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电感耦合等离子体原子发射光谱法测定耐火材料中的硫含量

Determination of sulfur content in refractories by inductively coupled plasma atomic emission spectrometry
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摘要 以无水碳酸钠和硼酸为混合熔剂,于1000℃保温10 min熔融试样,再用盐酸溶解后采用ICP-AES法测定耐火材料中硫含量。探讨了仪器测量条件、试样分解方法、基体干扰、共存元素、分析谱线等因素对结果的影响,确定了ICP-AES法的最佳试验条件,并进行准确度和精密度试验。结果表明:硫分析谱线为182.034 nm,校准工作曲线的线性相关系数达到了0.9999以上,线性关系非常好,测试灵敏度高,稳定性好,共存元素干扰小,标准物质的检测结果精密度和准确度均高,其相对标准偏差(n=6)在3%以内,满足生产检测需求。 The sulfur content in refractories was determined by inductively coupled plasma atomic emission spectrometry(ICP-AES)using anhydrous sodium carbonate and boric acid as the fluxing agents,heating at 1000℃for 10 min and dissolving in hydrochloric acid.The influence of the instrument working conditions,sample decomposition methods,matrix effect,coexisting elements and analysis spectral lines on the results was discussed to determine the optimum test conditions.The accuracy and precision tests were carried out.The results show that using the sulfur analysis spectral line of 182.034 nm,the correlation coefficient of the calibration curve is above 0.9999,indicating good linear relationship;the method also presents high sensitivity,good stability,and low interference of coexisting elements;meanwhile,the results of the reference materials present good precision and accuracy with the relative standard deviation(n=6)less than 3%,which meets the test requirements.
作者 王燕妮 张亚静 韩丹 雷小雨 Wang Yanni;Zhang Yajing;Han Dan;Lei Xiaoyu(Sinosteel Luoyang Institute of Refractories Research Co.,Ltd.,Luoyang 471039,Henan,China)
出处 《耐火材料》 CAS 北大核心 2020年第6期550-552,共3页 Refractories
关键词 电感耦合等离子体原子发射光谱法 耐火材料 硫含量 inductively coupled plasma atomic emission spectrometry refractories sulfur content
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