EDTA滴定法测定氧化锌浸出渣中铅含量

doi:10.13228/j.issn.1000-7571.2014.02.016

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摘要提出了一种采用EDTA滴定法测定含铁、硅较高的氧化锌浸出渣中铅的分析方法。将试样用盐酸和硝酸溶解, 加入氟化铵分解渣料中的硅酸盐, 使包裹在硅酸盐中铅全部溶解出来, 然后加入硫酸使铅形成硫酸铅沉淀, 过滤, 使铅与锌、铁等易溶于硫酸的共存元素分离。用乙酸-乙酸钠缓冲溶液溶解硫酸铅, 加入抗坏血酸掩蔽少量铁, 以二甲酚橙为指示剂, 在pH 5～6的条件下, 用EDTA标准溶液滴定溶液至亮黄色为终点。样品测定结果的相对标准偏差在0.23%～0.76 %之间, 平均加标回收率为100.2%。

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	付国秀
	牛勤学
	党小杰

关键词 ：氧化锌浸出渣, EDTA, 滴定法, 铅

Abstract：An analytical method was proposed for the determination of lead in zinc oxide leaching residue with higher iron and silicon by EDTA titrimetry. The sample was dissolved in hydrochloric acid and nitric acid, then ammonium fluoride was added to decompose the silicates and completely dissolve lead enclosed in the silicates. Sulfuric acid was added to form lead sulfate precipitate, which was filtered to separate lead from other coexisting elements liking zinc and iron soluble in sulfuric acid. Acetic acid-sodium acetate buffer solution was used to dissolve lead sulfate and ascorbic acid was added to mask the small amounts of iron. With xylenol orange as the indicator, at pH 5-6, EDTA standard solution was used to titrate the solution into the color of bright yellow as the end. The relative standard deviation of determination results was in the range of 0.23%-0.76% and the average recovery was 100.2 %.

Key words： zinc oxide leaching residue EDTA titrimetry lead

收稿日期: 2013-07-08

ZTFLH:

O655.25

通讯作者: 牛勤学(1969-), 男, 高级工程师;E-mail:13509146720@163.com E-mail: 13509146720@163.com

作者简介: 付国秀(1971-), 女, 工程师, 研究方向:有色金属冶金分析

引用本文:

付国秀, 牛勤学, 党小杰. EDTA滴定法测定氧化锌浸出渣中铅含量[J]. 冶金分析, 2014, 34(2): 70-73. FU Guo-xiu, NIU Qin-xue, DANG Xiao-jie. Determination of lead in zinc oxide leaching residue by EDTA titrimetry. , 2014, 34(2): 70-73.

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http://47.93.29.245/Jweb_yjfx/CN/10.13228/j.issn.1000-7571.2014.02.016 或 http://47.93.29.245/Jweb_yjfx/CN/Y2014/V34/I2/70

[1]	邓乐章.直读光谱法测定锌合金中的铝、铅、铁、镉、铜、锡量[J]. 分析试验室(Chinese Journal of Analysis Laboratory), 2009, 28(12):93-95.
[2]	陈安明. 电感耦合等离子体原子发射光谱法测定钢及生铁中痕量砷锑铋锡铅[J]. 冶金分析(Metallurgical Analysis), 2007, 27(3):68-70.
[3]	王霞, 张祥志, 陈素兰. ICP-AES同时测定固体废物浸出液中钡、铍、镉、铬、铜、镍、铅和锌[J]. 光谱实验室(Chinese Journal of Spectroscopy Laboratory), 2009, 26(6):1445-1447.
[4]	姚传刚, 杨丽飞, 王昊云, 等. 电感耦合等离子体原子发射光谱法测定精铝箔中铅镉砷[J]. 冶金分析(Metallurgical Analysis), 2008, 28(12):54-56.
[5]	李刚, 陈苏, 李艳, 等. 电感耦合等离子体原子发射光谱法测定核级锆合金中17种常量及痕量元素[J]. 冶金分析(Metallurgical Analysis), 2012, 32(11):56-60.
[6]	GB/T8151.20-2012 锌精矿化学分析方法:铜、铅、铁、砷、镉、锑、钙、镁量的测定—电感耦合等离子体原子发射光谱法[S].
[7]	张泽儒. ICP-AES法测定压铸锌合金中的铝、镁、铜、铅、铁、镉、锡量[J]. 甘肃冶金(Gansu Metallurgy), 2010, 32(2):18-21.
[8]	阁钰玮, 胡晓民, 索金玲, 等. FAAS测定进口铜铳中的铜、铁、铅、锌、镉和锰[J]. 光谱实验室(Chinese Journal of Spectroscopy Laboratory), 2012, 29(6):3357-3360.
[9]	张丽, 周永进. 原子吸收分光光度法测定硫酸钙盐中铅、镁含量[J]. 云南冶金(Yunnan Metallurgy), 2012, 39(6):18-21.
[10]	孙淑嫒, 等.矿石及有色金属分析手册[M]. 北京:冶金工业出版社, 2007.
[11]	GB/T8152.1-2006 铅精矿化学分析方法:铅量的测定— 酸溶解EDTA滴定法[S].
[12]	李春艳. EDTA滴定法在筛选铅锌矿中应用[J]. 中国科技信息(China Science Technology Information), 2008, (14):28-29.
[13]	杨理勤, 冯亮. EDTA滴定法连续测定铅锌矿中铅和锌[J]. 中国无机分析化学(Chinese Journal of Inorganic Analytical Chemistry), 2013.3(2):22-24.
[14]	陈珍娥.硫酸铅沉淀分离- EDTA滴定粗铅中铅含量[J]. 科技论坛(Science & Technology Assciation Forum), 2008, (10):40.
[15]	黄菊英, 谢辉. EDTA滴定法测定铅锡合金中铅[J]. 冶金分析(Metallurgical Analysis), 2013, 33(3):77-79.
[16]	王安红, 高风光. 铅基合金的溶解及铅的快速测定[J]. 理化检验:化学分册(Physical Testing and Chemical Analysis: Part B Chemical Analysis), 2003, 39(4):239-242.