Determination of barium sulfate in beneficiation process sample of barite by inductively coupled plasma atomic emission spectrometry
MAO Xiang-ju1,2, NI Wen-shan*1,2, XIAO Fang1,2, GAO Xiao-fei1,2, ZHANG Hong-li1,2
1. Zhengzhou Institute of Multipurpose Utilization of Mineral Resources, Chinese Academy of Geological Sciences, Zhengzhou 450006, China; 2.China National Engineering Research Center for Utilization of Industrial Minerals, Zhengzhou 450006, China
Abstract：The sample was dissolved at low temperature by diluted hydrochloric acid and filtrated for eliminating the impurities such as BaCO3, BaCl2, CaSO4 and other substances which were dissolved easily in HCl. The precipitate and filter paper was melted at high temperature with Na2CO3 followed by hot water leaching. The filtration was conducted again, and the precipitate was then dissolved with HNO3-HClO4. Then the content of Ba in sample solution was determined by inductively coupled plasma atomic emission spectrometry(ICP-AES) under optimal instrumental parameters with Ba 233.527{144} nm as analytical line. Thus, the content of BaSO4 in sample was indirectly calculated. Based on this, a determination method of barium sulfate in beneficiation process sample of barite (raw ore, tailing, middling and concentrate) was established by ICP-AES after Na2CO3 fusion. The results indicated that there was no obvious spectral interference by other elements at wavelength of Ba 233.527{144} nm. The mass concentration of Ba in range of 12-36 μg/mL showed good linearity to the corresponding emission intensity. The linear correlation coefficient of calibration curve was r=0.999 9. The detection limit of method for Ba was 0.14 μg/mL, which was equivalent to 0.24 μg/mL for BaSO4. The content of BaSO4 in the actual samples of raw ore, tailing, middling and concentrate in beneficiation process of barite was determined according to the experimental method. The results were consistent with those obtained by gravimetric method. The relative standard deviations (RSD, n=6) were between 0.39% and 4.1%.
罗道成,易平贵,陈安国,等.EDTA络合滴定法测定硅钙钡合金中钙和钡[J].冶金分析,2002,22(2):47-48.LUO Dao-cheng,YI Ping-gui,CHEN An-guo,et al.Determination of calcium and barium in calsibar alloy by EDTA complexometric titration[J].Metallurgical Analysis,2002,22(2):47-48.
[4]
王玉春,王瑞斌.EDTA置换滴定法准确测定氯化钡中钡含量[J].科学技术与工程,2009,9(4):988-993.WANG Yu-chun,WANG Rui-bin.Accurate determination of barium content in barium chloride by EDTA displacement titration[J].Science Technology and Engineering,2009,9(4):988-993.
[5]
刘建华,戴文杰,常欢.EDTA络合滴定法联合测定硅钙钡镁合金中钙钡镁[J].冶金分析,2015,35(2):70-73.LIU Jian-hua,DAI Wen-jie,CHANG Huan.Combined determination of calcium,barium,magnesium in silicon-calcium-barium-magnesium alloy by EDTA complexometric titration[J].Metallurgical Analysis,2015,35(2):70-73.
[6]
张博丽.火焰原子吸收光谱法测定硫酸钡中的游离钡[J].无机盐工业,2012,44(2):60-61.ZHANG Bo-li.Determination of free barium in barium sulphate by atomic absorption spectrometry[J].Inorganic Chemicals Industry,2012,44(2):60-61.
[7]
季海冰,刘劲松,庞晓露.石墨管涂覆-塞曼效应石墨炉原子吸收法测定土壤和沉积物中钡[J].光谱学与光谱分析,2007,27(11):2349-2352.JI Hai-bing,LIU Jin-song,PANG Xiao-lu.Determination of trace barium in soil and sediment by Zeeman graphite AAS with coated graphite tube [J].Spectroscopy and Spectral Analysis,2007,27(11):2349-2352.
[8]
倪文山.氢氧化镁共沉淀-电感耦合等离子体原子发射光谱法测定矿石样品中钍[J].冶金分析,2013,33(1)13-16.NI Wen-shan.Determination of thorium in mineral samples by inductively coupled plasma atomic emission spectrometry after preconcentration through coprecipitation of magnesium hydroxide [J].Metallurgical Analysis,2013,33(1):13-16.
[9]
A A Menegario,A J Silva,E Pozzi,et al.On-line determination of Sb(III) and total Sb using baker′s yeast immobilized on polyurethane foam and hydride generation inductively coupled plasma optical emission spectrometry [J].Spectrochimica Acta Part B:Atornic spectroscopy,2006,61(9):1074-1079.
[10]
S Karthikeyan,S Hirata.Simultaneous determination of arsenic(III) and arsenic(IV) by flow injection-inductively coupled plasma-atomic emission spectrometry (ICP-AES) with ultrasonic nebulization [J].Analytical Bioanalytical and Chemistry,2003,375(1):139-144.
[11]
C Z Hang,B Hu,Z C Jiang,et al.Simultaneous on-line preconcentration and determination of trace metals in environmental samples using a modified nanometer-sized alumina packed micro-column by flow injection combined with ICP-OES[J].Talanta,2007,71(3):1239-1245.
[12]
岩石矿物分析编写组.岩石矿物分析:第1分册 [M].3版.北京:地质出版社,1991:204.
[13]
李蓉,任轶,王劲榕,等.含铅重晶石中硫酸钡的测定[J].云南冶金,2014,43(4):62-65.LI Rong,REN Yi,WANG Jin-rong,et al.Determination of barium sulfate in lead-bearing barite[J].Yunnan Metallurgy,2014,43(4):62-65.
[14]
李芳,杨秀环,唐宝英,等.ICP-AES直接测定土壤、沉积物中常、微量元素的光谱干扰和校正方法研究[J].光谱学与光谱分析,2000,20(4):501-506.LI Fang,YANG Xiu-huan,TANG Bao-ying,et al. Studies on spectral interferences and correction in simultaneous determination of multielements in sediments with ICP-AES[J].Spectroscopy and Spectral Analysis,2000,20(4):501-506.
[15]
万家亮,金泽祥.ICP中钨基体对三十种元素的光谱干扰[J].分析化学,1989,17(11):1031-1032.WAN Jia-liang,JIN Ze-xiang.Spectral interference of wolfram matrix with thirty elements by ICP-AES[J].Analytical Chemistry,1989,17(11):1031-1032.
[16]
刘坤杰,李文军,李建强,等.ICP-AES分析法中铁基体非光谱干扰效应的机理研究[J].光谱学与光谱分析,2011,31(4):1110-1114.LIU Kun-jie,LI Wen-jun,LI Jian-qiang,et al.A study of non-spectral interference of iron matrix and its mechanisms in ICP-AES analysis[J].Spectroscopy and Spectral Analysis,2011,31(4):1110-1114.
郑国经,ICP-AES分析技术的发展及其在冶金分析中的应用[J].冶金分析,2001,21(1):36-43.ZHENG Guo-jing.Development of ICP-AES and its application in metallurgical analysis [J].Metallurgical Analysis,2001,21(1):36-43.
[19]
叶苑才,孟广政,杨菊亭,等,ICP-AES法在钢铁及其合金分析中的应用[J].光谱学与光谱分析,1991,11(4):61-70.YE Yuan-cai,MENG Guang-zheng,YANG Ju-ting,et al.Analysis of iron and steel by ICP-AES [J].Spectroscopy and Spectral Analysis,1991,11(4):61-70.
