熔融制样-X射线荧光光谱法测定矾土中主次成分  

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

作　　者：佡云 马晓卉 XIAN Yun;MA Xiaohui(CNMC Shenyang Research Institute of Nonferrous Metals Co.,Ltd.,Shenyang 110141,China)

机构地区：[1]沈阳有色金属研究院有限公司,辽宁沈阳110141

出　　处：《冶金分析》2024年第4期79-86,共8页Metallurgical Analysis

摘　　要：准确测定矾土中的主次成分对确定钒土等级及选择冶炼生产工艺参数具有重要意义。矾土中10余种主次成分含量范围较宽,常需采用两种及以上分析方法分别进行测定。实验用矾土标准样品及成分与矾土相似的3个粘土标准物质绘制校准曲线,以变化理论α系数校正法对基体效应进行校正,以Spectra plus软件进行烧失量校正,建立了熔融制样-X射线荧光光谱法(XRF)对矾土中主次成分(Al_(2)O_(3)、CaO、MgO、P_(2)O_(5)、Fe_(2)O_(3)、TiO_(2)、MnO、SiO_(2)、K_(2)O、Na_(2)O)的测定。实验表明,以四硼酸锂-偏硼酸锂混合熔剂(质量比为67∶33)为熔剂,控制样品稀释比为1∶23,将样品和熔剂搅拌均匀后加入1.0 g硝酸锂于600℃预氧化5 min,升至1075℃熔融制样10 min,期间分3次加入共50 mg碘化铵为脱模剂,可制成均匀、透明的玻璃片。考察了Spectra plus软件和对样品灼烧两种烧失量(LOI)校正方式对矾土中主次成分测定结果的影响,结果表明,两种方式基本一致。选择同一个矾土样品由同一人员在相同环境下于1 d内平行测定11次,测定结果的相对标准偏差(RSD)为0.20%~4.1%;选择不同的试验人员在相同的环境下于15 d内平行测定11次,测定结果的相对标准偏差(RSD)为0.25%~4.7%。采用实验方法对两个矾土样品中主次成分进行测定,结果分别与滴定法或电感耦合等离子体原子发射光谱法(ICP-AES)基本一致。The accurate determination of major and minor components in bauxite is of great significance for the assigning of bauxite grade as well as the selection of smelting and production parameters.The content range of more than ten major and minor components in bauxite is usually wide,and two or more analysis methods are commonly employed for the determination.In this study,the certified reference material of bauxite and three certified reference materials of clay having similar composition with bauxite were used to prepare the calibration curve.The matrix effect was corrected by the variation theoretical α coefficient.Spectra plus software was used for the correction of loss on ignition(LOI).The method for the determination of major and minor components in bauxite(Al_(2)O_(3),CaO,MgO,P_(2)O_(5),Fe_(2)O_(3),TiO_(2),MnO,SiO_(2),K_(2)O and Na_(2)O)by X-ray fluorescence spectrometry(XRF)with fusion sample preparation was established.The results showed that the uniform and transparent beads could be prepared under the following experimental conditions:the mixed flux of lithium tetraborate-lithium metaborate(mass ratio of 67∶33)was used as the flux;the dilution ratio was controlled at 1∶23;1.0 g of lithium nitrate was added into the mixture of sample and flux;the sample was peroxidized at 600℃ for 5 min and then fused at 1075℃ for 10 min;total 50 mg of ammonium iodide was added in three batches as the release agent.The influence of two correction methods of loss on ignition(i.e.,Spectra plus software and sample calcination)on the determination results of major and minor components in bauxite was investigated.The results showed that the results of two methods were basically consistent.One bauxite sample was determined in parallel for 11 times within one day by one analyst under same environment.The relative standard deviations(RSD,n=11)of determination results were between 0.20% and 4.1%.It was also determined in parallel for 11 times within 15 days by different analysts under same environment.The RSDs of determinat

关 键 词：X射线荧光光谱法(XRF) 熔融制样 矾土 Spectra plus软件 烧失量校正 变化理论α系数 

分 类 号：O657.34[理学—分析化学] TF031[理学—化学]