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高频燃烧红外吸收法测定攀西地区钛精矿中硫

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硫是钛精矿的重要质量指标之一,准确测定其含量,对后续工艺控制及产品质量监管有重要意义.由于攀西地区钛精矿中硫含量范围跨度较大,采用高频燃烧红外吸收法测定攀西地区钛精矿中硫含量时,部分矿区样品易出现积分延迟的问题.实验在前人研究基础上,结合扫描电镜技术及红外碳硫仪的程序升温功能,通过大量试验对攀西地区四大矿区产的钛精矿进行研究,得出了钛精矿中硫化物形态及含量的差异是造成硫积分延迟的主要原因,并通过优化助熔剂种类及其用量、助熔剂与样品添加顺序、仪器分析功率等分析条件,解决了硫积分延迟的问题,拓宽了硫的测定范围,实现了高频燃烧红外吸收法对攀西地区钛精矿中0.004%~4.77%(质量分数,下同)硫的测定.优化后的实验条件如下:样品量为0.20 g,助熔剂为0.50 g铁粒、0.30 g铜粒和1.50 g钨粒,助熔剂和样品的添加顺序为铁粒-铜粒-样品-钨粒,分析功率为95%.采用不同硫含量的钛精矿标准样品建立校准曲线,在硫含量为0.004%~0.201%时(低硫),校准曲线线性方程为y=1.006 5x-1.45 × 10-6,相关系数为0.999 7;在硫含量为0.201%~4.77%时(高硫),校准曲线线性方程为y=1.002 1x1.16 × 10-6,相关系数为0.999 8,方法检出限为0.000 1%.采用实验方法对攀西矿区钛精矿样品及钛精矿标准样品中硫含量平行测定7次,结果表明,标准样品的测定值在标准值的允许范围内,相对标准偏差(RSD)为1.2%~2.0%;样品测定结果的相对标准偏差(RSD)为0.28%~0.60%.
Determination of sulfur in titanium concentrate from Panxi area by high frequency combustion infrared absorption method
Sulfur is one of the important quality indicators for titanium concentrate.The accurate determina-tion of sulfur content is of great significance for subsequent process control and product quality supervi-sion.Since the content range of sulfur in titanium concentrate from Panxi area is relatively wide,the prob-lem 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 determi-nation 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 fre-quency combustion infrared absorption method.The optimized experimental conditions were listed as fol-lows:0.20 g of sample was selected;0.50 g of iron particle,0.30 g of copper particle and 1.50 g of tung-sten particle were used as the flux;the flux and sample addition sequence was iron particle,copper parti-cle,sample,tungsten particle;the analytical power was 95%.The reference materials of titanium concen-trate 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-1.1 6 × 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%.

high frequency combustion infrared absorption methodtitanium concentratePanxi areasulfur

刘林、王勇

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攀西钒钛检验检测院,国家钒钛制品质量检验检测中心,四川攀枝花 617000

高频燃烧红外吸收法 钛精矿 攀西地区

四川省市场监督管理局科技项目

SCSJZ2022019

2024

冶金分析
中国钢研科技集团有限公司(钢铁研究总院) 中国金属学会

冶金分析

CSTPCD北大核心
影响因子:1.124
ISSN:1000-7571
年,卷(期):2024.44(6)
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