学术论文

      EDTA返滴定法测定铅玻璃中铅

      Determination of lead content in lead glass by EDTA back titration method

      摘要:
      采用氢氟酸-盐酸-硝酸-高氯酸溶解样品,硫酸铅沉淀分离,在氨水-ED T A介质中溶解硫酸铅沉淀,在乙酸-乙酸钠缓冲体系下,以二甲酚橙为指示剂,乙酸铅返滴定测定铅含量,优化了沉淀陈化时间、氨水加入量、微沸时间以及乙酸-乙酸钠缓冲溶液加入量等实验条件,建立了采用ED T A返滴定法测定铅玻璃中铅的方法.实验方法用于测定铅玻璃中铅,结果的相对标准偏差(RSD,n=11)为0.32%.按照实验方法对铅玻璃样品进行加标回收试验,回收率为99.5%~102.0%.
      Abstract:
      The sample was dissolved with hydrofluoric acid-hydrochloric acid-nitric acid-perchloric acid sys-tem .Lead was separated in the form of lead sulfate precipitate ,which was then dissolved in ammonia-EDTA solution medium .The content of lead was finally determined by lead acetate back titration method in HAc-NaAc buffer solution using xylenol orange as the indicator .The experimental conditions ,including— 68 —the ageing time of precipitate ,the addition amount of ammonia ,the sub-boiling time and the dosage of HAc-NaAc buffer solution ,were optimized .The determination method of lead in lead glass by EDTA back titration was established .The proposed method was applied to the determination of lead in lead glass .The relative standard deviations (RSD ,n=11) of determination result was 0 .32% .The recovery test of lead glass sample was conducted according to the experimental method .The recoveries were between 99 .5%and 102 .0% .
      作者: 范丽新 [1] 陆青 [2]
      Author: FAN Li-xin [1] LU Qing [2]
      作者单位: 北京矿冶研究总院 ,北京102628;金属矿产资源评价与分析检测北京市重点实验室 ,北京 102628 钢铁研究总院 ,北京100081;钢研纳克检测技术有限公司 ,北京 100094
      刊 名: 冶金分析 ISTICPKU
      年,卷(期): 2017, 37(2)
      在线出版日期: 2017年3月30日
      基金项目: 北京市科技创新基地培育与发展专项