活化玻碳电极直接快速检测亚硝酸盐
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摘要
以活化玻碳电极作为工作电极,利用线性扫描伏安法探讨了测定NO_2~-的最佳实验条件,并优化了清洗电极的方法。结果表明,当pH=7,扫描速度100 mV/s,支持电解质为1.0 mol/L NaCl,起止电位为0.2～1.4 V时,得到最佳实验效果。NO_2~-的浓度在1.0×10~(-4)～5.0×10~(-2) mol/L范围与峰电流之间存在理想的线性关系,检测限为1.23×10~(-6) mol/L,相对标准偏差(RSD)为1.26%,加标回收率为105%,方法具有良好的重现性和准确性。并成功应用于湖水样品中亚硝酸盐的检测。
In this paper, using an electrochemical activation glassy carbon electrode as the working electrode,the optimum experimental conditions for the determination of nitrite(NO_2~-) were investigated by linear scanning voltammetry.At the same time,the method of cleaning electrode was optimized to make it simpler and faster.The results showed that the best experimental results were obtained when the pH=7 coupled with scanning speed being 100 mV/s,supporting electrolyte being 1.0 mol/L NaCl,and starting and stopping potential being 0.2-1.4 V.When the concentrations of NO_2~- were 1.0×10~(-4)-5.0×10~(-2) mol/L,the ideal linear relationship between max current(μA) and concentration(mol/L) could be observerd.In addition,the limit of detection was 1.23×10~(-6) mol/L,with the relative standard deviation of 1.26%,which indicated good reproducibility and accuracy.The recovery was 105% by standard addition method.The activated glassy carbon electrode was successfully applied to the detection of nitrite in the lake water samples.
In this paper, using an electrochemical activation glassy carbon electrode as the working electrode,the optimum experimental conditions for the determination of nitrite(NO_2~-) were investigated by linear scanning voltammetry.At the same time,the method of cleaning electrode was optimized to make it simpler and faster.The results showed that the best experimental results were obtained when the pH=7 coupled with scanning speed being 100 mV/s,supporting electrolyte being 1.0 mol/L NaCl,and starting and stopping potential being 0.2-1.4 V.When the concentrations of NO_2~- were 1.0×10~(-4)-5.0×10~(-2) mol/L,the ideal linear relationship between max current(μA) and concentration(mol/L) could be observerd.In addition,the limit of detection was 1.23×10~(-6) mol/L,with the relative standard deviation of 1.26%,which indicated good reproducibility and accuracy.The recovery was 105% by standard addition method.The activated glassy carbon electrode was successfully applied to the detection of nitrite in the lake water samples.
引文
[1] GB 1886.11-2016.Food Safety National Standard Food Additive Sodium Nitrite.National Health and Family Planning Commission of PRC(食品安全国家标准食品添加剂亚硝酸钠国家卫生和计划生育委员会).
[2] GB 5009.33-2010.Determination of Nitrate and Nitrite in Food.Ministry of Health,PRC(食品中硝酸盐、亚硝酸盐的测定中华人民共和国卫生部).
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[17] LIU Y,GU H Y.Microchimica Acta,2008,162(1-2):101.
[18] Rajesh S,Kanugula A K,Bhargava K,Ilavazhagan G,Kotamraju S,Karunakaran C.Biosensors and Bioelectronics,2010,26(2):689.
[19] Zhou L,Wang J P,Gai L,Li D J,Li Y B.Sensors and Actuators B:Chemical,2013, 181:65.
[20] Liu T S,Kang T F,Lu L P,Zhang Y,Cheng S Y.Journal of Electroanalytical Chemistry,2009,632(1-2):197.
[21] Wang P,Mai Z B,Dai Z,Li Y X,Zou X Y.Biosensors and Bioelectronics,2009,24(11):3242.
[2] GB 5009.33-2010.Determination of Nitrate and Nitrite in Food.Ministry of Health,PRC(食品中硝酸盐、亚硝酸盐的测定中华人民共和国卫生部).
[3] YU Y,JIAO F G,FAN X M.Journal of Analytical Science(于艳,焦锋刚,樊雪梅.分析科学学报),2017,33(1):142.
[4] Chatterjee S,Pillai A K,Gupta V K.Journal of the Chinese Chemical Society,2013,51(1):195.
[5] LIUH Y,YANG G H,Abdel-Halim E S,ZHU J J.Talanta,2013,104(2):135.
[6] WU F H,ZHANG Q,YANG J Q,et al.Journal of Analytical Science(吴芳辉,张琴,杨俊卿,等.分析科学学报),2018,34(2):171.
[7] YAN Y,HAN X X,FENG Y,et al.Journal of Analytical Science(闫玥,韩晓霞,冯芸,等.分析科学学报),2017,33(1):47.
[8] WANG Q H,YU L J,LIU Y,LIN L,LU R G.Talanta.2017,165:709.
[9] DAI X D,ZHANG A J,ZHANG X L.Chinese Journal of Health Laboratory Technology(戴兴德,张爱菊,张小林.中国卫生检验杂志),2015, 25(19):3266.
[10] Kozub Barbara R,Rees Neil V,Compton Richard G.Sensors and Actuators B:Chemical,2010,143(2):539.
[11] Manea F,Remes A,Radovan C,Pode R,Picken S,Schoonman J.Talanta,2010,83(1):66.
[12] DENG C Y,CHEN J Z,NIE Z,YANG M H,SI S H.Thin Solid Films,2012,520(23):7026.
[13] ZHU N N,XU Q,LI S,GAO H.Electrochemistry Communications,2009,11(12):2308.
[14] Cui Y P,Yang C Z,Zeng W,Oyama M,Pu W H,Zhang J D.Analytical Sciences,2007,23(12):1421.
[15] Eguílaz M,Agüí L,Yáňez-Sedeňo P,Pingarrón J M.Journal of Electroanalytical Chemistry,2010,644(1):30.
[16] Kamyabi M A,Aghajanloo F.Journal of Electroanalytical Chemistry,2008,614(1-2):157.
[17] LIU Y,GU H Y.Microchimica Acta,2008,162(1-2):101.
[18] Rajesh S,Kanugula A K,Bhargava K,Ilavazhagan G,Kotamraju S,Karunakaran C.Biosensors and Bioelectronics,2010,26(2):689.
[19] Zhou L,Wang J P,Gai L,Li D J,Li Y B.Sensors and Actuators B:Chemical,2013, 181:65.
[20] Liu T S,Kang T F,Lu L P,Zhang Y,Cheng S Y.Journal of Electroanalytical Chemistry,2009,632(1-2):197.
[21] Wang P,Mai Z B,Dai Z,Li Y X,Zou X Y.Biosensors and Bioelectronics,2009,24(11):3242.