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Na2EDTA滴定法测定铅滤饼中铅
- 作者：
吕茜茜
- 作者单位：
- （铜陵有色金属集团控股有限公司检测研究中心）
详细信息：
- 作者简介：
- 吕茜茜（1984—），女，高级工程师，从事仪器分析和有色重金属、稀贵金属、稀土等矿产品、中间产品的检测与研究工作；E‑mail: 282677188@qq. com
- PDF下载
Determination of lead in lead filter cake by Na2EDTA titration
- English Author：
Lü Qianqian
- Unit：
- （Testing and Research Center, Tongling Nonferrous Metals Group Holdings Co., Ltd.）
- 摘要
- 在线预览
- 参考文献
摘要:
研究建立了铅滤饼中铅量的分析方法。试样采用氟化氢铵、盐酸、硝酸和硫酸溶解，氢溴酸除去砷、锡干扰，利用硫酸沉淀铅与其他干扰元素分离，沉淀溶解于乙酸-乙酸钠缓冲溶液中，巯基乙酸作为掩蔽钬，二甲酚橙作为指示剂，用Na，EDTA标准滴定溶液滴定试液中铅，采用火焰原子吸收光谱法测定滤液中铅进行补正，二者相加即为试样中铅量。实验结果表明：在最佳实验条件下，方法测定结果的相对标准偏差为0.147%~0.269%，加标回收率为99.30%~101.00%，能够很好满足铅滤饼中铅量的测定需要。
关键词:
Na2EDTA滴定法；铅滤饼；铅；干扰元素；火焰原子吸收光谱法；补正
Abstract:
A method for analyzing lead content in lead filter cake was developed. The sample was dissolved using ammonium hydrogen fluoride, hydrochloric acid, nitric acid, and sulfuric acid. Arsenic, and tin interferences were removed with hydrobromic acid, while lead was separated from other interfering elements via sulfate precipitation. The precipitate was dissolved in an acetate-acetic acid buffer solution. Thioglycolic acid was employed to mask bismuth. and xylenol orange served as the indicator. Lead in the solution was titrated with a standardized Na, EDTA solution. Residual lead in the filtrate was corrected using fire atomic absorption spectrometry, and the total lead content was obtained by summing both results. Experimental data show that under optimal conditions, the method achieves a relative standard deviation of 0.147 %-0.269 % and a recovery rate of 99.30 %-101.00 %, effectively meeting the require-ments for lead determination in lead filter cakes.
Keywords:
Na2EDTA titration; lead filter cake; lead; interfering elements; fire atomic absorption spectrometry；correction
