Abstract:Iron-silicon-aluminum(Fe-Si-Al) alloy is an important magnetic material composed of silicon(7%-9.5%),aluminum(5%-6.5%) and iron matrix.The content of carbon impurity will reduce the magnetic conductivity of Fe-Si-Al alloy,and should be accurately monitored.At present,there are no standard analysis methods for carbon in Fe-Si-Al alloy,and the application studies are in lack.In this study,the method for the determination of carbon content in Fe-Si-Al alloy by high frequency induction combustion infrared absorption method was established.The effect of sample mass and flux on the determination results was investigated.The following conditions were obtained:0.2-0.3 g of sample was accurately weighed and then fused with ternary flux(1.5 g of tungsten+0.20 g of iron and 0.30 g of tin).The calibration curve of instrument was established using the certified reference materials of steel,and the linear correlation coefficient was 0.999 1.The content of carbon in the certified reference materials of steel was analyzed using the calibration curve,and the found results were consistent with the standard values.The limit of detection was 6 μg/g,and the limit of quantification was 21 μg/g.The Fe-Si-Al alloy with carbon of 0.005%-0.020% was determined according to the experimental method.The relative standard deviations(RSDs,n=6-7) of determination results were less than 8%,and the recoveries were between 89% and 110%.
[1] 中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 21219—2007 磁性材料 分类[S].北京:中国标准出版社,2007. [2] 王寿良.铁硅铝磁粉芯生产工艺的研究[C]//中国磁性材料行业与市场发展论坛暨磁性材料与器件行业协会六届一次会员大会论文集.上海:中国电子元件行业协会、中国电子材料行业协会、全国磁性材料与器件行业协会,2011. [3] 叶倡华,黄钧声.铁硅铝软磁粉芯研究进展[J].材料研究与应用,2016,10(1):1-4,32. YE Changhua,HUANG Junsheng.Progress on the research of FeSiAl soft magnetic powder cores[J].Materials Research and Application,2016,10(1):1-4,32. [4] 中华人民共和国工业和信息化部.YS/T 1485—2021 铁硅铝基复合吸波材料[S].北京:冶金工业出版社,2021. [5] 刘攀,唐伟,张斌彬,等.高频感应燃烧-红外吸收法在分析金属材料中碳、硫的应用[J].理化检验(化学分册),2016,52(1):109-118. LIU Pan,TANG Wei,ZHANG Binbin,et al.Application of high frequency induction combustion-infrared absorption spectroscopy for analysis of carbon or sulfur in metal materials[J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis),2016,52(1):109-118. [6] 刘攀,唐伟,张斌彬,等.高频感应燃烧-红外吸收光谱法在分析无机非金属样品中碳、硫的应用[J].理化检验(化学分册),2016,52(4):487-496. LIU Pan,TANG Wei,ZHANG Binbin,et al.Application of high frequency induction combustion-infrared absorption spectrometry to the determination of carbon or sulfur in inorganic non-metal samples[J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis),2016,52(4):487-496. [7] 刘攀,杜米芳,唐伟,等.无机固体样品中碳的分析方法综述[J].分析仪器,2018(4):8-15. LIU Pan,DU Mifang,TANG Wei,et al.Review of methods for analysis of carbon in inorganic solid samples[J].Analytical Instrumentation,2018(4):8-15. [8] 孙竹,向前,黄双,等.硅钢中C、N、O元素红外分析方法的研究[C]//2010年第十一届中国电工钢专业学术年会论文集.厦门:中国金属学会电工钢分会,2010. [9] 董珍萍,徐仁启.用CCS-140型高频红外碳硫分析仪测定硅钢中微量碳和硫[J].理化检验(化学分册),1996,32(3):174. DONG Zhenping,XU Renqi.Determination of trace carbon or sulfur in silicon steel using CCS-140 high frequency-infrared analyzer[J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis),1996,32(3):174. [10] 杨志,张颖,申茜辉,等.燃烧红外吸收法测定硅铝铁合金中的碳[J].天津冶金,2003(5):40-42. YANG Zhi,ZHANG Ying,SHEN Qianhui,et al.Measurement of carbon in Si-Al-Fe alloy with infrared absorption method[J].Tianjin Metallurgy,2003(5):40-42. [11] 刘攀,张毅,常国梁,等.高频感应燃烧红外吸收法测定铁硅硼非晶合金薄带中碳[J].冶金分析,2020,40(9):24-30. LIU Pan,ZHANG Yi,CHANG Guoliang,et al.Determination of carbon in iron-silicon-boron amorphous alloy strip by high frequency combustion infrared absorption method[J].Metallurgical Analysis,2020,40(9):24-30. [12] 刘攀,张毅,张健豪.单点校准线性测量系统不确定度的蒙特卡洛法评定模型构建与应用[J].冶金分析,2020,40(8):22-29. LIU Pan,ZHANG Yi,ZHANG Jianhao.Evaluation of the uncertainty for the single-point calibration linear measurement system based on Monte Carlo method[J].Metallurgical Analysis,2020,40(8):22-29. [13] 李广杰,杨柳,杨大蔚.助熔剂在碳硫分析中的使用[C]//2012国际冶金及材料分析测试学术报告会论文集.北京:中国金属学会,2012. [14] 刘瑞,李会影.红外吸收法在钒中碳分析中的应用研究[J].材料开发与应用,2017,32(4):50-54. LIU Rui,LI Huiying.Study on the application of infrared absorption method in carbon analysis of vanadium[J].Development and Application of Materials,2017,32(4):50-54. [15] 冯丽丽,宋飞,张庆建,等.高频燃烧红外吸收光谱法测定铅精矿中的硫[J].中国无机分析化学,2021,11(6):46-50. FENG Lili,SONG Fei,ZHANG Qingjian,et al.Sulfur determination in lead concentrate by high frequency combustion infrared absorption method[J].Chinese Journal of Inorganic Analytical Chemistry,2021,11(6):46-50.