直流辉光放电质谱法测定氧化铝中的杂质元素
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摘要
为了探索采用直流辉光放电质谱法(dc-GDMS)测定非导体样品中的杂质含量,建立了dc-GDMS法测定α-Al2O3粉末中杂质元素的方法。以Cu粉作为导电介质,与α-Al2O3粉末混合均匀,压片,考察辉光放电条件(放电电流、放电气体流量、离子源温度)和压片条件(两种粉末的混合比例、压片机压力等因素)对放电稳定性和灵敏度的影响,同时优化了实验条件。尝试将Al、O、Cu的总信号归一化进行计算,并用差减法计算了Al2O3粉末中的杂质含量。方法精密度在54%以内,元素检出限为0.005~0.57μg/g。该方法的测定结果与直流电弧发射光谱法的测定结果基本吻合。
In order to investigate elemental analysis in non-conducting samples by direct current glow discharge mass spectrometry(dc-GDMS),a method for detecting impurities inα-Al2O3powder was established.Copper powder acted as a kind of conducting host matrix,which was fully mixed withα-Al2O3 powder,and then pressed the mixture into wafers.Effect of glow discharge conditions,such as discharge current,discharge gas flow,ion source temperature,and pressure conditions,such as mixture ratio,pressure,etc.on discharge stability and sensitivity were investigated.The experiment condition was optimized.Total signal of Al,O and Cu normalization was adopted,and the impurities contents inα-Al2O3powder were calculated in subtraction.The method precision is within 54%and the detection limits are between 0.005μg/g and 0.57μg/g.The results coincide with that of direct current spark atomic emission spectrometry.
In order to investigate elemental analysis in non-conducting samples by direct current glow discharge mass spectrometry(dc-GDMS),a method for detecting impurities inα-Al2O3powder was established.Copper powder acted as a kind of conducting host matrix,which was fully mixed withα-Al2O3 powder,and then pressed the mixture into wafers.Effect of glow discharge conditions,such as discharge current,discharge gas flow,ion source temperature,and pressure conditions,such as mixture ratio,pressure,etc.on discharge stability and sensitivity were investigated.The experiment condition was optimized.Total signal of Al,O and Cu normalization was adopted,and the impurities contents inα-Al2O3powder were calculated in subtraction.The method precision is within 54%and the detection limits are between 0.005μg/g and 0.57μg/g.The results coincide with that of direct current spark atomic emission spectrometry.
引文
[1]任凤莲,游玉萍,石磊,等.微波消解萃取光度法测定高纯氧化铝中Fe2O3的研究[J].冶金分析,2005,25(5):24-27.REN Fenglian,YOU Yuping,SHI Lei,et al.Study on the determination of ferric oxide in highpurity alumina by extractive spectrophotometry combined with microwave digestion[J].Metallurgical Analysis,2005,25(5):24-27(in Chinese).
[2]游玉萍.微波消解-萃取光度法测定高纯氧化铝中SiO2的含量[J].材料研究与应用,2008,1:80-82.YOU Yuping.Determination of SiO2in high-purity alumina by extractive spectrophotometry combined with microwave digestion[J].Metals Research and Application,2008,1:80-82(in Chinese).
[3]姜郁,王通胜,魏志勇,等.微波消解-ICP-AES法测定氧化铝中杂质元素[J].分析实验室,2006,25(8):57-61.JIANG Yu,WANG Tongsheng,WEI Zhiyong,et al.Determination of impurity elements in alumina by inductively coupled plasma atomic emission spectrometry with microwave digestion[J].Chinese Journal of Analysis Laboratory,2006,25(8):57-61(in Chinese).
[4]王倩,明芳.微波消解等离子体光谱法测定高纯氧化铝中杂质元素[J].冶金分析,2003,23(4):53-54.WANG Qian,MING Fang.Determination of impurities in high purity alumina using ICP-AES with microwave digestion[J].Metallurgical Analysis,2003,23(4):53-54(in Chinese).
[5]谷红翠,高华,杨吉芳.分光光度法测定高纯氧化铝中的二氧化硅[J].分析实验室,2000,19(5):87-88.GU Hongcui,GAO Hua,YANG Jifang.Spectrophotometric method for determination of silicon in high pure alumina[J].Chinese Journal of Analysis Laboratory,2000,19(5):87-88(in Chinese).
[6]戴品中,李齐春,潘齐存,等.电感耦合等离子体原子发射光谱法测定高纯氧化铝中15种痕量元素[J].现代化工,2011,31(suppl 1):430-433.DAI Pinzhong,LI Qichun,PAN Qicun,et al.Determination of 15trace elements in high-purity alumina by ICP-AES[J].Modern Chemical Industry,2011,31(suppl 1):430-433(in Chinese).
[7]王云霞,苏献瑞.火焰原子吸收光谱法测定高纯氧化铝和氢氧化铝中痕量镍[J].理化检验-化学分册,2000,36(1):13-14.WANG Yunxia,SU Xianrui.FAAS determination of traces of nickel in high purity aluminium and aluminum hydroxide[J].PTCA(PART B:Chemical Analysis),2000,36(1):13-14(in Chinese).
[8]卢桂萍,汪正,邱德仁,等.悬浮液进样自吸扣背景石墨炉原子吸收光谱法测定高纯氧化铝中铜、铁和钠含量[J].光谱学与光谱分析,2011,31(1):244-248.LU Guiping,WANG Zheng,QIU Deren,et al.Direct determination of copper,iron and sodium in high-purity alumina by slurry introduction furnace atomic absorption spectrometry with smith-hieftje background correction[J].Spectroscopy and Spectral Analysis,2011,31(1):244-248(in Chinese).
[9]辛仁轩.原子发射光谱仪[J].分析测试仪器通讯,1995,5(3):149-167.XIN Renxuan.Atomic emission spectrometer[J].Analysis of Test Instrument Communication,1995,5(3):149-167(in Chinese).
[10]SCHELLES W,GRIEKEN R V.Direct current glow discharge mass spectrometric analysis of macor ceramic using a secondary cathode[J].Anal Chem,1996,68(20):3 570-3 574.
[11]MILTON D M P,HUTTON R C.Investigations into the suitability of using a secondary cathode to analyse glass using glow discharge mass spectrometry[J].Spectrochimica Acta,1993,48B(1):39-52.
[12]INOUE M,SAKA T.Elemental analysis of powders by glow discharge mass spectrometry[J].Analytica Chimica Acta,1999,395(1/2):165-171.
[13]TONG S L,HARRISON W W.Glow discharge mass spectrometric analysis of non-conducting materials[J].Spectrochimica Acta,1993,48B(10):1 237-1 245.
[14]BATTAGLIARIN M,SENTIMENTI E,SCATTOLIN R.An innovative sample preparation procedure for trace and ultra-trace analysis on non-conducting powders by direct current glow discharge mass spectrometry[J].Spectrochimica Acta,1995,50B(1):13-25.
[15]KUROCHKIN V D,KRAVCHENKO L P.Analysis of impurities in high-purity aluminum oxide by glow discharge mass spectrometry[J].Powder Metallurgy and Metal Ceramics,2006,45(9/10):493-499.
[16]SCHELLES W,GENDT S D,MULLER V,et al.Evaluation of secondary cathodes for glow discharge mass spectrometry analysis of different nonconducting sample types[J].Appl Spectrosc,1995,49(7):939-944.
[17]SCHELLES W,GRIEKEN R V.Direct current glow discharge mass spectrometry for elemental characterization of polymers[J].Anal Chem,1997,69(15):2 931-2 934.
[18]WOO J C,JAKUBOWSKI N,STUEWER D.Analysis of aluminum oxide powder by glow discharge mass spectrometry with low mass resolution[J].Anal Atom Spec,1993,8(6):881-889.
[2]游玉萍.微波消解-萃取光度法测定高纯氧化铝中SiO2的含量[J].材料研究与应用,2008,1:80-82.YOU Yuping.Determination of SiO2in high-purity alumina by extractive spectrophotometry combined with microwave digestion[J].Metals Research and Application,2008,1:80-82(in Chinese).
[3]姜郁,王通胜,魏志勇,等.微波消解-ICP-AES法测定氧化铝中杂质元素[J].分析实验室,2006,25(8):57-61.JIANG Yu,WANG Tongsheng,WEI Zhiyong,et al.Determination of impurity elements in alumina by inductively coupled plasma atomic emission spectrometry with microwave digestion[J].Chinese Journal of Analysis Laboratory,2006,25(8):57-61(in Chinese).
[4]王倩,明芳.微波消解等离子体光谱法测定高纯氧化铝中杂质元素[J].冶金分析,2003,23(4):53-54.WANG Qian,MING Fang.Determination of impurities in high purity alumina using ICP-AES with microwave digestion[J].Metallurgical Analysis,2003,23(4):53-54(in Chinese).
[5]谷红翠,高华,杨吉芳.分光光度法测定高纯氧化铝中的二氧化硅[J].分析实验室,2000,19(5):87-88.GU Hongcui,GAO Hua,YANG Jifang.Spectrophotometric method for determination of silicon in high pure alumina[J].Chinese Journal of Analysis Laboratory,2000,19(5):87-88(in Chinese).
[6]戴品中,李齐春,潘齐存,等.电感耦合等离子体原子发射光谱法测定高纯氧化铝中15种痕量元素[J].现代化工,2011,31(suppl 1):430-433.DAI Pinzhong,LI Qichun,PAN Qicun,et al.Determination of 15trace elements in high-purity alumina by ICP-AES[J].Modern Chemical Industry,2011,31(suppl 1):430-433(in Chinese).
[7]王云霞,苏献瑞.火焰原子吸收光谱法测定高纯氧化铝和氢氧化铝中痕量镍[J].理化检验-化学分册,2000,36(1):13-14.WANG Yunxia,SU Xianrui.FAAS determination of traces of nickel in high purity aluminium and aluminum hydroxide[J].PTCA(PART B:Chemical Analysis),2000,36(1):13-14(in Chinese).
[8]卢桂萍,汪正,邱德仁,等.悬浮液进样自吸扣背景石墨炉原子吸收光谱法测定高纯氧化铝中铜、铁和钠含量[J].光谱学与光谱分析,2011,31(1):244-248.LU Guiping,WANG Zheng,QIU Deren,et al.Direct determination of copper,iron and sodium in high-purity alumina by slurry introduction furnace atomic absorption spectrometry with smith-hieftje background correction[J].Spectroscopy and Spectral Analysis,2011,31(1):244-248(in Chinese).
[9]辛仁轩.原子发射光谱仪[J].分析测试仪器通讯,1995,5(3):149-167.XIN Renxuan.Atomic emission spectrometer[J].Analysis of Test Instrument Communication,1995,5(3):149-167(in Chinese).
[10]SCHELLES W,GRIEKEN R V.Direct current glow discharge mass spectrometric analysis of macor ceramic using a secondary cathode[J].Anal Chem,1996,68(20):3 570-3 574.
[11]MILTON D M P,HUTTON R C.Investigations into the suitability of using a secondary cathode to analyse glass using glow discharge mass spectrometry[J].Spectrochimica Acta,1993,48B(1):39-52.
[12]INOUE M,SAKA T.Elemental analysis of powders by glow discharge mass spectrometry[J].Analytica Chimica Acta,1999,395(1/2):165-171.
[13]TONG S L,HARRISON W W.Glow discharge mass spectrometric analysis of non-conducting materials[J].Spectrochimica Acta,1993,48B(10):1 237-1 245.
[14]BATTAGLIARIN M,SENTIMENTI E,SCATTOLIN R.An innovative sample preparation procedure for trace and ultra-trace analysis on non-conducting powders by direct current glow discharge mass spectrometry[J].Spectrochimica Acta,1995,50B(1):13-25.
[15]KUROCHKIN V D,KRAVCHENKO L P.Analysis of impurities in high-purity aluminum oxide by glow discharge mass spectrometry[J].Powder Metallurgy and Metal Ceramics,2006,45(9/10):493-499.
[16]SCHELLES W,GENDT S D,MULLER V,et al.Evaluation of secondary cathodes for glow discharge mass spectrometry analysis of different nonconducting sample types[J].Appl Spectrosc,1995,49(7):939-944.
[17]SCHELLES W,GRIEKEN R V.Direct current glow discharge mass spectrometry for elemental characterization of polymers[J].Anal Chem,1997,69(15):2 931-2 934.
[18]WOO J C,JAKUBOWSKI N,STUEWER D.Analysis of aluminum oxide powder by glow discharge mass spectrometry with low mass resolution[J].Anal Atom Spec,1993,8(6):881-889.