熔融制样-X射线荧光光谱法测定锆质耐火材料中11种主次组分  

Determination of eleven major and minor components in zirconize refractory by X-ray fluorescence spectrometry with fusion sample preparation

作　　者：王志彪 关海兰 WANG Zhibiao;GUAN Hailan(Yangquan Comprehensive Inspection and Testing Center,Yangquan 045000,China;National Silica Alumina Refratory Quality Inspection and Testing Center(Shanxi),Yangquan 045000,China)

机构地区：[1]阳泉市综合检验检测中心,山西阳泉045000 [2]国家硅铝质耐火材料质量检验检测中心(山西),山西阳泉045000

出　　处：《冶金分析》2022年第3期78-83,共6页Metallurgical Analysis

摘　　要：标准方法GB/T 4984—2007对于含锆耐火材料中主次组分的测定需要多种方法相结合,较为繁琐。采用选择日本耐火材料协会X射线荧光光谱分析专用锆质耐火材料系列标样和ZrO_(2)基准试剂混合配制2个校准样品,用该系列标准样品和校准样品制备出12个标准样品/校准样品玻璃片,建立了测定锆质耐火材料中11种主次组分(ZrO_(2)、HfO_(2)、Cr_(2)O_(3)、MgO、CaO、SiO_(2)、Al_(2)O_(3)、Fe_(2)O_(3)、TiO_(2)、K_(2)O、Na_(2)O)的X射线荧光光谱分析方法。实验表明,控制称样量为0.400 0 g,采用Li_(2)B_(4)O_(7)-LiBO_(2)(m∶m=12∶22)混合熔剂和1∶15的稀释比,加入0.2 mL 300 g/L NH_(4)I溶液为脱模剂,于1 050℃下熔融15 min,熔出的样片均匀光滑,达到检验要求。选择ZrLɑ和HfLβ1线为分析谱线,克服了ZrKɑ谱线荧光强度过高的影响;通过谱线校正消除谱线干扰,依据经验α系数法进行基体校正,扣除了样品中各元素的吸收增强效应。校准曲线精密度品质因子小于0.07,各组分检出限为0.007%~0.024%之间。采用实验方法对锆质耐火材料样品进行检测,各组分测量结果的相对标准偏差(RSD)在0.24%~4.9%之间。选择由专用锆质耐火材料系列标准样品和ZrO_(2)基准试剂混合配制的合成样品,分别采用实验方法和标准方法GB/T 4984—2007或GB/T 6900—2016对11种组分进行分析,发现实验方法和标准方法测定值保持一致,实验方法与参考值的误差在标准方法允许差范围内。According to the standard method of GB/T 4984-2007,the determination of major and minor components in zircon-containing refractory requires the combination of several methods.The operation was relatively complex and time-consuming.Two synthetic samples were prepared by certified reference materials of zirconize refractory special for X-ray fluorescence spectrometry(XRF) analysis by Technical Association of Refractories of Japan(TARJ) as well as primary reagent of ZrO_(2).Twelve glass sheets of CRMs/calibration samples were prepared with the series of CRMs and synthetic samples.Thus,an analysis method was established for determination of eleven major and minor components in zirconize refractory(ZrO_(2),HfO_(2),Cr_(2)O_(3),MgO,CaO,SiO_(2),Al_(2)O_(3),Fe_(2)O_(3),TiO_(2),K_(2)O,and Na_(2)O) by XRF.The results showed that the prepared sheets were uniform and smooth to meet the requirements for test under the following experimental conditions:the sample mass was 0.400 0 g;the mix flux of Li_(2)B_(4)O_(7)-LiBO_(2)(m∶m=12∶22) was used;the dilution ratio was 1∶15;0.2 mL of 300 g/L NH_(4)I solution was used as release agent;the sample was melted at 1 050 ℃ for 15 min.ZrLɑ and HfLβ1 lines were selected as the analytical lines to overcome the influence of excessive fluorescence intensity of ZrKɑ line.The spectral interference was eliminated by spectral line correction.The matrix effect was corrected by empirical α coefficient method to eliminate the absorption enhancement effect of each element in the sample.The precision quality factor of calibration curve was less than 0.07.The limits of detection of test components were between 0.007% and 0.024%.The zirconize refractory samples were determined according to the experimental method.The relative standard deviations(RSD) of determination results were between 0.24% and 4.9%.The synthetic samples,which were prepared with series of CRMs special for X-ray fluorescence spectrometry(XRF) analysis and primary reagent of ZrO_(2),were determined by the proposed method and

关 键 词：锆质耐火材料 X射线荧光光谱法(XRF) 熔融制样 基体校正 主次组分 

分 类 号：O657.34[理学—分析化学] TF031[理学—化学]