Determination of sulfur in titanium concentrate from Panxi area by high frequency combustion infrared absorption method
LIU Lin, WANG Yong*
Panxi Institute of Vanadium and Titanium Inspection and Testing,National Quality Supervision and Inspection Center of Vanadium and Titanium Products,Panzhihua 617000,China
Abstract：Sulfur is one of the important quality indicators for titanium concentrate. The accurate determination of sulfur content is of great significance for subsequent process control and product quality supervision. Since the content range of sulfur in titanium concentrate from Panxi area is relatively wide, the problem of integration delay easily happens for some titanium concentrate samples from Panxi area during the determination of sulfur by high frequency combustion infrared absorption method. On the basis of previous studies, combined with scanning electron microscopy technology and the programmed heating function of infrared carbon sulfur analyzer, a large number of experiments were conducted to investigate the titanium concentrate samples in the four major mining areas from Panxi region. It was found that the differences in morphology and content of sulfides in titanium concentrate were the main reason to cause sulfur integration delay. By optimizing analysis conditions such as flux type, flux dosage, flux and sample addition sequence, and instrument analysis power, etc., the problem of sulfur integration delay was solved, and the determination range of sulfur was expanded. Consequently, the determination of sulfur in range of 0.004%-4.77%(mass fraction, the same below) in titanium concentrate from Panxi area was realized by high frequency combustion infrared absorption method. The optimized experimental conditions were listed as follows: 0.20 g of sample was selected; 0.50 g of iron particle, 0.30 g of copper particle and 1.50 g of tungsten particle were used as the flux; the flux and sample addition sequence was iron particle, copper particle, sample, tungsten particle; the analytical power was 95%. The reference materials of titanium concentrate with different sulfur contents were used to draw calibration curve. When the content of sulfur was in range of 0.004%-0.201% (low sulfur), the linear equation of calibration curve was y=1.006 5x-1.45×10-6 with correlation coefficient of 0.999 7. When the content of sulfur was in range of 0.201%-4.77% (high sulfur), the linear equation of calibration curve was y=1.002 1x-1.16×10-6 with correlation coefficient of 0.999 8. The limit of detection of this method was 0.000 1%. The contents of sulfur in samples from Panxi mining area and reference materials of titanium concentrate were determined for 7 times according to the proposed method. For reference materials, the results were within the allowable ranges of standard values, and the relative standard deviations(RSDs) were between 1.2% and 2.0%. For actual samples, RSDs of deteramination results were between 0.28% and 0.60%.
刘林, 王勇. 高频燃烧红外吸收法测定攀西地区钛精矿中硫[J]. 冶金分析, 2024, 44(6): 74-80.
LIU Lin, WANG Yong. Determination of sulfur in titanium concentrate from Panxi area by high frequency combustion infrared absorption method. , 2024, 44(6): 74-80.
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