Determination of iron sulfide in iron ore by inductively coupled plasma atomic emission spectrometry with microwave digestion
ZHENG Zhi-kang1,2, QIAO Zhao-yu3, WANG Jia-song*1,2, ZHANG Nan1,2, ZENG Jiang-ping1,2,4, WANG Li-qiang1,2
1. Tianjin Center, China Geological Survey, Tianjin 300170, China; 2. North China Center for Geoscience Innovation, Tianjin 300170, China; 3. China Inspection (Tianjin) Testing Co., Ltd., Tianjin 300300, China; 4. Key Laboratory of Geological Environment of Muddy Coastal Zone, China Geological Survey, Tianjin 300170, China
Abstract：The accurate determination of iron sulfide in iron ore has great significance on the phase analysis of iron ore. At present, the system analysis method was usually used for the pretreatment of iron sulfide in iron ore. Although this method was relatively mature, there were still some problems such as complicated procedures, incomplete separation and easy loss of iron sulfide components, which easily caused inaccurate determination results. The comparative experiments of various sample dissolution methods were conducted. The mixed solution of saturated bromine water and potassium permanganate was selected for the direct leaching iron ore to completely leach iron sulfide. Moreover, the comparative experiments of various dilution methods were conducted, and the mixture of ammonium fluoride and hydrochloric acid was adopted for the leaching medium to inhibit the hydrolysis of iron to the full extent. Then the content of iron sulfide(in term of iron content, the same below) in iron ore was determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The linear correlation coefficient of calibration curve was 0.9999. The limit of detection for iron sulfide was 3μg/g. The proposed method was used to determine the content of iron sulfide in certified reference materials for phase composition analysis of iron ore. The relative standard deviation (RSD, n=8) of determination results were between 1.9% and 3.5%, and the relative errors were between 1.3% and 2.5%. The contents of iron sulfide in three iron ore actual samples were determined according to the proposed method, and RSDs (n=5) were between 0.68% and 3.0%. The proposed method was applicable for the determination of in iron sulfide (0.04%-8%) in iron ore.
毕建玲,孙鹏飞,陈璐,等.电感耦合等离子体发射光谱法在铁矿石物相分析中的应用[J].山东国土资源,2016,32(1):75-77,81.BI Jian-ling,SUN Peng-fei,CHEN Lu,et al.Application in the phase analysis of iron ores by inductively coupled plasma atomic emission spectrometry[J].Shandong Land and Resources,2016,32(1):75-77,81.
[2]
董娇,王微,耿鑫.铁矿石的物相分离及测定[J].辽宁化工,2018,47(4):288-292.DONG Jiao,WANG Wei,GENG Xin.Phase separation and determination of iron ore[J].Liaoning Chemical Industry,2018,47(4):288-292.
[3]
于春波.铁矿石物相分析检测方法的研究与应用[J].中国检验检测(China Inspection Body & Laboratory),2018,26(2):18-22.
[4]
孟晓龙.铁矿石物相分析与研究[J].中国化工贸易,2013,8(8):258-259.MENG Xiao-long.Phase analysis and research of the iron ore[J].China Chemical Trade,2013,8(8):258-259.
黄正海.饱和溴水浸取硫化铁的一些问题及铁矿石中硫化铁的测定[J].分析化学,1985,13(5):377-379.HUANG Zheng-hai.Some problems about leaching iron sulphides with brominesaturated water and measurement of iron sulphide phase[J].Chinese Journal of Analytical Chemistry,1985,13(5):377-379.
[7]
曾江萍,吴彦涛,谭生芸,等.盐酸-氯化亚锡-氟化铵体系溶样-火焰原子吸收光谱法测定水系沉积物中的低含量黄铁矿[J].分析试验室,2016,35(1):90-92.ZENG Jiang-ping,WU Yan-tao,TAN Sheng-yun,et al.Determination of low-content pyrite in stream sediments by flame atomic absorption spectrometry with hydrochloric acid-stannous chloride-ammonium fluoride dissolving[J].Chinese Journal of Analysis Laboratory,2016,35(1):90-92.
[8]
张金明,边朋沙,程文翠,等.碘量法测定铁矿石中全铁及磁性铁的分析方法探讨[J].冶金分析,2018,38(2):76-81.ZHANG Jin-ming,BIAN Peng-sha,CHENG Wen-cui,et al.Discussion on the analysis method of total iron and magnetic iron in iron ore by iodometry[J].Metallurgical Analysis,2018,38(2):76-81.
[9]
张珂,马明,马龙,等.电位滴定法测定铁矿石中氧化亚铁[J].冶金分析,2018,38(5):66-71.ZHANG Ke,MA Ming,MA Long,et al.Determination of ferrous oxide in iron ore by potentiometric titration method[J].Metallurgical Analysis,2018,38(5):66-71.
[10]
胡跃波,陈靳俊,岳宇超.碱熔-硼氢化钾还原重铬酸钾滴定法测定铁矿石中全铁[J].冶金分析,2015,35(5):77-80.HU Yue-bo,CHEN Jin-jun,YUE Yu-chao.Determination of total iron in iron ore by potassium borohydride reduction-potassium dichromate titration with sample preparation by alkali fusion[J].Metallurgical Analysis,2015,35(5):77-80.
[11]
向晓明,李花,张小林.光度法测定微量铁实验中还原剂的优化选择[J].化学教育,2016,37(24):42-44.XIANG Xiao-ming,LI Hua,ZHANG Xiao-lin.Optimization of reducing agent in spectrophotometric determination of trace iron[J].Chinese Journal of Chemical Education,2016,37(24):42-44.
[12]
赵增兵,苏晗,谢存明,等.硫化钼中总铁含量的测定[J].无机盐工业,2018,50(6):78-80.ZHAO Zeng-bing,SU Han,XIE Cun-ming,et al.Determination of total iron content in molybdenum disulfide[J].Inorganic Chemicals Industry,2018,50(6):78-80.
[13]
吴永明,陶武,黄飞雪,等.邻菲罗啉示差分光光度法测定铁矿石中全铁含量[J].化学试剂,2018,40(1):45-48.WU Yong-ming,TAO Wu,HUANG Fei-xue,et al.Measurement of total iron content in iron ore by phenanthroline spectrophotometry[J].Chemical Reagents,2018,40(1):45-48.
[14]
朱国忠,徐艳燕,庞燕.连续光源火焰原子吸收光谱法测定氧化镍中钴铜锌铁钙镁[J].冶金分析,2017,37(3):48-52.ZHU Guo-zhong,XU Yan-yan,PANG Yan.Determination of cobalt,copper,zinc,iron,calcium and magnesium in nickel oxide by continuum source flame atomic absorption spectrometry[J].Metallurgical Analysis,2017,37(3):48-52.
[15]
王娜,滕新华,吴彦涛,等.三氯化铝浸取-火焰原子吸收光谱法测定水系沉积物中低含量的碳酸铁[J].岩矿测试,2015,34(2):229-233.WANG Na,TENG Xin-hua,WU Yan-tao,et al.Determination of low-content iron carbonate in stream sediments by flame atomic absorption spectrometry with aluminum chloride extraction[J].Rock and Mineral Analysis,2015,34(2):229-233.
[16]
李颖娜,徐志彬.基于神经网络集成-X射线荧光光谱法的铁矿石中全铁含量的测定[J].冶金分析,2019,39(1):35-41.LI Ying-na,XU Zhi-bin.Determination of total iron in iron ore based on ensembleneural network-X-ray fluorescence spectrometry[J].Metallurgical Analysis,2019,39(1):35-41.
[17]
鲍希波,赵亮,李才红,等.熔融制样-X射线荧光光谱法测定硅锰合金和锰铁合金中硅锰磷铁[J].冶金分析,2019,39(2):51-55.BAO Xi-bo,ZHAO Liang,LI Cai-hong,et al.Determination of silicon,manganese,phosphorus and iron in silicomanganese and ferromanganese alloys by X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgical Analysis,2019,39(2):51-55.
[18]
王斌,李强.电感耦合等离子体原子发射光谱法测定铀矿石中全铁[J].冶金分析,2016,36(4):66-70.WANG Bin,LI Qiang.Determination of total iron in uranium ore by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2016,36(4):66-70.
[19]
曾昭文,郑成,毛桃嫣,等.微波在化工过程中的研究及应用进展[J].化工学报,2019,70(S1):1-14.ZENG Zhao-wen,ZHENG Cheng,MAO Tao-yan,et al.Progress in research and application of microwave in chemical process[J].CIESC Journal,2019,70(S1):1-14.
[20]
胡昌文,刘元生,刘念,等.ICP-OES法测定碱式碳酸钴中镍、铜、铁、钠、锌、钙[J].无机盐工业,2015,47(5):64-65.HU Chang-wen,LIU Yuan-sheng,LIU Nian,et al.Determination of nickel,copper,iron,sodium,zinc and calcium in basic cobalt carbonate by ICP-OES method[J].Inorganic Chemicals Industry,2015,47(5):64-65.
