Abstract:In the process of blast furnace smelting, the condition of the furnace and the quality of molten iron produced can be directly fed back by measuring the chemical composition of the nickel sinter. Due to the lack of matching reference materials and appropriate X-ray fluorescence spectrometry (XRF), the traditional wet method is still used in the industry for the determination of the chemical components of the nickel sinter. The operation is complicated and the measurement period is long. In experiments, the contents of 10 components in nickel sinter (including Ni, TFe, Cr, Mn, SiO2, CaO, MgO, Al2O3, P and TiO2) were determined by XRF with fusion sample preparation. The effects of flux, dilution ratio, release agent, fusion temperature and fusion time on the sample fusion and determination results were discussed. The results showed that the glassy sample was uniform, transparent and free of impurities when prepared under the following conditions: the flux was anhydrous lithium tetraborate-lithium carbonate (mass ratio of 6∶1), the dilution ratio between flux and sample was 20∶1, the release agent was 160 mg of ammonium iodide, the fusion temperature was 1 050 ℃, and the fusion time was 15 min. The certified reference materials of common sinter ore was used as the main body, and the nickel standard solution and high purity chromium trioxide were added in a certain proportion to prepare 11 calibration samples with different content gradients for establishing the calibration curve. The interference of matrix effect could be effectively avoided. The correlation coefficients of calibration curves of various components were in range of 0.999 6-1.000 0. The proposed method was applied to the determination of components in nickel sinter, and the relative standard deviations (RSD, n=10) of the measurement results were between 0.07% and 3.2%. The certified reference materials and actual production samples of the nickel sinter were determined, and the found results were basically consistent with the certified values and those obtained by the traditional wet method. The use of proposed method for the determination of nickel sinter had a good promoting effect on the upgrading of blast furnace smelting process.
[1] 唐萍芝,陈欣,王京.全球镍资源供需和产业结构分析[J].矿产勘查,2022,13(1):152-156. TANG Pingzhi,CHEN Xin,WANG Jing.Analysis of industrial structure and global nickel resources supply and demand [J].Mineral Exploration,2022,13(1):152-156. [2] 朱有康,沈强华,董梦奇,等.红土镍矿冶金工艺现状及前景分析[J].矿冶,2022,31(4):108-113. ZHU Youkang,SHEN Qianghua,DONG Mengqi,et al.Status and prospect analysis of metallurgical process of laterite nickel ore[J].Mining and Metallurgy,2022,31(4):108-113. [3] 张国成,罗果萍,柴轶凡,等.碱度对烧结矿液相形成性能和微观结构特性的影响[J].钢铁研究学报,2021,33(7):584-592. ZHANG Guocheng,LUO Guoping,CHAI Yifan,et al.Effect of basicity on liquid phase formation properties and microstructure of sinter[J].Journal of Iron and Steel Research,2021,33(7):584-592. [4] 潘向阳,龙跃,李神子,等.MgO/Al2O3对烧结矿冶金性能的影响[J].钢铁钒钛,2019,40(4):100-105. PAN Xiangyang,LONG Yue,LI Shenzi,et al.Effect of MgO/Al2O3 on metallurgical properties of sinter[J].I-ron Steel Vanadium Titanium,2019,40(4):100-105. [5] 唐艳云,代梦博,春铁军,等.成分在线检测技术进展及其在铁矿烧结应用趋势[J].烧结球团,2021,46(3):1-8. TANG Yanyun,DAI Mengbo,CHUN Tiejun,et al.Development of online composition detection technology and its application tendency in iron ore sintering[J].Sin-tering and Pelletizing,2021,46(3):1-8. [6] 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 6730.65—2009 铁矿石 全铁含量的测定 三氯化钛还原重铬酸钾滴定法(常规方法) [S].北京:中国标准出版社,2009. [7] 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 6730.39—2017铁矿石 镍含量的测定 丁二酮肟分光光度法[S].北京:中国标准出版社,2017. [8] 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 6730.22—2016 铁矿石 钛含量的测定 二安替吡啉甲烷分光光度法[S].北京:中国标准出版社,2016. [9] 杨新能,陈德,李小青.碱熔-电感耦合等离子体原子发射光谱法测定铁矿石中铬铌钼钨锡[J].冶金分析,2019,39(12):55-60. YANG Xinneng,CHEN De,LI Xiaoqing.Determination of chromium,niobium,molybdenum,tungsten,tin in iron ore by inductively coupled plasma atomic emission spectrometry with alkali fusion[J].Metallurgical Analysis,2019,39(12):55-60. [10] 魏春艳,董玉兰,刘刚耀,等.ICP-AES法测定铁矿石中SiO2,CaO,MgO,Al2O3,MnO和TiO2[J].冶金分析,2004,24(1):58-60. WEI Chunyan,DONG Yulan,LIU Gangyao,et al.Determination of SiO2,CaO,MgO,Al2O3,MnO and TiO2in iron ore by ICP-AES[J].Metallurgical Analysis,2004,24(1):58-60. [11] 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 6730.62—2005 铁矿石 钙、硅、镁、钛、磷、锰、铝和钡含量的测定 波长色散X射线荧光光谱法[S].北京:中国标准出版社,2005. [12] 李敏,周景涛,房尧宇,等.X荧光熔融法测定烧结矿和球团矿中5种组分[J].包钢科技,2019,45(5):93-95,98. LI Min,ZHOU Jingtao,FANG Yaoyu,et al.Determination of five components in sinter and pellet with X-ray fluorescent measurement[J].Science and Technology of Baotou Steel,2019,45(5):93-95,98. [13] 吕善胜,徐金龙,曲强.理论α系数和经验系数法相结合校正-X射线荧光光谱法测定铁矿石中14种组分[J].冶金分析,2016,36(4):46-51. LÜ Shansheng,XU Jinlong,QU Qiang.Determination of fourteen components in iron ore by X-ray fluorescence spectrometry with theoretical α coefficient and empirical coefficient method correction[J].Metallurgi-cal Analysis,2016,36(4):46-51. [14] 吉昂. X射线荧光光谱分析[M].北京:科学出版社,2003.