氧化锌-还原氧化石墨烯-多壁碳纳米管复合材料修饰电极检测对硝基苯酚
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摘要
以乙二醇(EG)为溶剂,柠檬酸钠为还原剂,采用一步溶剂热法制备了氧化锌(ZnO)-还原氧化石墨烯(r GO)-多壁碳纳米管(MWCNT)复合材料(ZnO-rGO-MWCNT),利用扫描电镜(SEM)和X-射线粉末衍射(XRD)技术对其形貌和组成进行了表征。通过滴涂法制备了ZnO-rGO-M WCNT/GCE电极。在对其电化学性质研究的基础上研究了对硝基苯酚(4-NP)在该修饰电极上的电化学行为。结果表明,在各组分的协同作用下,此电极对4-NP的电极过程表现出高的电化学活性。在pH 7. 0的PBS溶液中,一阶导数伏安法检测4-NP的线性范围为0. 5～50μmol/L,检出限(3Sb)为0. 1μmol/L。该电极用于延河水样中4-NP的测定,加标回收率为96. 9%～102. 4%。
A zinc oxide-reduced graphene oxide-multi-walled carbon nanotubes composite( Zn O-rGOMWCNT) modified electrode was fabricated by two steps. Firstly,Zn O-rGO-MWCNT was prepared by hydrothermal method which utilized ethylene glycol as sovent and sodium citrate as reducing agent. The morphology and composition of this ZnO-rGO-MWCNT composites were studied by scanning electron microscopy( SEM) and X-ray diffraction technology,respectively. Secondly,this composite was modified on glassy carbon electrode surface using drooping method to form ZnO-rGO-MWCNT/GCE.The electrochemical behavior of 4-nitrophenol( 4-NP) on the modified electrode was investigated. The results showed that this modified electrode exhibited high electrochemical activity for 4-NP under the synergic action of the components in the composite. The determination of 4-NP in 0. 1 mol/L PBS( pH7. 0) illustrated a linear range from 0. 5 to 50 μmol/L. The detection limit is 0. 1 μmol/L( 3 Sb).This modified electrode was successfully used to determine 4-NP in the water sample collected from the river,and a recovery range of 96. 9%-106. 4% was obtained.
A zinc oxide-reduced graphene oxide-multi-walled carbon nanotubes composite( Zn O-rGOMWCNT) modified electrode was fabricated by two steps. Firstly,Zn O-rGO-MWCNT was prepared by hydrothermal method which utilized ethylene glycol as sovent and sodium citrate as reducing agent. The morphology and composition of this ZnO-rGO-MWCNT composites were studied by scanning electron microscopy( SEM) and X-ray diffraction technology,respectively. Secondly,this composite was modified on glassy carbon electrode surface using drooping method to form ZnO-rGO-MWCNT/GCE.The electrochemical behavior of 4-nitrophenol( 4-NP) on the modified electrode was investigated. The results showed that this modified electrode exhibited high electrochemical activity for 4-NP under the synergic action of the components in the composite. The determination of 4-NP in 0. 1 mol/L PBS( pH7. 0) illustrated a linear range from 0. 5 to 50 μmol/L. The detection limit is 0. 1 μmol/L( 3 Sb).This modified electrode was successfully used to determine 4-NP in the water sample collected from the river,and a recovery range of 96. 9%-106. 4% was obtained.
引文
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[2] Niazi A,Yazdanipour A. J. Hazard. Mater.,2007,146(1-2):421
[3] Luo B R,Wan X,Deng X L,Yu Y Y,Xie Z W. Chinese J. Chromatogr.,2016,34(5):473罗碧容,万旭,邓星亮,余媛媛,谢振伟.色谱,2016,34(5):473
[4] Guo X F,Wang Z H,Zhou S P. Talanta,2004,64(1):135
[5] Huo F,Yuan H Y,Yang X P,Xiao D,Choi Martin M F. Anal. Sci.,2011,27(9):879
[6] Li X,Wang X L. Chin. J. Anal. Lab.,2016,35(3):301李鑫,王学亮.分析试验室,2016,35(3):301
[7] Wang J M,Fan Z F. Chin. J. Anal. Lab.,2015,34(9):1086王峻敏,范哲锋.分析试验室,2015,34(9):1086
[8] Barman K,Changmai B,Jasimuddin S k. Electroanalysis,2017,29(12):2780
[9] Zhang C,Govindaraju S,Giribabu K,Huh Y S,Yun K. Sens. Actuators B,2017,252:616
[10] Chu L,Han L,Zhang X. J. Appl. Electrochem.,2011,41(6):687
[11] Bashami R M,Hameed A,Aslam M,Ismail Iqbal M I,Soomro M T. Anal. Methods,2015,7(5):1794
[12] Sinhamahapatra A,Dhrubajyoti B,Yu J S. RSC Adv.,2015,5(47):37721
[13] Gu Y E,Zhang Y Z,Zhang F Y,Wei J P,Wang C M,Du Y L,Ye W C. Electrochim. Acta,2010,56(2):953
[14] Wu J W,Wang Q,Umar A,Sun S H,Huang L,Wang J Y,Gao Y S. New J. Chem.,2014,38(9):4420
[15] Noorbakhsh A,Mirkalaei M M,Yousefi M H,Manochehri S. Electroanalysis,2014,26(12):2716
[16] Luo L Q,Zou X L,Ding Y P,Wu Q S. Sens. Actuators B,2008,135(1):61
[17] Wiench P,Grzyb B,Gonzalez Z,Menendz R,Handke B,Gryglewicz G. J. Electroanal. Chem.,2017,787(2):80
[18] Woo S,Kim Y R,Chung T D,Piao Y Z,Kim H. Electrochim. Acta,2012,59(1):509
[19] Yu H,Feng X,Chen X X,Qiao J L,Gao X L,Xu N,Gao L J. Chinese J. Anal. Chem.,2017,45(5):713于浩,冯晓,陈先霞,乔金丽,高小玲,高楼军.分析化学,2017,45(5):713