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%.
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% .
参考文献
| [1] | 韩业斌.含铅玻璃可资源化研究[J].硅酸盐通报,2015(1):164-167. |
| [2] | 张兵;陈奇;宋鹂;陆剑英.含铅玻璃及其无铅化的研究[J].玻璃与搪瓷,2006(1):50-53. |
| [3] | 武明丽.快速EDTA滴定法测定高铅渣料中铅[J].现代化工,2015(7):171-172,174. |
| [4] | 方文韬;史旭峰;朱克聪.铋矿石中高含量铅的测定方法[J].云南地质,2015(3):480-483. |
| [5] | 张萍玲.EDTA滴定法测定铅精粉中的铅含量[J].新疆有色金属,2016(4):76-77. |
| [6] | Chulsung Kim;Say-Kee Ong.Recycling of lead-contaminated EDTA wastewater[J].Journal of hazardous materials,19993(3):273-286. |
| [7] | Kim C.;Lee Y.;Ong SK..Factors affecting EDTA extraction of lead from lead-contaminated soils[J].Chemosphere,20039(9):845-853. |
| [8] | 李艳.EDTA返滴定法测定含钡矿物中的铅量[J].湖南有色金属,2014(3):74-76. |
| [9] | 向德磊.EDTA滴定法测定铅冶炼原料中铅含量结果正确度的探讨[J].冶金分析,2016(8):35-40. |
| [10] | 李志伟.EDTA络合滴定法快速测定含钡铅矿石中的铅[J].岩矿测试,2013(06):920-923. |
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