Determination of fixed carbon in floatation process samples from typical flake graphite mine area in Heilongjiang Province by high frequency combustion infrared absorption method
XIAO Fang1,2,3, ZHAO Heng-qin1,2,3, GAO Xiao-fei*1,2,3 , MAO Xiang-ju1,2,3, SUN Qi-liang1,2,3, NI Wen-shan1,2,3
1. Zhengzhou Institute of Multipurpose Utilization of Mineral Resources, CAGS, Zhengzhou 450006, China; 2. China National Engineering Research Center for Utilization of Industrial Minerals, Zhengzhou 450006, China; 3. Northwest China Center for Geosience Innovation, Xi′an 710054, China
Abstract：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 1021.5-2007). The relative standard deviation (RSD, n=6) were between 0.83% and 2.7%. The contents of fixed carbon in three random floatation process samples of flake graphite (raw ores, coarse concentrates, middlings and tailings) were determined according to the experimental method. The determination value was substituted into the law of conservation of mass to calculate the fixed carbon content in the fourth process sample. The determination value of fixed carbon content in the fourth process sample was compared with the calculated value to obtain the back-calculation rate. The results showed that the back-calculation rates for the fixed carbon content in the fourth process sample were between 98.4% and 105%.
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XIAO Fang, ZHAO Heng-qin, GAO Xiao-fei , MAO Xiang-ju, SUN Qi-liang, NI Wen-shan. Determination of fixed carbon in floatation process samples from typical flake graphite mine area in Heilongjiang Province by high frequency combustion infrared absorption method. , 2020, 40(4): 8-14.
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