Determination of niobium in constant current electrolysis precipitates of niobium microalloyed steel by inductively coupled plasma atomic emission spectrometry after microwave digestion
SONG Peng-xin, YANG Zhi-qiang, JU Xin-hua, LIU Wei-ping
Research Institute of Technology of ShouGang Group Co.,Ltd.,Beijing 100043,China
Abstract：Based on the difference of precipitation amount and solid solution quantity of niobium in various processes, the quality and property of steel can be improved by adding niobium. Therefore, the analysis of niobium precipitates in steel had important significance to study the strengthening mechanism of niobium in steel and improve the process. The precipitates from niobium microalloyed steel was extracted in 50g/L potassium chloride and 10g/L citric acid solution by constant-current electrolysis at 0.05A/cm2 in range of 5-10℃. The polycarbonate filtration membrane and extracts were treated by microwave digestion using aqua regia and sulfuric acid as solvent. Tartaric acid was added as complexing agent to inhibit the hydrolysis of niobium. The content of niobium compounds in steel was determined by inductively coupled plasma atomic emission spectrometry (ICP-AES). The results showed that the polycarbonate filtration membrane and extracts could be completely dissolved by microwave digestion. The addition of 5mL of tartaric acid (200g/L) was enough to fully complex niobium. Nb 316.340nm with little interference was selected as the analytical line. The treatment method of calibration curve was same with that of sample to eliminate the negative factors such as physical interference. The correlation coefficient of calibration curve was higher than 0.9997, and the detection limit of method was 0.0062mg/L. The content of niobium compounds in three steel samples was determined, and the relative standard deviations (RSD) were less than 0.12%. The determination results were consistent with those obtained by national standard method GB/T 223.40—2007. The proposed method was applicable for the extraction and determination of niobium compounds in niobium microalloyed steel, and the results were reliable.
宋鹏心, 杨志强, 鞠新华, 刘卫平. 微波消解-电感耦合等离子体原子发射光谱法测定铌微合金化钢恒电流电解析出物中铌[J]. 冶金分析, 2017, 37(11): 40-45.
SONG Peng-xin, YANG Zhi-qiang, JU Xin-hua, LIU Wei-ping. Determination of niobium in constant current electrolysis precipitates of niobium microalloyed steel by inductively coupled plasma atomic emission spectrometry after microwave digestion. , 2017, 37(11): 40-45.
余卫华,姜凤琴.含铌低合金钢相分析[J].钢铁研究,1997(3):37-39.YU Wei-hua,JIANG Feng-qin.Phase analysis on Nb-containing low-alloyed steel[J].Research on Iron & Steel,1997(3):37-39.
贾荣征,焦玲环,李建华,等.几种分光光度法测定铌的方法比较[J].分析化学,1979,7(4):247-251.JIA Rong-zheng,JIAO Ling-huan,LI Jian-hua,et al.Comparison of several methods for spectrophotometry determination of niobium[J].Chinese Journal of Analytical Chemistry,1979,7(4):247-251.
[4]
杨丽荣,于媛君,亢德华,等.电感耦合等离子体原子发射光谱法测定钢中铌钨锆[J].冶金分析,2014,34(11):51-55.YANG Li-rong,YU Yuan-jun,KANG De-hua,et al.Determination of niobium,tungsten and zirconium in steel by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2014,34(11):51-55.
[5]
凌礼照,杨文玮.ICP-AES法测定特殊钢中铌和钽[J].冶金分析,1999,19(5):48-50.LING Li-zhao,YANG Wen-wei.Determination of niobium and tantalum in special steel by ICP-AES[J].Metallurgical Analysis,1999,19(5):48-50.
[6]
崔宏利,张宏霞.电感耦合等离子体原子发射光谱法测定中低合金钢中微量铌[J].分析试验室,2009,28(增刊):235-237.CUI Hong-li,ZHANG Hong-xia.Determination of niobium in medium and low alloy steel by inductively coupled plasma atomic emission spectrometry[J].Chinese Journal of Analysis Laboratory,2009,28(supplement):235-237.
[7]
张家相.ICP法测定钢中微量Nb的技术分析[J].四川有色金属,2006(3):42-44.ZHANG Jia-xiang.Technical analysis of ICP determination minim Nb in steel[J].Sichuan Nonferrous Metals,2006,(3):42-44.
[8]
米戎.ICP-AES法测定钢中铌[J].光谱实验室,1993,10(3):12-15.MI Rong.Determination of niobium in steel by ICP-AES[J].Chinese Journal of Spectroscopy Laboratory,1993,l0(3):12-15.
[9]
叶晓英,冯艳秋.ICP-AES法测定超高强度钢中Mn,Si,Al,Ti,Nb,La杂质元素[J].材料工程,2007(2):46-48.YE Xiao-ying,FENG Yan-qiu.ICP-AES determination of Mn,Si,Al,Ti,Nb,La in ultrahigh strength steel[J].Journal of Materials Engineering,2007(2):46-48.
[10]
韦莉,周素莲,何小虎.微波消解-电感耦合等离子体原子发射光谱法测定中低合金钢中铌钨锆钴钒锡[J].冶金分析,2012,32(8):75-78.WEI Li,ZHOU Su-lian,HE Xiao-hu.Microwave digestion and inductively coupled plasma atomic emission spectrometric method for the determination of niobium,tungsten,zirconium,cobalt,vanadium and tin in low-medium alloy steel[J]. Metallurgical Analysis,2012,32(8):75-78.
[11]
张杰,郝静,王慧清,等.微波消解-ICP-AES 法测定装甲材料中的铌含量[J].化学分析计量,2014,23(5):58-59.ZHANG Jie,HAO Jing,WANG Hui-qing,et al.Determination of niobium content in a new type armor materials by microwave digestion-ICP-AES[J].Chemical Analysis and Meterage,2014,23(5):58-59.
[12]
郭晓爽,杨婧,付强,等.微波消解体系与聚四氟乙烯滤膜对 PM2.5中重金属测定的影响[J].中国环境监测,2014,30(4):129-133.GUO Xiao-shuang,YANG Jing,FU Qiang,et al.Effect microwave digestion system and PTFE filter on quantitative research of heavy metals in PM2.5[J].Environmental Monitoring in China,2014,30(4):129-133.
[13]
张六一,付 川,杨复沫,等.微波消解ICP-OES法测定PM2.5中金属元素[J].光谱学与光谱分析,2014,34(11):3109-3112.ZHANG Liu-yi,FU Chuan,YANG Fu-mo,et al.Determination of metal elements in PM2.5 by ICP-OES with microwave digestion[J].Spectroscopy and Spectral Analysis,2014,34(11):3109-3112.
[14]
朱奕,葛飞,许雄飞.微波消解ICP-OES 法同时测定总悬浮颗粒物中多种重金属[J].环境科学导刊,2013,32(2):112-115.ZHU Yi,GE Fei,XU Xiong-fei.Determination of heavy metals in total suspended particulate by microwave-assisted digestion coupled with plasma spectroscopy (ICP-OES)[J].Environmental Science Survey,2013,32(2):112-115.
