Synthesis of New Type ZnO Nanomaterial and Its Application for Electrochemical Detection of p-Nitrophenol†

doi:10.7503/cjcu20160673

Abstract

Abstract:

A new type nanomaterial, peanut-like ZnO, was synthesized via hydrothermal method, and SEM and XRD were utilized to characterize and analyze the surface morphology and crystalline lattices of the nanomaterials. The electrochemical performance of the peanut-like ZnO was investigated by cyclic voltammetry, Nyquist and differential pulse voltammetry ulteriorly. The peanut-like ZnO modified electrode displayed excellent conductivity and had a strong electroreduction ability to detect p-nitrophenol, showing a good linear relationship within the concentration ranges of 0.8―24 μmol/L and 32―80 μmol/L, and the detection limits were calculated to be 0.25 μmol/L(3S/N). The modified electrodes were used to analyze and detect p-nitrophenol in real water samples with the recovery from 95.6% to 103.4%, and gave a satisfactorily result.

Key words: New type zinc oxide nanomaterial, Modified electrode, Electroreduction, p-Nitrophenol

CLC Number:

O657.1
O646

TrendMD:

HU Haixia, HU Shirong, DONG Peihui, TANG Yuanjun, HONG Kejun, WANG Songhua. Synthesis of New Type ZnO Nanomaterial and Its Application for Electrochemical Detection of p-Nitrophenol^†[J]. Chem. J. Chinese Universities, 2017, 38(7): 1171.

Figures/Tables 11

Fig.1 SEM images of ZnO(11)(A), ZnO(15)(B) and ZnO(23)(C) and high magnification SEM

Fig.2 XRD patterns(A) and FTIR spectra(B) of ZnO(11)(a), ZnO(15)(b) and ZnO(23)(c) and zeta potential of ZnO(23)(C)

Fig.3 Nyquist plots of bare GCE(a) and ZnO(23)/GCE(b) in 5 mmol/L[Fe(CN)]3-/4-+0.1 mol/L KCl(A) and CV curves of bare GCE(a) and ZnO(23)/GCE(b) in 0.1 mol/L PBS(pH=7)+20 μmol/L p-NP(B)(scan rate: 100 mV/s)

Fig.4 CV curves of ZnO(23)/GCE in 20 μmol/L p-NP and 0.01 mol/L PBS at different scan rates(A) and the relationship between peak current at about -0.8 V and square root of scan rateScan rate/(mV·s-1) from a to j: 10, 20, 40, 60, 80, 100, 120, 150, 200, 250.

Fig.5 CV curves of ZnO(23)/GCE in 20 μmol/L p-NP and 0.01 mol/L PBS at different pH values(from 4 to 9)(A) and the effect of pH on peak current at about -0.8 V(B)The inset is the plots of peak potential of p-NP vs. pH values.

Scheme 1 Schematic drawing of electrochemical sensing p-NP

Fig.6 DPV curves of different concentrations of p-NP in 0.1 mol/L PBS(pH=6)(A) and plots of peak current vs. concentration of p-NP(B)c(p-NP)/(μmol·L-1) from a to p: 0.8, 1.6, 3.2, 4.8, 6.4, 8.0, 9.6, 12, 16, 20, 24, 32, 40, 48, 64, 80.

Table 1 Characteristics of different modified electrodes

Modified electrode	Method	Linear range/(μmol·L^-1)	LOD/(μmol·L^-1)	Recovery(%)	Ref.
GO/GCE	DPV	0.1—120(R²=0.9975)	0.02	99.0—102.3	[1]
Mg(Ni)FeO/CPE^a	DPV	2—200(R²=0.9990)	0.2	96.8—100.2	[2]
OMCs^b/GCE	DPV	2.0—90(R²=0.9970)	0.1	97.2—98.8	[3]
α-CD/CRG^c/GCE	DPV	0.1—150(R²=0.9990)	0.033	96.7—102.4	[4]
rGO-Au/GCE	DPV	0.05—2.0(R²=0.9981)	0.01	98.4—104.0	[5]
CD-Au@CGS^d/GCE	DPV	0.01—200( )		97.5—105.6	[6]
ZnO/GCE	CV	10—1000(R²=0.9950)	13		[7]
GC-Co₃O₄/GCE	SWV	2—47(R²=0.9970)	0.93		[8]
ZnO/F/GCE	SWV	0.035—1.4(R²=0.9988); 2.1—6.3(R²=0.9977)	0.008	96.8—105.7	[9]
rGO-Ag/GCE	AP^e	1—10( ); 10—110( )	0.32	94.26—100.2	[10]
ZnO(23)/CHCl₃/GCE	DPV	0.8—24(R²=0.9932); 32—80(R²=0.9916)	0.25	95.6—103.4	This work

Fig.7 Stability(A) and reproducibility(B) of ZnO(23)/GCE with repetitive measurements of DPV response for 20 μmol/L p-NP in 0.1 mol/L PBS with pH=6

Fig.8 DPV of ZnO(23)/GCE in 20 μmol/L p-NP, o-NP, m-NP, and mixture of 20 μmol/L o-NP, m-NP, p-NP(0.1 mol/L PBS)

Table 2 Experimental results for determination of p-NP in water

Sample	p-NP Added/(μmol·L^-1)	p-NP Found/(μmol·L^-1)	Recovery(%)	RSD(%)
Chiu-lung river	4.8	4.62	96.3	4.4
	9.6	9.18	95.6	4.1
	20.0	20.56	102.8	3.9
Barrelled water	4.8	4.68	97.5	4.3
	9.6	9.32	97.1	3.7
	20.0	20.68	103.4	4.7

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