高频燃烧红外吸收法测定黑龙江典型鳞片石墨矿区浮选流程样品中固定碳  

Determination of fixed carbon in floatation process samples from typical flake graphite mine area in Heilongjiang Province by high frequency combustion infrared absorption method

作　　者：肖芳[1,2,3] 赵恒勤 高小飞[1,2,3] 毛香菊 孙启亮[1,2,3] 倪文山 XIAO Fang;ZHAO Heng-qin;GAO Xiao-fei;MAO Xiang-ju;SUN Qi-liang;NI Wen-shan(Zhengzhou Institute of Multipurpose Utilization of Mineral Resources, CAGS, Zhengzhou 450006, China;China National Engineering Research Center for Utilization of Industrial Minerals, Zhengzhou 450006, China;Northwest China Center for Geosience Innovation, Xi′an 710054, China)

机构地区：[1]中国地质科学院郑州矿产综合利用研究所,河南郑州450006 [2]国家非金属矿资源综合利用工程技术研究中心,河南郑州450006 [3]西北地质科技创新中心,陕西西安710054

出　　处：《冶金分析》2020年第4期8-14,共7页Metallurgical Analysis

基　　金：国家自然科学基金青年基金项目(201806149);中国地质调查局地质调查项目(DD20190186,DD20189263)。

摘　　要：鳞片石墨矿浮选流程样品中的固定碳含量是确定浮选实验条件以及浮选实验所能达到选矿指标的重要依据。由于矿样中的碳酸盐、有机物,以及残留在样品表面的碳酸盐浮选药剂、有机浮选药剂等都会对固定碳含量的测定产生干扰,所以实验先将样品在高温下灼烧除去其中的有机碳,用酸将碳酸盐中的碳转化为二氧化碳挥发除去,然后以铁屑和钨锡混合助熔剂进行助熔,以人工配制的石墨矿校准物质绘制校准曲线,建立了高频燃烧红外吸收法测定鳞片石墨矿浮选流程样品中固定碳含量的方法。对称样量、灼烧温度、灼烧时间、酸处理条件和助熔剂用量进行了优化,确定实验条件如下:称样量为0.04000~0.1200g,灼烧温度为470℃,灼烧时间为60min,采用王水(1+4)分解样品中碳酸盐;采用0.5g铁屑和0.8g钨锡混合助熔剂进行助熔。在选定的实验条件下,固定碳质量在1.51~36.24mg范围内与其对应红外吸收信号的积分面积呈良好的线性关系,相关系数为0.9992,方法检出限为0.0053%,定量限为0.015%。将实验方法应用于黑龙江典型鳞片石墨矿浮选流程样品的原矿、粗精矿、中矿、尾矿中固定碳含量的测定,测定值与行业标准JC/T 1021.5—2007中的烧碱石棉吸收重量法基本一致,相对标准偏差(RSD,n=6)为0.83%~2.7%。按实验方法对鳞片石墨矿选流程中任意3个流程样品(原矿、粗精矿、中矿和尾矿)中的固定碳含量进行测定,将其测定值代入浮选流程样品中元素的质量守恒定律公式计算得到第4个流程样品中固定碳的含量,将第4个流程样品中固定碳含量的测定值与其计算值相比可得到第4个流程样品中固定碳的回算率,结果表明,固定碳的回算率为98.4%~105%。The fixed carbon content in flotation process sample of flake graphite is an important basis for determining the flotation conditions and the indexes that can be achieved in flotation experiments.The carbonates and organic matters in sample,as well as the carbonate flotation agents and organic flotation agents remaining on sample surface will cause interference with the determination results of fixed carbon content.Therefore,the organic carbon in sample was firstly removed by burning at high temperature.Meanwhile,the carbon in carbonates was converted into carbon dioxide for evaporation and removal using acids.Then,a mixture of iron filings and tungsten-tin flux was used to facilitate the melting.The calibration curve was established with the artificially prepared calibration materials of graphite ore.The determination method of fixed carbon content in the flake graphite flotation process samples by high frequency combustion infrared absorption was established.The sample mass,burning temperature,burning time,acid treatment conditions and flux dosage were optimized.The following experimental conditions were selected:the sample mass was 0.04000-0.1200g;the burning temperature was 470℃;the burning time was 60min;the carbonates in sample was decomposed using aqua regia(1+4);0.5g of iron filings and 0.8g of tungsten-tin flux was used to facilitate the melting.Under the selected experimental conditions,the mass of fixed carbon in the range of 1.51-36.24mg had a good linear relationship with the integral area of its infrared absorption signal,and the correlation coefficient was 0.9992.The limit of detection was 0.0053%,and the limit of quantification was 0.015%.The proposed method was applied to the determination of fixed carbon content in raw ores,coarse concentrates,middlings and tailings of flotation process samples of typical flake graphite ore in Heilongjiang Province.The found results were basically consistent with those obtained by the caustic soda asbestos gravimetry in industrial standard method(JC/T 1021.5-2

关 键 词：鳞片石墨矿 浮选流程样品 固定碳 高频燃烧红外吸收法 回算率 

分 类 号：O659.2[理学—分析化学] TF033[理学—化学]