Abstract:Rapid and accurate determination of multiple components in furnace slag is not only the requirement of smelting process,but also the requirement of environmental protection and comprehensive utilization of metallurgical waste.The sample was prepared by pressed powder pellet method with polyester (PET) thin film package in experiments.The calibration samples of furnace slag series with certain content gradient were synthesized using the certified reference materials (CRMs) of furnace slag and high purity substance with the same particle size as the sample to be tested.The calibration curves were fitted.Consequently, a rapid analysis method for the simultaneous determination of SiO2,TFe,Al2O3,CaO,MgO,TiO2,S,P2O5 and TMn in blast furnace slag,converter slag,electric furnace slag and open-hearth furnace slag by X-ray fluorescence spectrometry (XRF) was established.The sample preparation with PET package reduced the dust contamination,which deceased the probability of instrument damage to a minimum.Moreover,it could also prevent the sample from being exposed to the air,thus increasing the preservation time of the sample.The spectral overlapping interference and matrix effect were corrected by adjusting the parameters of instrument analysis, controlling the consistency of sample particle size,and using the TL+ equation of OXSAS software.The spectral overlapping interference and matrix effect in complex system of furnace slag were overcome effectively.The determination of components in furnace slag by XRF with pressed powder pellet was realized.The precision tests of blast furnace slag were performed according to the experimental method.The relative standard deviations (RSD, n=10) of measured results were between 0.16% and 2.1%.The proposed method was applied for the determination of components in CRM and actual samples of blast furnace slag,converter slag,electric furnace slag or open-hearth furnace slag.The found results were in good agreement with the certified values or those obtained by fusion methods.
[1] 王欣,曲月华,王一凌,等.碘-乙醇非水体系分离-重铬酸钾滴定法测定炉渣中金属铁与氧化亚铁[J].冶金分析,2013,33(8):28-32. WANG Xin,QU Yuehua,WANG Yiling,et al.Determination of metallic iron and ferrous oxide in furnace slag by potassium dichromate titration after separation in iodine-ethanol non-aqueous system[J].Metallurgical Analysis,2013,33(8):28-32. [2] 丁美英,乔宇,张桂梅.电感耦合等离子体原子发射光谱法测定炉渣中10种化学成分[J].冶金分析,2011,31(9):38-41. DING Meiying,QIAO Yu,ZHANG Guimei.Determination of ten chemical compositions in slags by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2011,31(9):38-41. [3] 中华人民共和国国家发展与改革委员会,中国国家标准化管理委员会.YB/T 4177—2008 炉渣 X射线荧光光谱分析方法[S].北京:中国标准出版社,2008. [4] 武映梅,罗惠君,林丽芳,等. X射线荧光光谱法测定冶金炉渣中9种成分[J].冶金分析,2010,30(8):7-11. WU Yingmei,LUO Huijun,LIN Lifang,et al.Determination of nine components in metallurgical slag by X-ray fluorescence spectrometry[J].Metallurgical Analysis,2010,30(8):7-11. [5] 杨新能,冯宗平.熔融制样-X射线荧光光谱法测定钒钛渣中10种组分[J].冶金分析,2018,38(7):57-62. YANG Xinneng,FENG Zongping.Determination of ten components in vanadium-titanium slag by X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgical Analysis,2018,38(7):57-62. [6] 童晓民,赵宏风,黄春燕,等.X射线荧光光谱法测定炉渣中13种组分[ J].冶金分析,2005,25(6):12-15. TONG Xiaomin,ZHAO Hongfeng,HUANG Chunyan,et al.Determination of 13 components in slag by X-ray fluorescence spectrometry[J].Metallurgical Analysis,2005,25(6):12-15. [7] 李艳萍,高光洁子,李红,等.X射线荧光光谱法测定FeCuNbSiB纳米晶合金炉渣中9种组分[J].冶金分析,2012,32(4):41-45. LI Yanping,GAO Guangjiezi,LI Hong,et al.Determination of nine components in slag of FeCuNbSiB nanocrystal alloy by X-ray fluorescence spectrometry[J].Metallurgical Analysis,2012,32(4):41-45. [8] 朱春要,顾锋,年季强,等.X射线荧光光谱法测定冶金渣料中主次成分[J].冶金分析,2014,34(8):39-44. ZHU Chunyao,GU Feng,NIAN Jiqiang,et al.Determination of major and minor components in metallurgical slags by X-ray fluorescence spectrometry[J].Metallurgical Analysis,2014,34(8):39-44. [9] 任维萍,冯淑琴,王珺,等.粉末样品的粒度对压片-X射线荧光光谱法测定炉渣准确度的影响[J].冶金分析,2017,37(1):21-25. REN Weiping,FENG Shuqin,WANG Jun,et al.Influence of particle size of powdered sample on the determination accuracy of slag by X-ray fluorescence spectrometry with pressed powder pellet[J].Metallurgical Analysis,2017,37(1):21-25. [10] 张乔,田一光,童晓民.X射线荧光光谱法测定平炉渣中主成分[J].理化检验(化学分册),2006,42(9):756-758. ZHANG Qiao,TIAN Yiguang,TONG Xiaomin.XRFS determination of main components in slags of open hearth furnace[J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis),2006,42(9):756-758. [11] 杨再军.粉末压片-X射线荧光光谱法测定高钛型高炉渣中化学成分[J].理化检验(化学分册),2019,55(4):451-456. YANG Zaijun.Determination of chemical compositions in high-titanium blast furnace slag by X-ray fluorescence spectrometry with powder tablet forming preparation[J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis),2019,55(4):451-456. [12] 段家华,马林泽,张李斌.压片制样-X射线荧光光谱法测定高磷钢渣组分[J].冶金分析,2013,33(5):36-40. DUAN Jiahua,MA Linze,ZHANG Libin.Determination of components in high-phosphorus steel slag by X-ray fluorescence spectrometry with tableting sample preparation[J].Metallurgical Analysis,2013,33(5):36-40. [13] 张殿英,李超,钱菁.X射线荧光光谱法测定转炉渣中8种成分[J].冶金分析,2009,29(6):41-46. ZHANG Dianying,LI Chao,QIAN Jing.Determination of eight components in converter slag by X-ray fluorescence spectrometry[J].Metallurgical Analysis,2009,29(6):41-46. [14] 樊鑫,赵艳兵,张瑞霖.粉末压片制样-X射线荧光光谱法测定炉渣中氟钾钠硫[J].冶金分析,2021,41(7):82-86. FAN Xin,ZHAO Yanbing,ZHANG Ruilin.Determination of fluorine,potassium,sodium and sulfur in slag by X-ray fluorescence spectrometry with pressed powder pellet[J].Metallurgical Analysis,2021,41(7):82-86.