Determination of thallium in manganese ore by inductively coupled plasma atomic emission spectrometry afterion exchange separation
XIE Xiao-yan1, WU Wen-qi1, LI Fen1, LIAO Hong-mei2 , LIU Yuan-yuan1
1. Liuzhou Entry-Exit Inspection and Quarantine Bureau, Liuzhou 545006, China; 2. The Technology Center of Guangxi Entry-Exit Inspection and Quarantine Bureau, Nanning 530022, China
Abstract：The manganese ore was dissolved with hydrochloric acid, nitric acid, hydrofluoric acid and perchloric acid. The pH of sample solution was adjusted to 1.7-2.0 with sodium hydroxide solution. The Tl(Ⅰ) in solution was oxidized to Tl(Ⅲ) with bromine water. After D401 ion exchange resin column and elution with 0.015 mol/L of nitric acid, the Tl(Ⅲ) on column was reduced to Tl(Ⅰ) with 2 mL of 3 g/L sulfurous acid solution. Then, the Tl(Ⅰ) was eluted with 0.015 mol/L nitric acid solution. The Tl 190.857 nm was selected as the analytical line. The content of thallium in solution after separation was determined by inductively coupled plasma atomic emission spectrometry. The detection limit of method was 1 ng/mL, and the lower determination limit was 0.8 μg/g. The interference test results showed that tolerant amount of co-existing ions for 0.1 μg/mL of thallium was listed as following (in μg/mL): iron (50); manganese (2); aluminum, cadmium, chromium, nickel, lead and zinc (10). The general manganese ore samples were separated and determined according to the experimental method. The iron, manganese, aluminum, cadmium, chromium, nickel, lead and zinc did not interfere with the determination of thallium. The thallium in manganese ore sample was determined according to the experimental method. The relative standard deviations (RSD, n=8) of determination results were between 1.6% and 11%, and the recoveries of standard addition were between 90% and 108%.
广西壮族自治区人民政府办公厅.广西壮族自治区全面深入开展环境安全隐患大清查大整治行动方案[J].安全生产与监督,2013(8):7-12.The General Office of the Guangxi Zhuang Autonomous Region People's Government.Fully carry out a large inventory of environmental safety risks remediation action plan of the Guangxi Zhuang Autonomous Region[J].Work Safety & Supervision,2013(8):7-12.
[2]
张利群,王晓辉,宋晓春,等.电感耦合等离子体原子发射光谱法测定锑精矿中铅硒碲铊[J].冶金分析,2012,32(4):50-53.ZHANG Li-qun,WANG Xiao-hui,SONG Xiao-chun,et al. Determination of plumbum,selenium,tellurium,thallium in antimony concentrates by inductively coupled plasmatomic emission spectrometry[J].Metallurgical Analysis,2012,32(4):50-53.
[3]
李连仲,林海.亚甲基蓝-萃取荧光法测定痕量铊[J].岩矿测试,1990,9(1):24-29.LI Lian-zhong,LIN Hai.Extraction-fluorimetic determination of thallium with methylene blue[J].Rock and Mineral Analysis,1990,9(1):24-29.
[4]
陈金武,曾法刚,沈慧君.甲基异丁基酮负载泡塑富集-原子吸收测定岩矿中痕量金银铊镉[J].岩矿测试,1993,12(2):85-88.CHEN Jin-wu,ZENG Fa-gang,SHEN Hui-jun.Determination of trace of gold,silver,thallium ang cadmium by AAS after concentration with MIBK loaded polyurethane foam[J].Rock and Mineral Analysis,1993,12(2):85-88.
[5]
吴惠明,郭慧清,陈永亨,等.活性炭吸附分离-分光光度法测定硫化矿和土壤中的痕量铊[J].岩矿测试,2001,20(4):275-278.WU Hui-ming,GUO Hui-qing,CHEN Yong-heng,et al. Spectrophotometric determination of trace thallium in geological samples using activated carbon as an adsorption-separation material[J].Rock and Mineral Analysis,2001,20(4):275-278.
[6]
吴惠明,陈永亨,刘浓.地质样品中痕量铊的纸色谱法分离-分光光度法测定[J].分析测试学报,2003,22(4):86-88.WU Hui-ming,CHEN Yong-heng,LIU Nong.Determination of trace thallium in geological samples by paperchromatography with spectrophotometric detection[J].Journal of Instrumental Analysis,2003,22(4):86-88.
[7]
董云会,张少全.痕量铊的液膜分离富集与测定[J].分析科学学报,2005,21(2):191-193.DONG Yun-hui,ZHANG Shao-quan.Determination of trace thallium after liquid membrane separation and enrichment[J].Journal of Instrumental Analysis,2005,21(2):191-193.
[8]
李玉珍,饶竹,朱玉伦.410哌啶树脂在分离富集中的应用研究Ⅱ.岩矿中痕量金银铊镓铟的分离富集[J].岩矿测试,1993,12(1):1-5.LI Yu-zhen,RAO Zhu,ZHU Yu-lun.Separation and preconcentration of trace elements with piperidine resinⅡ.separation of gold,silver,thallium,gallium and indium in rocks and minerals[J].Rock and Mineral Analysis,1993,12(1):1-5.
[9]
Strelow F W E.An ion exchange selectivity scale of cations based on equilibrium distribution coefficients[J]. Anal. Chem., 1960, 32(9):1185-1188.
[10]
周锦帆,王慧,吴骋,等.离子交换分离的试验技巧及研究方法[J].理化检验:化学分册,2010,46(8):960-962.ZHOU Jin-fan,WANG Hui,WU Pin,et al. Test techniques and research methods of ion exchange separation[J].Physical Testing and Chemical Analysis Part B: Chemical Analysis,2010,46(8):960-962.
