干扰系数校正-电感耦合等离子体原子发射光谱法测定镍基合金中铈  

Determination of cerium in nickel-base alloy by inductively coupled plasma atomic emission spectrometry with interference coefficient correction

作　　者：张亮亮 吴锐红 聂海明 张方 李晓丽 ZHANG Liangliang;WU Ruihong;NIE Haiming;ZHANG Fang;LI Xiaoli(AVIC Metal Test Technology Company Limited,Xi'an 710018,China;Thermo Fisher Scientific(China)Co.,Ltd.,Beijing 100102,China)

机构地区：[1]中航金属材料理化检测科技有限公司,陕西西安710018 [2]赛默飞世尔科技(中国)有限公司,北京100102

出　　处：《冶金分析》2021年第4期73-80,共8页Metallurgical Analysis

摘　　要：在测定镍基合金中Ce时,考虑到Ce的常规分析线在多款仪器中均未找到或分析时不可用,因而很有必要找出相对强度高、干扰程度小的其他可用分析线。实验选用5~10mL盐酸和1mL硝酸溶解镍基合金,采用电感耦合等离子体原子发射光谱法(ICP-AES)和干扰系数法(IEC)相结合的方式,建立了镍基合金中Ce的分析方法。实验预先采用Ce标准溶液系列对从Ce谱线序列中所摘选出的20多条谱线进行一系列相关分析,初步筛选出了6条谱线,并进一步研究了选择这6条谱线时酸的影响与共存元素的干扰行为。经干扰结果分析,可选取Ce 404.076nm、Ce 413.765nm和Ce 456.236nm作为测定镍基合金中Ce的分析线,其中,Ce 404.076nm主要受Co干扰,受V和Mn干扰较小;Ce 413.765nm受W和Nb干扰严重,受Co、Ti和V干扰较小;Ce 456.236nm受Ti干扰严重,Zr、Nb干扰次之,受Co、Mn干扰较小。但由于镍基合金中V、Mn、Zr常为杂质掺入,为了有效简化运算过程,在执行干扰校正时,各谱线主要是校正或消除Co(404.076nm)、W和Nb(413.765nm)、Ti和Co(456.236nm)的干扰。通过对镍基合金GH4099和GH4133B进行分析,经IEC校正后其测定结果与认定值相一致,结果的相对标准偏差(RSD,n=6)小于8.0%。During the determination of Ce in nickel-base alloy,considering that the conventional analysis lines of Ce have not been found in many types of instruments or are not available,it is necessary to find other available analysis lines with high relative intensity and small interference degree.5-10 mL of hydrochloric acid and 1 mL of nitric acid were used to dissolve nickel-base alloy,and the method for determination of Ce in nickel-base alloy by inductively coupled plasma atomic emission spectrometry(ICP-AES)-interference coefficient method(IEC)was established.A series of correlation analysis were carried out on more than twenty spectral lines selected from the Ce spectral line list by using Ce series standard solution.Six spectral lines were selected preliminarily,and the effects of acids and the interfering behavior of co-existing elements were further studied.By analyzing the results of interference experiments,Ce 404.076 nm,Ce 413.765 nm and Ce 456.236 nm were selected as the analytical lines for the determination of Ce in nickel-base alloy,in which Ce 404.076 nm was mainly interfered by Co and less interfered by V and Mn;Ce413.765 nm was seriously interfered by W and Nb,and less interfered by Co,Ti and V;Ce 456.236 nm was seriously interfered by Ti,followed by Zr and Nb,and less interfered by Co and Mn.However,because V,Mn and Zr in nickel-base alloy were often doped as impurities,in order to simplify the calculation process effectively,the spectral lines were mainly used to correct or eliminate the interference of Co(404.076 nm),W and Nb(413.765 nm),Ti and Co(456.236 nm)when performing interference correction.Based on the analysis of nickel-base alloys(GH4099 and GH4133 B),the determination results were consistent with the certified values after the correction of IEC,and the relative standard deviations(RSD,n=6)were less than 8.0%.

关 键 词：电感耦合等离子体原子发射光谱法(ICP-AES) 干扰系数法(IEC) 镍基合金 铈 光谱干扰校正 

分 类 号：O657.31[理学—分析化学] TF125.212[理学—化学]