摘要
建立氧弹燃烧–自动电位滴定法测定助焊剂中卤素的分析方法。在氧弹罐加入20 mL 0.25 mol/L氢氧化钠溶液作为吸收液,通过氧弹罐燃烧使得助焊剂中共价态的卤素转变成为离子态,利用氢氧化钠溶液吸收氧弹燃烧所释放的离子态卤素,吸收后的溶液用硝酸溶液(1∶1)进行酸化,消除碳酸根、碳酸氢根、氢氧根离子的干扰。处理后的样品溶液用0.01 mol/L硝酸银标准溶液进行滴定。助焊剂样品中卤素测定结果的相对标准偏差为0.51%~3.24%(n=5),加标回收率为95.24%~100.49%。该方法样品处理简单,操作简便,成本低廉。
The oxygen bomb combustion–automatic potentiometric titration method was established for the determination of the halogen in flux.Adding 20 mL of 0.25 mol/L sodium hydroxide solution to the oxygen bomb tank as the absorption solution,the covalent halogen in the flux was transformed into an ionic form,sodium hydroxide solution was used to absorb ionic halogens released by oxygen bomb combustion.The solution after absorption was acidified with nitric acid solution(1∶1)to eliminate interference of carbonate,bicarbonate and hydroxide ions.The treated solution was titrated with 0.01 mol/L silver nitrate standard solution.The relative standard deviation of the determination of the halogen in the flux sample was 0.51%–3.24%(n=5),and the recovery rate of the standard addition was between 95.24%–100.49%.The method is simple in sample processing and easy to operate,which is economical and effective.
作者
李丽
段泽平
韩红兰
秦俊虎
卢红波
熊晓娇
赵中梅
何江华
LI Li;DUAN Zeping;HAN Honglan;QIN Junhu;LU Hongbo;XIONG Xiaojiao;ZHAO Zhongmei;HE Jianghua(Tin Products Manufacturing Co.Ltd.,of YTCL,Kunming 650500,China)
出处
《化学分析计量》
CAS
2022年第6期32-35,共4页
Chemical Analysis And Meterage
关键词
自动电位滴定法
氧弹
助焊剂
卤素
automatic potentiometric titration method
oxygen bomb
flux
halogen
