Correction of certified values and reuse of metamorphic magnesia standard sample for the determination of magnesium-based refractories by X-ray fluorescence spectrometry
PENG Zhan, MA Hui-xia, LIU Jing, BAI Wan-li
Zhengzhou Non-ferrous Metals Research Institute Co., Ltd., of CHALCO, Zhengzhou 450041, China
Abstract：The standard sample of magnesia is easily metamorphic due to moisture absorption. In order to discuss the possibility of continuing to use the metamorphic standard sample of magnesia, nine metamorphic standard sample of magnesia (the loss on ignition had been changed) were used for condition experiments. The recommended values of metamorphic standard sample of magnesia were corrected. The sample was firstly treated by high temperature burning. Then the type and content of unknown elements were obtained by qualitative and semi-quantitative procedures. Finally, the analysis method of MgO, SiO2, CaO, Al2O3, Fe2O3, K2O, MnO and P2O5 in high-silicon magnesium-based refractories by X-ray fluorescence spectrometry (XRF) based on metamorphic standard sample of magnesia was established after fusion sample preparation. The proposed method was applied for the determination of MgO, SiO2, CaO, Al2O3, Fe2O3, K2O, MnO and P2O5 in one metamorphic standard sample of magnesia 425. The relative standard deviation (RSD, n=11) of determination results of K2O was 11%, and the RSDs (n=11) of other components were all less than 3%. The contents of MgO, SiO2, CaO, Al2O3, Fe2O3, MnO and P2O5 in two metamorphic standard sample of magnesia and two synthetic samples were determined according to the experimental method. The found results were consistent with the certified values or theoretical values. The allowable error could meet the analytical requirements of national standard analysis method. The metamorphic standard samples of magnesia could be recycled.
彭展, 马慧侠, 刘静, 白万里. 用于X射线荧光光谱法测定镁质耐火材料的变质镁砂标样认定值的修正与再利用[J]. 冶金分析, 2019, 39(10): 67-72.
PENG Zhan, MA Hui-xia, LIU Jing, BAI Wan-li. Correction of certified values and reuse of metamorphic magnesia standard sample for the determination of magnesium-based refractories by X-ray fluorescence spectrometry. , 2019, 39(10): 67-72.
边立槐,朱建筑,袁亦秋.镁质耐火材料氧化镁含量化学分析方法的改进[J].天津冶金,2002(4):8-10.BIAN Li-kui,ZHU Jian-zhu,YUAN Yi-qiu.Improvement of chemical analysis method of magnesial content for magnesial refractory materials[J].Tianjin Metallurgical,2002(4):8-10.
[3]
王立新,王烽,曹吉祥,等.冶金仪器分析技术与应用[M].北京:化学工业出版社,2010.
[4]
于杰,刘长春,丁健,等.镁质耐火材料X-射线荧光光谱分析—粉末压片法与熔融玻璃片法之比较[J].辽东学院学报:自然科学版,2012,19(2):80-85.YU Jie,LIU Chang-chun,DING Jian,et al.Determination of magnesite refractory by XRF:a comparison of powder pressed method and glass flux sheet method[J].Journal of Liaodong University:Natural Sciences,2012,19(2):80-85.
苗国玉,杜建民,董中华.镁砂的粉末直接压片法X荧光光谱分析[J].冶金分析,2001,21(1):53-55.MIAO Guo-yu,DU Jian-min,DONG Zhong-hua.X-ray fluorescence spectrometric analysis of magnesia powder pressed into disks[J].Metallurgical Analysis,2001,21(1):53-55.
[7]
王芙云,袁翠菊,任向阳.X射线荧光光谱法快速分析镁质耐火材料中硅铝铁钛钙镁[J].岩矿测试,2008,27(3):232-234.WANG Fu-yun,YUAN Cui-ju,REN Xiang-yang.Rapid determination of SiO2,Al2O3,Fe2O3,TiO2,CaO and MgO in magnesium-based refractory materials by X-ray fluorescence spectrometry with powder pellet sample preparation[J].Rock and Mineral Analysis,2008,27(3):232-234.
[8]
宋祖峰,阚斌,陈健.镁铝铬质耐火材料的X射线荧光光谱分析[J].理化检验:化学分册,2005,41(9):648-653.SONG Zu-feng,KAN Bin,CHEN Jian.XRFS analysis of Mg-Al-Cr refractories[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2005,41(9):648-653.
[9]
唐红霞,付宝荣.X射线荧光光谱法测定镁质耐火材料中的多元素[J].甘肃冶金,2011,33(6):91-93.TANG Hong-xia,FU Bao-rong.Determination of multi-elements in magnesite based refractory materials using X-ray fluorescence spectrometer[J]. Gansu Metallurgy,2011,33(6):91-93.
[10]
张香荣,陈洁,张立新.铝质硅质和镁质耐火材料的X射线荧光光谱快速分析[J].冶金分析,2005,25(1):13-18.ZHANG Xiang-rong,CHEN Jie,ZHANG Li-xin.Rapid analysis of silicon,magnesium and aluminium base refractory materials by XRF[J].Metallurgical Analysis,2005,25(1):13-18.
[11]
赵恩好,岳明新,周国兴,等.X射线荧光光谱法测定镁质耐火材料及其原料中10种成分[J].冶金分析,2013,33(7):62-67.ZHAO En-hao,YUE Ming-xin,ZHOU Guo-xing,et al.Determination of ten components in magnesia refractory materials and raw materials by X-ray fluorescence spectrometry[J].Metallurgical Analysis,2013,33(7):62-67.
[12]
李颖,李长贵,张志刚.X-射线荧光光谱法测定耐火材料组分[J].青海科技(Qinghai Science and Technology),2009,16(2):49-51.
[13]
张鹏,曲月华,王一凌.X射线荧光光谱法测定镁砂、镁石及菱镁矿中主次成分[J].冶金分析,2010,30(9):28-31.ZHANG Peng,QU Yue-hua,WANG Yi-ling.Determination of major and minor elements in magnesia,humite and magnesite by X-ray fluorescence spectrometry[J].Metallurgical Analysis,2010,30(9):28-31.
