Determination of lead and cadmium in regenerated zinc by inductively coupled plasma atomic emission spectrometry after extraction separation with strongly basic anion exchange fiber
Abstract：During the direct determination of lead and cadmium in regenerated zinc by inductively coupled plasma atomic emission spectrometry (ICP-AES), the coexisting elements such as zinc and iron would cause interference. When the content of zinc in testing solution was 20 times higher than that of lead and cadmium, the relative error of both lead and cadmium by direct determination was higher than 5%. In fact, the content of zinc in regenerated zinc was much higher than this fold compared to lead and cadmium. In presence of I-, it was found that Pb2+ and Cd2+ in regenerated zinc sample could form PbI2-4 and CdI2-4 complex anions with the structure of 8-hydroxyquinoline chelate. Meanwhile, the cations such as Zn2+, Fe2+ and Ca2+ would not react with I- to form complex anions. PbI2-4 and CdI2-4 in solution were extracted with strongly basic anion exchange fiber (SBAEF). SBAEF could specifically absorb 8-hydroxyquinoline chelates (PbI2-4 and CdI2-4), realizing the separation of lead and cadmium from interference elements including zinc, iron and calcium. Then PbI2-4 and CdI2-4 were simultaneously eluted with EDTA solution for the determination by ICP-AES. Thus the determination method of lead and cadmium in regenerated zinc was established. The proposed method could effectively eliminate the interference of coexisting elements such as zinc and iron. The determination range was 0.10%≤wPb≤10.00% and 0.050%≤wCd≤5.00%. The proposed method was applied to the determination of lead and cadmium in actual samples of regenerated zinc. The relative standard deviations (RSD, n=5) of determination methods were between 0.89% and 1.7%, and the recoveries were between 99% and 101%. The contents of lead and cadmium in certified reference material of zinc concentrate with similar composition to regenerated zinc were determined according to the experimental method. The found results were consistent with the certified values. The simulated solution of regenerated zinc was determined according to the experimental method. The recoveries of lead and cadmium were between 97% and 104%.
吴雪英,魏雅娟,刘晓玲,等.EDTA滴定法测定再生锌原料中铁[J].冶金分析,2016,36(5):53-57.WU Xue-ying,WEI Ya-juan,LIU Xiao-ling,et al.Determination of iron in regenerated zinc by EDTA titration[J].Metallurgical Analysis,2016,36(5):53-57.
[2]
江荆,魏雅娟,伍斯静,等.强碱性阴离子交换纤维吸附-电感耦合等离子体原子发射光谱法测定含锌物料中镉[J].冶金分析,2016,36(12):38-43.JIANG Jing,WEI Ya-juan,WU Si-jing,et al.Determination of cadmium in zinc containing materials by adsorption-inductively coupled plasma atomic emission spectrometry with strongly alkaline anion exchange fibers[J].Metallurgical Analysis,2016,36(12):38-43.
[3]
向德磊.EDTA滴定法测定铅冶炼原料中铅含量结果正确度的探讨[J].冶金分析,2016,36(8):35-40.XIANG De-li.Discussion on the accuracy of determination of lead content in lead smelting raw materials by EDTA titration[J].Metallurgical Analysis,2016,36(8):35-40.
[4]
胡健平,王日中,杜宝华,等.火焰原子吸收光谱法和电感耦合等离子体发射光谱法测定硫化矿中的银铜铅锌[J].岩矿测试,2018,37(4):388-395.HU Jian-ping,WANG Ri-zhong,DU Bao-hua,et al.Determination of silver,copper,lead and zinc in sulfide ore by flame atomic absorption spectrometry and inductively coupled plasma emission spectrometry[J].Rock and Mineral Analysis,2008,37(4):388-395.
[5]
黄俭惠,卢汉堤.火焰原子吸收光谱法测定高锑烟尘中的银、铅、镉[J].中国无机分析化学,2014,4(4):28-31.HUANG Jian-hui,LU Han-ti.Determination of silver,lead and cadmium in high antimony dust by flame atomic absorption spectrometry[J]. Chinese Journal of Inorganic Analytical Chemistry,2014,4(4):28-31.
[6]
王松君,常平,王璞珺,等.电感耦合等离子体发射光谱法直接测定黄铜矿中多元素[J].岩矿测试,2004,23(3):228-230.WANG Song-jun,CHANG Ping,WANG Pu-jun,et al.Direct determination of multiple elements in chalcopyrite by inductively coupled plasma emission spectrometry[J].Rock and Mineral Analysis,2004,23(3):228-230.
[7]
王奎,张尼,魏增,等.微波消解-电感耦合等离子体质谱法测定砂仁中的铜、铅、砷、镉[J].化学分析计量,2018,27(5):25-28.WANG Kui,ZHANG Ni,WEI Zeng,et al.Determination of copper,lead,arsenic and cadmium in amomum chinensis by microwave digestion-inductively coupled plasma mass spectrometry[J].Chemical Analysis and Meterage,2008,27(5):25-28.
GONG Qi,WEI Xiao-ling,WU Jing-na,et al.A solid phase extraction method for determination of trace gal-lium in aluminum iron samples by atomic spectrometry[J].Journal of Analytical Atomic Spectrometry,2012,27(11):1920-1927.
[11]
杨姝丽,余焘,龚琦.强碱性阴离子交换纤维富集-石墨炉原子吸收光谱法测定海水中痕量铅和镉[J].理化检验:化学分册,2017,53(2):172-176.YANG Shu-li,YU Tao,GONG Qi.Determination of trace amounts of lead and cadmium in seawater with strong alkaline anion exchange fiber enrichment using graphite furnace atomic absorption spectrometry[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2017,53(2):172-176.
[12]
孟时贤,邓飞跃,杨远,等.电感耦合等离子体发射光谱法测定铅锌矿中15个主次量元素[J].岩矿测试,2015,34(1):48-54.MENG Shi-xian,DENG Fei-yue,YANG Yuan,et al.Determination of fifteen primary and secondary elements in lead-zinc ore by inductively coupled plasma emission spectrometry[J].Rock and Mineral Analysis,2015,34(1):48-54.
