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攀西地区钒钛磁铁矿中硫含量测定方法优化

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硫是钒钛磁铁矿中重要的质量和环保指标,准确测定其含量对后续工艺控制和污染评价具有重要意义.攀西地区钒钛磁铁矿中硫赋存形态多样且含量范围宽,采用高频燃烧红外吸收法测定硫时,部分矿区样品易出现积分延迟、低硫精密度差的问题.本文结合扫描电镜技术及红外碳硫仪的程序升温功能,通过大量实验,得出钒钛磁铁矿中硫化物形态及含量的差异是造成上述问题的主要原因,并通过优化仪器分析功率、助熔剂及添加顺序、样品质量等分析条件,实现高频燃烧红外吸收法对攀西地区钒钛磁铁矿中0.0004%~1.52%硫的测定.优化后的实验条件如下:样品质量0.30g、助熔剂为0.30g铁粒、0.20g铜粒和1.0g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95%.采用不同硫含量的钒钛磁铁矿标准物质建立标准曲线,硫的质量分数为0.0004%~0.200%时(低硫),标准曲线线性方程为y=1.0028x-1.35×10-6(r=0.9998);硫的质量分数为0.201%~1.52%时(高硫),标准曲线线性方程为y=1.0062x-1.49×10-6(r=0.9998),方法检出限为0.0004%.采用本方法对标准物质及攀西地区钒钛磁铁矿实际样品进行测定,标准物质硫含量测定值在标准值的允许范围内,相对标准偏差(RSD)为0.72%~1.40%;实际样品硫含量测定值的RSD为0.40%~0.67%.
Optimization of Sulfur Determination in Vanadium-Titanium Magnetite Ore in the Panxi Area
Sulfur is an important quality and environmental indicator in vanadium-titanium magnetite ore,so the accurate measurement of sulfur is of great significance for subsequent process control and pollution evaluation.There are some problems such as integration delay and poor precision in low sulfur when measuring sulfur in vanadium-titanium magnetite ore with the high-frequency combustion infrared absorption method.To solve the problems,scanning electron microscope(SEM)and infrared absorption carbon-sulfur analyzer with programmed heating function were used,and the analysis conditions such as power,flux and addition sequence,and sample mass were optimized.The optimized experimental conditions were as follows:analysis power of 95%,iron particle flux of 0.30g,copper particle flux of 0.20g,and tungsten particle flux of 1.0g,sample mass of 0.30g.The order of addition is iron-copper-sample-tungsten.The optimized method was used to measure sulfur content,and the results of sulfur in the standard sample were within the allowable error,with satisfactory accuracy.The relative standard deviation(RSD)in samples was 0.40%-0.67%,with satisfactory precision.The range of the method was 0.0004%-1.52%,and the detection limit was 0.0004%.

Panxi areavanadium-titanium magnetite oresulfurhigh-frequency combustion infrared absorption methodmethod optimization

王勇、李子敬、刘林、李国伟

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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

攀西地区 钒钛磁铁矿 高频燃烧红外吸收法 方法优化

四川省市场监督管理局科技项目

SCSJZ2022019

2024

岩矿测试
中国地质学会岩矿测试技术专业委员会 国家地质实验测试中心

岩矿测试

CSTPCD北大核心
影响因子:1.344
ISSN:0254-5357
年,卷(期):2024.43(3)