硫酸铵存在下碘化钾-丙醇双水相体系萃取分离镉及其应用

doi:10.13228/j.boyuan.issn1000-7571.010104

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摘要试验研究了在硫酸铵存在下碘化物-丙醇双水相体系萃取分离镉的行为及最佳分相条件。考察了络合剂的选择、KI和(NH₄)₂SO₄用量、pH值等反应条件对萃取率的影响。结果表明,体系中加入0.5 mL 200 g/L KI溶液和1.5 g (NH₄)₂SO₄、在pH 值为1~5的介质中,无需使用三苯甲烷类阳离子染料,Cd²⁺与KI络合生成的CdI^2-₄络离子可与丙醇阳离子生成离子缔合物,进而被萃取到丙醇上层。实验方法通过火焰原子吸收光谱法(FAAS)检测萃取后丙醇相中Cd的含量得到证实。Cd²⁺质量浓度在0.20～2.50 μg/mL范围内呈线性关系,相关系数r=0.996 51。干扰试验表明,在±5%的误差范围内,铅烟灰样品中最大质量分数范围内的共存元素(8%Zn、2.5%Fe、2%Cu、0.7%In)不干扰Cd的测定。实验方法应用于铅烟灰中Cd的测定,结果的相对标准偏差(RSD,n=5)在1.8%～2.3%之间,加标回收率在90%～92%之间。

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	左国强
	周鸿燕
	李雅倩
	李全民

关键词 ：镉, 硫酸铵, 碘化钾-丙醇双水相体系, 原子吸收光谱法(AAS)

Abstract：In the presence of ammonium sulfate, the extraction behavior of Cd²⁺ was studied by potassium iodide-propanol aqueous two-phase in the presence of ammonium sulfate, and the optimal conditions of phase separation were selected. The reaction conditions, such as the selection of complexant, the amount of KI and (NH₄)₂SO₄, pH value, on the extraction rate were investigated. Results showed that, without the need of chromogenic agent, CdI^2-₄ can be extracted into the upper layer of propanol by the formation of ion association with propanol cations, in the medium of pH 1-5, when 0.5 mL of 200 g/L KI solution and 1.5 g of (NH₄)₂SO₄ were added. The method was verified through the determination of Cd in the extracted propanol phase by flame atomic absorption spectrometry. The mass concentration of Cd²⁺ was linear in the range of 0.20-2.50 μg/mL. The correlation coefficient is 0.996 51. The interfering experiment shows that Cd²⁺ can be dissociated completely from the coexisting elements in the maximum mass fraction range of lead dust (8%Zn、2.5%Fe、2%Cu、0.7%In), within the error range of ±5%. The proposed method was successfully applied to the determination of cadmium in lead dust. The relative standard deviation (RSD,n=5) was between 1.8%-2.3%, and the recovery of standard addition was between 90%-92%.

Key words： cadmium ammonium sulfate potassium iodide-propanol aqueous two-phase system atomic absorption spectrometry(AAS)

收稿日期: 2017-02-06

基金资助:河南省高等学校重点科研资助项目(16B150008)

作者简介: 左国强(1982－),男,硕士,讲师,主要从事光谱分析研究与教学工作;E-mail: guoqiangzuo@126.com

引用本文:

左国强, 周鸿燕, 李雅倩, 李全民. 硫酸铵存在下碘化钾-丙醇双水相体系萃取分离镉及其应用[J]. 冶金分析, 2017, 37(8): 73-77. ZUO Guo-qiang,ZHOU Hong-yan,LI Ya-qian,LI Quan-min. Extraction of cadmium by potassium iodide-propanol aqueous two-phase systems in the presence of ammonium sulfate and its application. , 2017, 37(8): 73-77.

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