碱熔-电感耦合等离子体原子发射光谱法测定石灰石中8种组分  

Determination of 8 components in limestone by inductively coupled plasma atomic emission spectrometry with alkali fusion

作　　者：滕广清 王彬果 TENG Guangqing;WANG Binguo(HBIS Group HanSteel Company Technology Center,Handan 056003,China)

机构地区：[1]河钢集团邯钢公司技术中心,河北邯郸056003

出　　处：《冶金分析》2024年第7期88-94,共7页Metallurgical Analysis

摘　　要：石灰石中常规组分含量的准确测定对指导冶金生产具有重要意义。为解决酸溶法过程繁琐且硅含量测定难度大,碱熔法熔融物黏附坩埚且钠、钾含量测定受制于熔融试剂等问题,借鉴X射线荧光光谱法(XRF)的硼酸盐熔融制样的方法,即在铂-金坩埚内将0.2 g样品与1.0 g四硼酸锂-偏硼酸锂混合熔剂(m∶m=67∶33)、8~10滴300 g/L碘化铵溶液混合,经1000℃高温熔融10 min,形成可完全剥离的玻璃熔珠,使用10%硝酸(V/V)加热溶解玻璃熔珠,采用电感耦合等离子体原子发射光谱法(ICP-AES)测定Al、Fe、Mg、Mn、Si、Ti、K、Na共8种元素。根据谱线的强度大小及干扰情况,选择背景简单、干扰元素少的分析谱线;用基体匹配法消除了熔剂和主成分基体的基体效应的影响;在选定的工作条件下,各元素校准曲线的线性相关系数均大于0.999;方法检出限为0.001~0.03μg/g。按照实验方法对两个石灰石样品进行精密度考察,Al、Fe、Mg、Mn、Si、Ti、K、Na(均以氧化物计)测定结果的相对标准偏差(RSD,n=6)为0.53%~4.8%。对2个石灰石标准物质/标准样品(GBW03106a、YSBC28707a-2013)进行测定,标准物质/标准样品的测定值与认定值/标准值一致,符合GB/T 27417—2017《合格评定化学分析方法确认和验证指南》的要求。The accurate determination of conventional components in limestone has important significance for guiding metallurgical production.To address the challenges posed by the complicated acid dissolution process and the challenges in determining the silicon content,as well as issues with the crucible adhesion of molten material and limitations in the determination of sodium and potassium content due to the use of molten reagents in the alkali fusion method,the borate fusion sample preparation method of X-ray fluorescence spectrometry(XRF)was referenced.0.2 g of sample,1.0 g of Li_2B_4O_7-LiBO_2(m∶m=67∶33)mixture flux,and 8-10 drops of 300 g/L ammonium iodide solution were mixed in a platinum-gold crucible.After fusion at high temperature(1000℃)for 10 min,the fully detachable glass beads could be formed.The glass beads were then dissolved with 10%nitric acid(V/V)by heating.The contents of eight elements,including Al,Fe,Mg,Mn,Si,Ti,K and Na,were determined by inductively coupled plasma atomic emission spectrometry(ICP-AES).Based on the intensity and interference of spectral lines,the analytical lines with simple background and few interfering elements were selected.The matrix matching method was used to eliminate the influence of matrix effects caused by the flux and the main component matrix.Under the selected working conditions,the linear correlation coefficients of the calibration curves for each element were all greater than 0.999,and the limits of detection were in range of 0.001-0.03μg/g.The precision tests were conducted using two limestone samples according to the experimental method.The relative standard deviations(RSD,n=6)of determination results of Al,Fe,Mg,Mn,Si,Ti,K and Na(in oxides)were between 0.53%and 4.8%.Two certified reference materials(GBW03106a,YSBC28707a-2013)were determined,and the found results were consistent with the certified value/standard value,which could meet the requirements of GB/T 27417-2017 Guidelines for Confirmation and Validation of Chemical Analysis Methods for Conformity As

关 键 词：硼酸盐 熔融 电感耦合等离子体原子发射光谱法(ICP-AES) 石灰石 常规组分 

分 类 号：O657.31[理学—分析化学] TF031[理学—化学]