Abstract:Copper-lead-zinc ore was an important raw material for steel smelting, and its sulfur content would directly affect these properties such as of steel brittleness and fluidity. Therefore, the accurate and rapid determination of sulfur content in copper-lead-zinc ore was of great significance for the smelting of copper-lead-zinc ore. Several certified reference materials of copper-lead-zinc ores with similar chemical properties as the actual sample were selected to establish the calibration curve for eliminating the matrix effect. Thus, a determination of sulfur content with mass fraction in range of 0.106%-10.76% in copper-lead-zinc ore was realized by high frequency combustion infrared absorption method with iron and tungsten-tin as flux. The effect of determination conditions such as sample mass, the mass of tungsten-tin flux, comparator level, analysis time and crucible covered or not were discussed. The optimum analytical conditions were obtained as follows: the sample mass was 0.1000g; the mass of tungsten-tin flux was 1.6g; the comparator level was 1%; the analysis time was 50s; the crucible was not covered. The results showed that the linear correlation coefficient of calibration curve was 0.9999. The limit of detection was 0.0264%, and the limit of quantification was 0.106%. Different certified reference materials of copper-lead-zinc ore were determined according to the experimental method. The relative errors were all less than the allowance limit of relative error obtained in accordance with The specification of testing quality management for geological laboratories of DZ/T 0130-2006. The content of sulfur in actual sample of copper-lead-zinc ores was determined parallel for 11 times according to the experimental method. The results were compared with those obtained by combustion iodine method and barium sulfate gravimetry. The relative standard deviation (RSD, n=11) were between 0.50% and 4.6%.
张世文.HCS系列高频红外碳硫分析仪测定铜铅锌矿石中的硫[J].新疆有色金属,2014(S1):145-147.ZHANG Shi-wen.Determination of sulfur in copper,lead and zinc ores by HCS series high frequency infrared carbon and sulphur analyzer[J].Xinjiang Nonferrous Metal,2014(S1):145-147.
[6]
史世云,温宏利,李冰,等.高频燃烧-红外碳硫仪测定地质样品中的碳和硫[J].岩矿测试,2011,20(4):267-271.SHI Shi-yun,WEN Hong-li,LI Bing,et al.Determination of carbon and sulfur in geological samples by high frequency IR-absorption spectrometric method[J].Rock and Mineral Analysis,2011,20(4):267-271.
[7]
王小松,陈曦,王小强,等.高频燃烧-红外吸收光谱法测定钼矿石和镍矿石中的高含量硫[J].岩矿测试,2013,32(4):581-585.WANG Xiao-song,CHEN Xi,WANG Xiao-qiang,et al.Determination of high content sulfur in molybdenum ore and nickel ore using high frequency combustion-infrared absorption spectrometry[J].Rock and Mineral Analysis,2013,32(4):581-585.
[8]
张彦甫,蒋晓光,韩峰.高频燃烧红外吸收法测定高硫铜磁铁矿中硫含量[J].冶金分析,2015,35(6):44-48.ZHANG Yan-fu,JIANG Xiao-guang,HAN Feng.Determination of sulfur in high sulfur copper magnetite by high frequency combustion infrared absorption method[J].Metallurgical Analysis,2015,35(6):44-48.
[9]
姜云军,李星,姜海伦,等.四酸敞口溶解-电感耦合等离子体发射光谱法测定土壤中的硫[J].岩矿测试,2018,37(2):152-158.JIANG Yun-jun,LI Xing,JIANG Hai-lun,et al.Determination of sulfur in soil by inductively coupled plasma-optical emission spectrometry with four acids open dissolution[J].Rock and Mineral Analysis,2018,37(2):152-158.
[10]
柳轶男,姜立强,张书菊,等.CS-800红外碳硫分析仪测定合金钢中的碳和硫[J].光谱实验室,2011,28(4):1958-1962.LIU Yi-nan,JIANG Li-qiang,ZHANG Shu-ju,et al.Determination of carbon and sulfur in alloy steel by CS-800 infrared carbon/sulfur analyzer[J].Chinese Journal of Spectroscopy Laboratory,2011,28(4):1958-1962.
[11]
张明杰,戴雪峰,陆丁荣,等.高频燃烧-红外碳硫仪用于农用地土壤质量调查样品中碳硫的快速测定[J].岩矿测试,2010,29(2):139-142.ZHANG Ming-jie,DAI Xue-feng,LU Ding-rong,et al.Rapid determination of carbon and sulfur in farm land soil samples by high frequency-infrared carbon-sulfur analyzer[J].Rock and Mineral Analysis,2010,29(2):139-142.
[12]
顾涛,王迪民,杨梅,等.高频红外碳硫仪测定土壤/沉积物中总有机碳研究[J].华南地质与矿产,2015,31(3):306-310.GU Tao,WANG Di-min,YANG Mei,et al.Determination of total organic carbon in soil and sediment by high frequency infrared carbon sulfur analyzer[J].Geology and Mineral Resources of South China,2015,31(3):306-310.
[13]
龚仓,付桂花,黄艳波.高频燃烧-红外碳硫仪测定岩心钻探样品中碳硫[J].黄金,2016,37(12):77-80.GONG Cang,FU Gui-hua,HUANG Yan-bo.Determination of carbon and sulfur in drilling core samples by high frequency combustion-infrared carbon and sulfur analyzer[J].Gold,2016,37(12):77-80.
[14]
王宝玲.高频红外吸收法快速测定硫精矿中高含量硫[J].冶金分析,2013,33(8):52-54.WANG Bao-ling.High frequency infrared absorption method for rapid determination of high-content sulfur in sulfur concentrate[J].Metallurgical Analysis,2013,33(8):52-54.
[15]
赵海峰,白云.高频加热-红外线吸收法测定石灰石样品中硫含量[J].分析仪器,2018(3):101-104.ZHAO Hai-feng,BAI Yun.High frequency heating-infrared absorption method for determination of sulfur content in limestone samples[J].Analytical Instrumentation,2018(3):101-104.
[16]
黄启华,徐志强,杨玮玮.高频红外碳硫仪测定重晶石和黄铁矿中的硫[J].岩矿测试,2017,36(2):130-135.HUANG Qi-hua,XU Zhi-qiang,YANG Wei-wei.Determination of sulfur in barite and pyrite by high frequency infrared carbon-sulfur spectrometer[J].Rock and Mineral Analysis,2017,36(2):130-135.
[17]
邓军华,王一凌,亢德华,等.高频燃烧红外吸收法测定磷铁中碳和硫[J].冶金分析,2017,37(3):83-87.DENG Jun-hua,WANG Yi-ling,KANG De-hua,et al.Determination of carbon and sulfur in forrophosphorus by high frequency combustion infrared absorption method[J].Metallurgical Analysis,2017,37(3):83-87.
[18]
吕新明,孙振泽,王东,等.高频燃烧-红外吸收光谱法同时测定铬矿石中碳和硫含量[J].中国无机分析化学,2018,8(3):19-22.LÜ Xin-ming,SUN Zhen-ze,WANG Dong,et al.Simultaneous determination of carbon and sulfur in chromium ores by high frequency combustion-infrared absorption spectrometry[J].Chinese Journal of Inorganic Analytical Chemistry,2018,8(3):19-22.
[19]
郭飞飞,万双,魏中凯,等.无水硫酸钠校准-高频燃烧红外吸收法测定铜精矿中高含量硫[J].冶金分析,2015,35(10):73-76.GUO Fei-fei,WAN Shuang,WEI Zhong-kai,et al.Determination of high content sulfur in copper concentrate by high frequency combustion-infrared absorption method with anhydrous sodium sulfate calibration[J].Metallurgical Analysis,2015,35(10):73-76.