悬浮液进样-液体阴极辉光放电原子发射光谱法测定高纯氮化硅粉体中微量杂质元素
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摘要
针对高纯氮化硅粉体中的9种微量杂质元素(Al、Ca、Co、Fe、K、Mg、Mn、Na、Ni),建立了悬浮液进样-液体阴极辉光放电原子发射光谱定量分析方法。考察了制备稳定悬浮液对样品颗粒度的要求,并通过六通阀将悬浮液引入液体阴极辉光放电原子发射光谱装置检测。本方法采用水溶液标准进行定量分析,无需对悬浮液的p H值进行精确调节,能够保持液体阴极辉光等离子体的稳定性。研究了仪器装置的操作电压、载液流速、光电倍增管积分时间等因素对检出限的影响。优化后得到的最佳实验条件为操作电压1080 V,载液流速1.2 m L/min,光电倍增管积分时间800 ms。利用六通阀进样系统对原有的液体阴极辉光放电原子发射光谱装置进行改进,从而实现悬浮液直接进样检测。用此装置对氮化硅实际样品进行检测,得到各种元素的检出限在0.2~53 mg/kg之间,RSD在1.1%~5.0%之间。通过对氮化硅标准参考物质ERM-ED101进行分析,其测定结果与高温高压消解-电感耦合等离子体发射光谱法一致,并与标准参考值吻合,表明此方法可用于氮化硅粉体的悬浮液直接进样检测,结果准确可靠,灵敏度高,具备应用价值。
Trace impurities of Al,Ca,Co,Fe,K,Mg,Mn,Na,Ni in silicon nitride powder were determined by slurry introduction into a solution-cathode glow discharge-atomic emission spectrometer( SCGDAES). The effect of particle size on the stability of suspension was investigated. A 6-port valve was selected to link sampling system and SCGD-AES,by which the suspension could be introduced into the SCGD-AES to get instantaneous spectrum signal. The calibration curves for quantitative analysis could be established using aqueous standards and the p H of suspension was not required to be adjusted accurately. The applied voltage,solution flow rate,and integral time of PMT were set to 1080 V,1. 2 mL/min and 800 ms,respectively. In this work,slurry sampling was combined with SCGD-AES by a 6 port 2-pos valve. Powder Si3N4 was tested by this way and the limits of detection for all nine elements were 0.2-53.0 mg/kg. The RSDs were 1.1%-5.0%.The detection result of trace impurities in standard reference material ERM-ED101 agreed with that obtained from inductively coupled plasma atomic emission spectrometry. This method was proved to be accurate,reliable and valuable.
Trace impurities of Al,Ca,Co,Fe,K,Mg,Mn,Na,Ni in silicon nitride powder were determined by slurry introduction into a solution-cathode glow discharge-atomic emission spectrometer( SCGDAES). The effect of particle size on the stability of suspension was investigated. A 6-port valve was selected to link sampling system and SCGD-AES,by which the suspension could be introduced into the SCGD-AES to get instantaneous spectrum signal. The calibration curves for quantitative analysis could be established using aqueous standards and the p H of suspension was not required to be adjusted accurately. The applied voltage,solution flow rate,and integral time of PMT were set to 1080 V,1. 2 mL/min and 800 ms,respectively. In this work,slurry sampling was combined with SCGD-AES by a 6 port 2-pos valve. Powder Si3N4 was tested by this way and the limits of detection for all nine elements were 0.2-53.0 mg/kg. The RSDs were 1.1%-5.0%.The detection result of trace impurities in standard reference material ERM-ED101 agreed with that obtained from inductively coupled plasma atomic emission spectrometry. This method was proved to be accurate,reliable and valuable.
引文
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25 WANG Zheng,WANG Shi-Wei,QIU De-Ren,YANG Peng-Yuan.Spectroscopy and Spectral Analysis,2009,29(10):2838-2842汪正,王士维,邱德仁,扬芃原.光谱学与光谱分析,2009,29(10):2838-2842
2 Evans J R G,Moulson A.J.Mater.Sci.,1983,18:3721-3728
3 Engel W.Powder Metall.Int.,1978,10:124-127
4 Friese K C,Krivan V.Anal.Chem.,1995,67(2):354-359
5 Graule T,von Blhlen A,Broekaert J A C,Grallath E,Klockenkamper R,Tschopel P,Tolg G,Fresenius Z.Anal.Chem.,1989,335:637-642
6 Kim K H,Kin H Y,Lim H B.Bull.Korean Chem.Soc.,2001,22(2):159-163
7 Wang Z,Zhang J Y,Zhang G X,Qiu D R,Yang P Y.J.Anal.At.Spectrom.,2015,30:909-915
8 Cserfalvi T,Mezei P.Fresenius J.Anal.Chem.,1996,12(10):1203-1208
9 ZHANG Zhen,WANG Zheng,ZOU Hui-Jun,SHI Ying.Chinese J.Anal.Chem.,2013,41(10):1606-1613张真,汪正,邹慧君,施鹰.分析化学,2013,41(10):1606-1613
10 Zhu Z L,Liu J X,Zhang S C,Na X,Zhang X R.Anal.Chim.Acta,2008,607(2):136-141
11 Xing Z,Wang J,Zhang S C,Zhang X R.Talanta,2009,80(1):139-142
12 Wang Z,Schwartz A J,Ray S J,Hieftje G M.J.Anal.At.Spectrom.,2013,28:234-240
13 XI Xiao-Qin,ZHENG Pei-Chao,WANG Hong-Mei,LI Jian-Quan,HAN Hai-Yan,CHU Yan-Nan.Chinese J.Anal.Chem.,2010,38(3):449-452席晓琴,郑培超,王鸿梅,李建权,韩海燕,储焰南.分析化学,2010,38(3):449-452
14 ZHENG Pei-Chao,ZHANG Bin,WANG Jin-Mei,WANG Xiao-Meng,LIU Hong-Di,YANG Rui.Spectroscopy and Spectral Analysis,2015,35(7):2012-2016郑培超,张斌,王金梅,王晓蒙,刘红弟,杨蕊.光谱学与光谱分析,2015,35(7):2012-2016
15 GAI Rong-Yin,WANG Zheng,HE Yan-Feng,LI Qing,ZOU Hui-Jun,ZHANG Guo-Xia.Chinese J.Anal.Chem.,2014,42(11):1617-1622盖荣银,汪正,贺岩峰,李青,邹慧君,张国霞.分析化学,2014,42(11):1617-1622
16 Yang C,Wang L,Zhu Z L,Jin L L,Zheng H T,Belshaw N S,Hu S H.Talanta,2016,155:314-320
17 Liu X,Zhu Z L,He D,Zheng H T,Gan Y Q,Belshaw N S,Hu S H,Wang Y X.J.Anal.At.Spectrom.,2016,31(5):1089-1096
18 WANG Zheng,QIU De-Ren,TAO Guang-Yi,YANG Peng-Yuan.Spectroscopy and Spectral Analysis,2006,26(3):542-547汪正,邱德仁,陶光仪,扬芃原.光谱学与光谱分析,2006,26(3):542-547
19 ZHANG Jun-Ye,WANG Zheng,DU Yi-Ping,QIU De-Ren,YANG Peng-Yuan.Chinese J.Anal.Chem.,2011,39(5):658-663张军烨,汪正,杜一平,邱德仁,扬芃原.分析化学,2011,39(5):658-663
20 Xiao Q,Zhu Z L,Zheng H T,Huang C Y,Hu S D.Talanta,2013,106:114-119
21 Wang Z,Gai R,Zhou L,Zhang Z.J.Anal.At.Spectrom.,2014:29:2042-2044
22 Webb M R,Andrade F J,Hieftje G M.J.Anal.At.Spectrom.,2007,22:766-774
23 Webb M R,Andrade F J,Hieftje G M.Anal.Chem.,2007,79:7807-7812
24 Broekaert J A C,Lathen C,Brandt R,Fresenius J.Anal.Chem.,1994,349:20-25
25 WANG Zheng,WANG Shi-Wei,QIU De-Ren,YANG Peng-Yuan.Spectroscopy and Spectral Analysis,2009,29(10):2838-2842汪正,王士维,邱德仁,扬芃原.光谱学与光谱分析,2009,29(10):2838-2842
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