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电感耦合等离子体原子发射光谱法测定炼钢促进剂中低含量三氧化二铁

Determination of low content of iron oxide in steelmaking promoter by inductively coupled plasma atomic emission spectrometry

  • 摘要: 针对炼钢促进剂中三氧化二铁含量检测标准与产品标准范围不匹配,以及现行检测方法存在不足的问题,本文建立了电感耦合等离子体原子发射光谱法(ICP-AES)测定炼钢促进剂中低含量三氧化二铁(w≤5%)的分析方法。样品经盐酸加热溶解、过滤后,将残渣灰化,再以碳酸钠-硼酸混合熔剂(mm=2∶1)熔融,熔融物经盐酸浸取后合并于滤液,稀释后上机测定。系统考察了溶样方式与基体干扰等关键条件,结果表明:酸溶结合碱熔融法对炼钢促进剂样品溶解效果最佳;铝基体对三氧化二铁测定存在干扰,本实验采用基体匹配法绘制校准曲线,即通过使标准溶液系列中的铝基体与待测样品溶液基本保持一致,以消除基体效应的影响。三氧化二铁含量为0.01%~5.00%(质量分数)时,校准曲线线性关系良好,相关系数为0.999 9;方法检出限为0.003%。按照实验方法测定炼钢促进剂样品中三氧化二铁,结果的相对标准偏差(RSD,n=7)为0.46%~0.70%,分析结果与邻二氮杂菲光度法吻合;F检验结果表明,两种方法无显著性差异。对炼钢促进剂样品进行加标回收试验,加标回收率为95%~100%。

     

    Abstract: In view of the mismatch between the detection standard and product specification range for iron oxide in steelmaking promoter,as well as the deficiencies of current testing methods,an analytical method for the determination of low content of iron oxide (w≤5%) in steelmaking promoter by inductively coupled plasma atomic emission spectrometry(ICP-AES) was established.The sample was dissolved with hydrochloric acid by heating followed by filtration.The residue was ashed and subsequently fused with sodium carbonate-boric acid mixed flux (mm=2∶1).The melt was leached with hydrochloric acid,combined with the original filtrate,diluted to a constant volume,and then determined by instrumental analysis.The key conditions including sample digestion method and matrix interference were systematically investigated.The results showed that the combined acid dissolution and alkali fusion method achieved the best digestion effect for steelmaking promoter samples.The aluminum matrix had interference with the determination of iron oxide.The matrix matching method was adopted to prepare the calibration curve to eliminate the influence of matrix effect in this study,in other words,the aluminum matrix concentration in the standard solution series was basically consistent with that of the sample solution.The calibration curve exhibited good linearity when the iron oxide content(mass fraction) was in range of 0.01%-5.00%,and the correlation coefficient was 0.999 9.The limit of detection(LOD) was 0.003%.The content of iron oxide in steelmaking promoter samples was determined according to the experimental method.The relative standard deviation(RSD,n=7) was 0.46%-0.70%.The analytical results were in good agreement with those obtained by orthophenanthroline spectrophotometry.The results of F-test indicate that there is no significant difference between the two methods.Spiked recovery tests were performed on steelmaking promoter samples,and the recovery was between 95% and 100%.

     

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