熔融制样-X射线荧光光谱法测定钢包水口絮流物中5种组分  

Determination of 5 components in ladle nozzle flocculation by X-ray fluorescence spectrometry with fusion sample preparation

作　　者：亢德华 杨洁 胡忠新 邓军华 王一凌 KANG Dehua;YANG Jie;HU Zhongxin;DENG Junhua;WANG Yiling(State Key Laboratory of Metal Material for Marine Equipment and Application,Anshan 114009,China;Iron&Steel Research Institute of Ansteel Group,Anshan 114009,China)

机构地区：[1]海洋装备用金属材料及其应用国家重点实验室,辽宁鞍山114009 [2]鞍钢集团钢铁研究院,辽宁鞍山114009

出　　处：《冶金分析》2024年第6期64-68,共5页Metallurgical Analysis

摘　　要：炼钢厂在浇注某些钢种时经常发生钢包水口絮流现象,经X射线荧光光谱(XRF)半定量分析,水口絮流物是一种以Al_(2)O_(3)、CaO、SiO_(2)、MgO和Fe为主要成分的物质,其化学成分的分析一般采用滴定法、分光光度法或原子吸收光谱法(AAS)等,这些方法操作相对繁琐、流程长。采用Li_(2)B_(4)O_(7)-LiBO_(2)混合熔剂(m∶m=67∶33)按稀释比为1∶12.5的比例进行熔融制样,加入0.15 g NH_(4)I脱模剂,消除了样品的矿物效应,降低了基体效应的影响;选择与水口絮流物基体相似的矾土、莫来石、焦宝石、高炉渣等标准样品及用这些标准样品按不同比例混合配制的校准样品绘制校准曲线,解决了水口絮流物没有标准物质的难题;以经验系数法校正基体对分析线光谱强度的吸收-增强影响,校准曲线的相关系数均大于0.9989,建立了熔融制样-X射线荧光光谱法同时测定钢包水口絮流物中Al_(2)O_(3)、CaO、SiO_(2)、MgO和总铁(TFe)含量的分析方法。各组分方法检出限为0.009%~0.014%。选取同一水口絮流物试样,按实验方法测定,各组分测定结果的相对标准偏差(RSD,n=10)均小于3.0%。分别采用实验方法与标准方法GB/T 5069—2015测定2个水口絮流物试样,两种方法的差值均小于标准方法GB/T 5069—2015的允许差。The phenomenon of flocculation at ladle nozzle often occurs during the pouring of certain steel grades in steel-making plants.The semiquantitative analysis by X-ray fluorescence spectrometry(XRF)indicated that the nozzle flocculation was mainly composed of Al_(2)O_(3),CaO,SiO_(2),MgO and Fe.The chemical composition analysis usually adopts titration,spectrophotometry or atomic absorption spectrometry(AAS),and so on.However,these methods have some disadvantages such as complex operation and long procedures.The sample was prepared by fusion method with Li_(2)B_(4)O_(7)-LiBO_(2) mixed flux(m:m=67:33)and dilution ratio of 1:12.5,and 0.15 g of NH_(4)I was added as release reagent.The mineral effect of sample was eliminated,and the influence of matrix effect was reduced.The certified reference materials such as bauxite,mullite,pyroxene,and blast furnace slag,which have the similar matrix with ladle nozzle flocculation were selected.Then the calibration curves were drawn with these certified reference materials and the calibration samples by mixing these certified reference materials in different proportions,solving the problem that there was no certified reference material of ladle nozzle flocculation.The absorption enhancement effect of spectral intensity caused by the matrix was corrected with empirical coefficient method.The correlation coefficients of calibration curves were all greater than 0.9989.The analysis method for simultaneous determination of Al_(2)O_(3),CaO,SiO_(2),MgO,and total iron(TFe)in ladle nozzle flocculation was established by XRF with fusion sample preparation.The limits of detection were between 0.009% and 0.014%.One ladle nozzle flocculent sample was determined according to the proposed method.The relative standard deviations(RSD,n=10)of determination results were all less than 3.0%.Two ladle nozzle flocculent samples were determined respectively by the proposed method and GB/T 5069-2015,and the differences of the two above methods were all less than the tolerance of GB/T 5069-2015.

关 键 词：熔融制样 X射线荧光光谱法(XRF) 钢包水口絮流物 二氧化硅 氧化铝 氧化钙 氧化镁 全铁 

分 类 号：O657.34[理学—分析化学] TF031[理学—化学]