Discussion on interference and correction method during the analysis of trace silicon in complex superalloy by inductively coupled plasma atomic emission spectrometry
LIU Xiao-bo, YANG Guo-wu, HOU Yan-xia, QI Rong, LIU Qing-bin*, HU Jing-yu
Beijing NCS Analytical Instruments Co., Ltd., Beijing 100081, China
Abstract：The physical and chemical properties of superalloy materials are affected by the content of silicon. The accurate determination of silicon in superalloy is an important guarantee for quality control. Obvious matrix effect and complex spectral interference exist during the determination of trace silicon in superalloy by inductively coupled plasma atomic emission spectrometry (ICP-AES). The sample was dissolved with hydrochloric acid-nitric acid mixture and hydrofluoric acid. The matrix effect was eliminated through preparing standard solution series by matrix matching method. Si 184.685nm, Si 185.005nm and Si 251.611nm were selected as the analytical lines. According to the characteristic that silicon could form volatile substances with hydrofluoric acid and silicon was easily interfered by alloying elements such as tantalum, molybdenum, rhenium and tungsten, the determination results were corrected by interference equivalent concentration (IEC) method and matrix blank subtraction method. The analysis and interference correction methods of trace silicon in complex superalloy by ICP-AES were established. The calibration curve was linear when the mass fraction of silicon was in range of 0.005%-0.40%, and the linear correlation coefficient (r) was 0.9999. The detection limit was less than 0.001%. The proposed method was applied for the determination of silicon in superalloy samples. The relative standard deviation (RSD, n=7) of results was less than 2%. The found results using two types of correction methods were compared with those obtained by glow discharge mass spectrometry (GD-MS), and the consistency was good.
刘晓波, 杨国武, 侯艳霞, 齐荣, 刘庆斌, 胡净宇. 电感耦合等离子体原子发射光谱法分析复杂高温合金中痕量硅的干扰及校正方法探讨[J]. 冶金分析, 2018, 38(7): 12-19.
LIU Xiao-bo, YANG Guo-wu, HOU Yan-xia, QI Rong, LIU Qing-bin, HU Jing-yu. Discussion on interference and correction method during the analysis of trace silicon in complex superalloy by inductively coupled plasma atomic emission spectrometry. , 2018, 38(7): 12-19.
王会阳,安云岐,李承宇,等.镍基高温合金材料的研究进展[J].材料导报,2011(18):482-486.WANG Hui-yang,AN Yun-qi,LI Cheng-yu,et al.Research progress of Ni-based superalloy[J].Material Review,2011(18):482-486.
[2]
郭建亭.几种微量元素在高温合金中的作用与机理[J].中国有色金属学报,2011,21(3):465-475.GUO Jian-ting.Effects of several minor elements on superalloys and their mechanism[J].The Chinese Journal of Nonferrous Metals,2011,21(3):465-475.
姚金玉,谢文兵,胡庆兰,等.石墨炉原子吸收法直接测定高温合金中硅[J].分析化学,1995,23(3):284-287.YAO Jin-yu,XIE Wen-bing,HU Qing-lan,et al. Direct determination of silicon in high temperature alloy by graphite furnace atomic absorption spectrometry[J].Chinese Journal of Analytical Chemistry,1995,23(3):284-287.
[6]
李佗.电感耦合等离子体-原子发射光谱法测定镍基高温合金中的硅、锰、铁、铬、钼、钴和钨[J].光谱实验室,2013,30(2):840-842.LI Tuo.Determination of Si,Mn,Fe,Cr,Mo,Co and W in nickel-base high-temperature alloy by ICP-AES[J]. Chinese Journal of Spectroscopy Laboratory,2013,30(2):840-842.
[7]
赵荣超,唐本玲.电感耦合等离子体光谱法测定镍基高温合金中的硅锰磷[J].化学分析计量,2011,20(4):54-56.ZHAO Rong-chao,TANG Ben-ling.Determination of silicon,manganese and phosphorus in nickel-base superalloy by ICP-AES[J].Chemical Analysis and Meterage,2011,20(4):54-56.
[8]
杜米芳.微波消解-电感耦合等离子体原子发射光谱法测定镍基合金中硅[J].冶金分析,2017,37(4):71-75.DU Mi-fang.Determination of silicon in nickel base alloy by inductively coupled plasma atomic emission spectrometry after microwave digesion[J].Metallurgical Analysis,2017,37(4):71-75.
李帆,范键.ICP-AES分析中干扰及其校正方法的进展(1)[J].光谱学与光谱分析,1998,18(3):325-328.LI Fan,FAN Jian.Recent development of studies on the interferences and their correction methods in ICP-AES (1)[J].Spectroscopy and Spectral Analysis,1998,18(3):325-328.
[11]
曹宏燕.冶金材料分析技术与应用[M].北京:冶金工业出版社,2008:14-21.
[12]
周勇义,谷学新,范国强,等.微波消解技术及其在分析化学中的应用[J].冶金分析,2004,24(2):30-36.ZHOU Yong-yi,GU Xue-xin,FAN Guo-qiang,et al.Application of microwave digestion in analytical chemistry[J].Metallurgical Analysis,2004,24(2):30-36.
