ICP-OES法测定铜冶炼烟尘中铋含量
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楚雄滇中有色金属有限责任公司, 云南 楚雄 675000

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李超(1987—),男,云南楚雄人,工程师,长期从事分析检测工作。

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TF811;TF803+1

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Determination of bismuth in copper smeltingdust by ICP-OES
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    摘要:

    某冶炼厂烟尘中铋含量达到2%~4%,不适合采用原子吸收光谱法、氢化物发生-原子荧光法和硫脲光度法,但采用EDTA滴定法时,存在耗时长、滴定酸度范围较窄(pH值为1.5~1.7)、滴定过程酸度难以控制的问题。本文采用电感耦合等离子体原子发射光谱(ICP-OES)分析方法对铜冶炼烟尘中的铋含量测定进行了试验,对样品分解方法、仪器工作条件、谱线选择、基体效应进行了分析,得出以下结论:采取加长雾化系统清洗时间可以克服雾化器的堵塞,从而消除干扰;在5%硝酸介质中,样品中3%以下含量的锑不会发生水解反应,不会对测定带来干扰;采用Bi 190.241nm作为分析线,避免与Cu 223.00nm的谱线重叠,可消除测定过程中铜对铋的干扰。此方法测定烟尘中铋含量的回收率为99.0%~101.1%,相对标准偏差为1.51%,结果准确可靠。

    Abstract:

    The bismuth content in the dust of a smelter reaches 2% to 4%, which is not suitable for the use of atomic absorption spectroscopy, hydride generation-atomic fluorescence method and thiourea photometry. However, when the EDTA titration method is used, there are problems such as long time-consuming, narrow titration acidity range (pH 1.5 to 1.7), and difficulty in controlling acidity in the titration process. In this paper, inductively coupled plasma atomic emission spectroscopy (ICP-OES) was used to test the determination of bismuth in copper smelting dust. The sample decomposition method, instrument working conditions, spectral line selection, and matrix effect were analyzed, and the following results were obtained. Adopting a longer cleaning time of the atomization system can overcome the blockage of the atomizer and eliminate the interference; in a 5% nitric acid medium, the antimony content of less than 3% in the sample will not undergo hydrolysis reaction and will not interfere with the determination; use Bi 190.241nm as the analysis line to avoid overlapping with the Cu 223.00nm spectrum line, which can eliminate the interference of copper on bismuth during the measurement process. The recovery rate of bismuth content in the smoke and dust determined by this method is 99.0%~101.1%, the relative standard deviation is 1.51%, and the result is accurate and reliable.

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李超,李义,田强坤. ICP-OES法测定铜冶炼烟尘中铋含量[J].中国有色冶金,2021,50(2):77-80

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  • 收稿日期:2020-09-16
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  • 在线发布日期: 2025-12-24
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