Abstract:The potential was not stable in determination of chloride ion by potentiometric titration. To solve this problem, a determination method of chloride ion content in copper electrolyte was established by automatic potentiometric titration with small dose isopropanol as stabilizer. The experimental method was described as follows: 10.00 mL of copper electrolyte sample was accurately transferred into 50 mL beaker; the reaction temperature was controlled at 20-30°C; after adding 2 mL of isopropanol, the solution was diluted with water to about 50 mL;after the silver combination electrode and dropper were washed with water and then inserted into testing solution, the rotate speed of stirrer was control at 625 r/min; finally, the solution was titrated with 0.010 0 moL/L silver nitrate standard solution. The interference test indicated that the influence of sulfuric acid, copper matrix and other coexisting elements in copper electrolyte sample on the determination of chloride ion could be ignored. The proposed method was applied to the determination of chloride ion in copper electrolyte actual sample. The results were basically consistent with those obtained by turbidimetry. The relative standard deviation (RSD, n=5) was less than 0.74%. The recoveries were between 98% and 102%.
安泰莹,文庆珍,朱金华.氯离子测定方法研究进展[J].河南化工(Henan Chemical Industry),2013,30(3-4):8-11.
[2]
佟琦,高丽华.莫尔法与自动电位滴定法测定水中氯离子含量的比较[J].工业水处理,2008,28(11):69-71.TONG Qi,GAO Li-hua.The comparison between Mohr method and automatic potentiometry in determining chloride ion content in water[J].Industrial Water Treatment,2008,28(11):69-71.
[3]
巫来富.氯化银浊度法测定铜电解液中氯离子[J].嘉应学院学报:自然科学,2012,30(8):52-55.WU Lai-fu.Determination of chlorine ion in copper electrolyte using chloride turbidimetric method[J].Journal of Jiaying University:Natural Science,2012,30(8):52-55.
[4]
张敏,王德淑.氯化银比浊法测定铜箔镀液中微量氯[J].理化检验:化学分册,2000,36(6):257-260.ZHANG Min,WANG De-shu.Turbidimetric determination of microamounts of chloride (as AgCl) in copper electroplating solution[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2000,36(6):257-260.
胡一航,王海北,王玉芳.水蒸气蒸馏-离子色谱法测定湿法炼锌溶液中氟和氯[J].冶金分析,2015,35(5):59-62.HU Yi-hang,WANG Hai-bei,WANG Yu-fang.Determination of fluorine and chlorine in solution of wet zinc hydrometallurgy by steam distillation-ion chromatography[J].Metallurgical Analysis,2015,35(5):59-62.
[7]
马毅红,吴纯,尹艺青.火焰原子吸收光谱法间接测定铝箔腐蚀液中氯含量[J].理化检验:化学分册(Physical Testing and Chemical Analysis Part B:Chemical Analysis),2012,48(12):1494-1495.
王婷香.硝酸银电位滴定法测定高纯二氧化锗中氯[J].冶金分析,2015,35(5):74-76.WANG Ting-xiang.Determination of chlorine in high-purity germanium dioxide by silver nitrate potentiometric titration[J].Metallurgical Analysis,2015,35(5):74-76.
[11]
张文娟,李谨.铜电解液中水溶氯测定方法的探讨与研究[J].昆明冶金高等专科学校学报,2013,29(3):68-70.ZHANG Wen-juan,LI Jin.Determination of water soluble chloride copper electrolyte discussion and research methods[J].Journal of Kunming Metallurgy College,2013,29(3):68-70.
[12]
邵海青.电位滴定法测定铜电解液中氯离子[J].冶金分析,2001,21(4):64-65.SHAO Hai-qing. Determination of chloride ion in copper electrolyte by potentiometric titration[J].Metallurgical Analysis,2001,21(4):64-65.
[13]
白小叶.酸性镀铜溶液中氯离子的测定[J].有色矿冶,2006,22(3):70-72.BAI Xiao-ye.Detecting chlorine ion in copper foil electrolyte[J].Non-Ferrous Mining and Metallurgy,2006,22(3):70-72.