熔融制样-X射线荧光光谱法测定铌铁中铌等7个元素质量分数  

Determination of Niobium and Other Seven Elements in Ferroniobium by X-ray Fluorescence Spectrometry with Melting Sample Preparation

作　　者：张幸英 邢文青 黄合生 陈颖 吴红兵 ZHANG Xing-ying;XING Wen-qing;HUANG He-sheng;CHEN Ying;WU Hong-bin(SGIS Songshan Co., Ltd. of Baowu Group Zhongnan Iron & Steel Co., Ltd.,Shaoguan,Guangdong,512123,P.R. China)

机构地区：[1]宝武集团中南钢铁广东韶钢松山股份有限公司,广东韶关512123

出　　处：《南方金属》2022年第2期20-26,共7页Southern Metals

摘　　要：采用传统湿法和电感耦合等离子发射光谱法,测定铌铁中主次元素含量时操作繁琐、不易掌握,熔融制样-X射线荧光光谱法测定铌铁中铌等的含量已有应用。为拓宽X射线荧光光谱(XRF)检测铌铁的应用,采用四硼酸锂熔剂挂壁打底保护铂合金坩埚,以四硼酸锂和碳酸锂做熔剂,用过氧化钡和硝酸钠做氧化剂对样品进行处理,实现了X射线荧光光谱对铌铁中铌、硅、磷、钛、钽、锰、铝的测定。通过高频熔融炉中对样品进行分段预氧化,经预氧化处理将样品中的单质元素转化成氧化物,避免高温状态下单质元素易与铂形成低温共熔体而腐蚀损坏铂金坩埚,解决了熔融法处理铌铁试样时容易腐蚀坩埚的难点。在最佳实验条件下,采用铌铁标准样品和用高纯铁粉及铌铁标样配制的合成标样,建立相关校准曲线,铌、硅、磷、铝、锰、钽钛校准曲线的相关系数均大于0.993。对标准样品进行精密度考察,7种组分测定结果的相对标准偏差(RSD,n=11)在0.119~4.22。对铌铁标准样品进行分析,测定值与认定值相吻合。采用实验方法对铌铁样品中各组分进行测定,所得结果和湿法测得值一致性较好。The determination of major and minor elements in ferroniobium by traditional wet method and inductively coupled plasma-atomic emission spectrometry is complicated and difficult to master,and the determination of niobium in ferroniobium by melting sample preparation-x-ray fluorescence spectrometry has been applied.In order to broaden the application of x-ray fluorescence spectrometry(XRF)in the detection of ferroniobium,the platinum alloy crucible is protected by hanging the wall with the lithium tetraborate flux,the lithium tetraborate and lithium carbonate are used as flux,and the samples are treated with Barium peroxide and sodium nitrate as oxidant,the determination of Nb,Si,P,Ti,Ta,Mn and Al in ferroniobium by X-ray fluorescence spectrometry has been realized.The sample is pre-oxidized in high-frequency melting furnace,and the single element in the sample is converted into oxide after pre-oxidation treatment,which avoids the corrosion of the Platinum crucible caused by the low-temperature co-melting of the single element and platinum at high temperature,the difficulty of melting ferroniobium sample to corrode the crucible is solved.The calibration curves of Nb,Si,P,Ti,Ta,Mn and Al are all greater than 0.993 under the best experimental conditions,using standard samples of ferroniobium and synthetic standard samples of high purity iron powder and ferroniobium.The relative standard deviation(RSD,n=11)of the results of seven components is in the range of 0.119~4.22.The standard sample of ferroniobium is analyzed,and the determined value is consistent with the certified value.The content of each component in ferroniobium sample is determined by the experimental method.The results obtained are in good agreement with those obtained by wet method.

关 键 词：熔融制样 X射线荧光光谱 铌铁 

分 类 号：O657.34[理学—分析化学] TF701.3[理学—化学]