酸溶-碱熔法处理复杂含铅样品铅的检测
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1.河南省黄金资源综合利用重点实验室, 河南 三门峡 472000 ;2.河南中原黄金冶炼厂有限责任公司, 河南 三门峡 472000

作者简介:

孙婷婷(1988—),女,吉林延边人,冶金工程师,主要从事有色金属冶炼分析检测工作。

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Measurement of lead in complex lead-containing samples treated by the acid leaching-alkali fusion method
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1.Key Laboratory of Comprehensive Utilization of Gold Resources of Henan Province, Sanmenxia 472000 , China ;2.Henan Zhongyuan Gold Smelter Co., Ltd., Sanmenxia 472000 , China

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    摘要:

    火法炼铜行业综合回收产生的含铋铅精粉在分析检测时为复杂含铅样品,其中含有钡、砷、锑、锡、铋等元素,在进行铅含量分析时,元素间相互影响,共生包裹严重,现有检测方法不能同时解决铅完全溶解和多种杂质元素干扰的问题。本文采用酸溶-碱熔的方法对复杂含铅样品进行处理,酸溶部分的铅采用EDTA滴定法测定,碱熔部分的铅采用原子吸收光谱法测定;对酸溶溶液采用硫酸分离钡,溴化氢除砷、锑、锡,EDTA络合铋的方法,能够消除多种杂质元素对铅的干扰;对该方法进行精密度试验和准确度试验,结果表明相对标准偏差和相对误差均小于1%。该方法操作相对简便、重现性好、准确度高,对复杂含铅样品中铅的准确测定具有很好的借鉴作用。

    Abstract:

    Complex lead-containing samples from comprehensive recovery in pyrometallurgical copper smelting industry contain elements such as Ba, As, Sb, Sn and Bi. In the analysis of lead content, the elements are severely symbiotic and enwrapped due to interaction. The existing detection methods can not solve the problems of complete dissolution of lead and interference of various impurity elements at the same time. In this paper, the acid leaching-alkali fusion method was adopted to treat complex lead-containing samples. The lead leached by acid was measured by EDTA titration, and the lead dissolved by alkali fusion was measured by atomic absorption spectrometry. For acid-leaching solution, sulfuric acid was adopted for separating Ba, hydrogen bromide for removing As, Sb and Sn, and EDTA for Bi complexation, which eliminated the interference of various impurity elements on lead. The method was applied to the measurement of lead in Reference Material Lead Concentrates GBW(E)070173, and the relative error of the obtained result was less than 1%. The method is relatively easy and convenient in operation, with good reproducibility and high accuracy, which is of great reference for accurate measurement of lead in complex lead-containing samples.

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孙婷婷, 姜艳水, 张厚杰, 等. 酸溶-碱熔方法处理复杂含铅样品铅的检测[J]. 中国有色冶金, 2022,51(4):76-80.

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  • 收稿日期:2021-12-26
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  • 在线发布日期: 2025-12-24
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