摘要
使用Li2B4O7和LiBO2混合熔剂(质量比为67∶33),NH4NO3作氧化剂,饱和LiBr溶液作脱模剂,在电加热熔样机上制备玻璃熔片,建立了波长色散X射线荧光光谱法(WD-XRF)测定钛铁矿物中TiO2、TFe、SiO2、A12O3、V2O5、MgO、CaO、S、P、Na2O的分析方法。实验表明,在熔样比例(质量比)为15∶1、熔样温度为1 100℃、熔样时间为15min时熔样效果最佳。在最佳实验条件下,在自制钛铁矿标准样品的含量范围内,各组分的含量与其荧光强度呈线性关系,相关系数在0.995 6～0.999 7之间。采用基本参数法对基体效应进行校正后,平行测定样品10次,所得结果的相对标准偏差除P为9.8%外,其它各组分均不大于1.3%。采用实验方法对钛铁矿样品中各组分进行测定,所得结果和湿法测得值一致。
The glass fusion piece of sample was prepared on electrical heating fusion machine with Li2B4O7-LiBO2（mass ratio of 67∶33）as mixed flux,NH4NO3as oxidant and saturated LiBr solution as releasing agent.Consequently,a method for determination of TiO2,TFe,SiO2,A12O3,V2O5,MgO,CaO,S,P and Na2O in ilmenite was established by wavelength dispersion X-ray fluorescence spectrometry.The results showed that the optimal sample fusion conditions were as follows：sampleflux ratio（mass ratio）of 15∶1,sample fusion temperature of 1 100 ℃ and fusion time of 15min.Under the optical experiments conditions,component content was linear to the fluorescence intensity within the content range of self-made lmenite reference samples,and correlation coefficients were between 0.995 6and 0.999 7.After matrix effect was corrected by fundamental parameter method,the relative standard deviations（RSD,n=10）were not more than 1.3%except for P（9.8%）.The proposed method was applied to the determination of components in ilmenite actual samples,and the results were consistent with those obtained by wet method.
出处
《冶金分析》
CAS
CSCD
北大核心
2013年第6期32-36,共5页
Metallurgical Analysis
关键词
X射线荧光光谱法
钛铁矿
熔融制样
基体效应
X-ray fluorescence spectrometry
ilmenite
fusion sample preparation
matrix effect
