室电解池恒电流电解法溶解黄铜,使基体铜在铂阴极上沉积并用电重量法测定,用阴离子交换树脂吸附基体锌并用络合滴定法测定,消除了基体对ICP-AES测定杂质和微量合金元素的影响,延长了雾化器和石英炬管的使用寿命.用Faraday定律计算电溶解样品的质量(m=kIt).应用此法测定了黄铜中铜、锌、锡、锑、铋、铁、磷与标准值一致,加标回收率为90%～108%.
In the analysis, brass sample, in the form of rod, cubes chips or granules was used as the anode,and Pt gauze electrode as the cathods, and dissolution of the sample was performed by electrolysis, during which cupric ions were reduced and plated on the Pt cathode. Copper content of the sample was determined by electrogravimetry. Amount of sample dissolved by the electrolytic method was calculated by the formula given in the paper. Appropriate amount of conc. HC1 was added to the electrolyte to make it 0. 1 mol· L^-1 in H2SO4, 0. 05 mol · L^-1 in HNO3 and 1.0 mol· L^-1 in HC1, and its volume was made up to 200 mL. An aliquat of the solution having its zinc content around 60 mg, was taken and passed through an ion-exchange column packed with an ion exchange resin to adsorb the zinc in the form of ZnCl4^2-. The effluent solution from the column was used for ICP-AES determination of other alloying elements and also the impurity elements. Dilute nitric acid of 0.1 mol· L^-1 was used as eluant to desorb the ZnCl4^2- from the resin and determined by EDTA titration. Three CRM＇s of brass were analyzed by the proposed method, and results in consistency with the certified values were obtained. Discussion and optimization of analytical conditions and parameters were also given.
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2005年第8期569-572,共4页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
湛江师范学院重点科研项目(L0314)
关键词
ICP-AES
单室电解池
电解溶样
黄铜
ICP-AES
Single compartment electrolytic cell
Electrolytic sample dissolution
Brass analysis
