Arabian Journal of Chemistry (2016) 9, S1563–S1568

King Saud University

Arabian Journal of Chemistry

www.ksu.edu.sa
www.sciencedirect.com

ORIGINAL ARTICLE

Voltammetric determination of resorcinol on the

surface of a glassy carbon electrode modified with
multi-walled carbon nanotube
Sayed Mehdi Ghoreishi *, Mohsem Behpour, Elahe Hajisadeghian,
Mahshid Golestaneh

Department of Analytical Chemistry, Faculty of Chemistry, University of Kashan, Kashan, Islamic Republic of Iran

Received 7 February 2011; accepted 18 April 2012

Available online 27 April 2012

KEYWORDS Abstract A multi-walled carbon nanotubes (MWCNTs) film coated glassy carbon electrode
Multi-walled carbon (GCE) was fabricated, and the electrochemical oxidation of resorcinol (RS) was studied in
nanotubes; Britton–Robinson (BR) buffer (pH 6.0) using cyclic, square wave, and differential pulse voltamme-
Resorcinol; try (CV, SWV, and DPV). The results revealed that the modified electrode shows an electrocatalytic
Glassy carbon electrode; activity toward the oxidation of RS by a marked enhancement in the current response in buffered
Voltammetry; solution. The oxidation of RS at this nano-structured film coated electrode was irreversible and dif-
Determination fusion-controlled. Under the optimum conditions, the anodic peak current showed a linear relation
versus RS concentration in the range of 1.2 · 106 to 1.9 · 104 M with detection limits of 4.9 · 107
and 1.1 · 106 M (signal-to-noise = 3) for SWV and DPV, respectively. Moreover, the modified
electrode demonstrated good reproducibility (RSD = 2.4%, n = 10) and long-term stability. This
method has been applied to the determination of RS in wastewater, and the recoveries were from
93% to 104%.
ª 2012 Production and hosting by Elsevier B.V. on behalf of King Saud University. This is an open access
article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/3.0/).

1. Introduction

Phenolic compounds are highly toxic environmental pollutants,

and seriously threaten human’s health. They are widely used in
* Corresponding author. Tel.: +98 3615552930; fax: +98 many fields, such as tanning, cosmetic, dye, chemical and phar-
3615552935. maceutical industries (Wang et al., 2007). Phenolic compounds
E-mail address: s.m.ghoreishi@kashanu.ac.ir (S.M. Ghoreishi). in environment come from different sources, including indus-
Peer review under responsibility of King Saud University. trial wastewater, solid castoff of coal tar, coking factory, gas-
works, paper mill, chemical plants and pharmaceutical
industry (Ware, 1992). Some of the phenolic compounds have
been listed as control targets because of their toxicities in many
Production and hosting by Elsevier
countries. Phenolic compounds are also poisonous organic
http://dx.doi.org/10.1016/j.arabjc.2012.04.009
1878-5352 ª 2012 Production and hosting by Elsevier B.V. on behalf of King Saud University.
This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/3.0/).
S1564
pollutants. Therefore, many governments have spent a lot of ef-
fort in their detection and control.
Resorcinol (RS) is one kind of phenolic compounds with
high toxicity. It can be easily absorbed through the gastric tract
and human skin, which can cause dermatitis, catarrh, convul-
sion, cyanopathy, and even death (Guardia et al., 1995). At pres-
ent, various methods have been employed for RS determination,
including spectrophotometric (Kang et al., 2000), high-perfor-
mance liquid chromatography with diode array detection
(Yang et al., 2006), microchip capillary electrophoresis with
end channel amperometric detection (Wu and Lin, 2006), quartz
crystal microbalance (Mirmohseni and Oladegaragoze, 2004),
flow injection chemiluminescence (Du et al., 2001), surface plas-
mon resonance (Wright et al., 1998), fluorescence (del Olmo
et al., 2000; Pistonesi et al., 2006) and spectrofluorimetric (Fan
et al., 2007; Wenxiang and Dan, 2007).
Electrochemistry has always provided analytical techniques
characterized by instrumental simplicity, moderate cost, and
portability. These techniques have introduced the most promis-
ing methods for specific applications (Goyal et al., 2006, 2007a,
2009a; Gupta et al., 2010, 2011a). But these methods normally
have low sensitivity at conventional electrodes. However, low
sensitivity and poor selectivity of electrochemical methods can
be overcome by electrode modification (Goyal et al., 2005,
2007b, 2007c, 2008a, 2008b; Gupta et al., 2011b).
Carbon nanotubes (CNTs) are a novel nanoscale material,
mainly consisting of SWCNTs and MWCNTs (Bethune et al.,
1993; Fernandez-Abedul and Costa-Garcia, 2008). These nano-
scale materials have attracted considerable interest owing to
their extraordinary mechanical and unique electrochemical
properties (Goyal et al., 2008c). The subtle electronic behavior
of CNTs demonstrates that they have the ability to promote
electron-transfer reactions when used as electrode materials
(Nugent et al., 2001). Several types of CNT electrodes have been
reported, including CNT paste electrodes (Davis et al., 1997;
Valentini et al., 2003), CNT film-coated electrodes (Luo et al.,
2001; Guo et al., 2004), CNT powder microelectrodes (Zhao
et al., 2002) and CNT paper electrodes (Barisci et al., 2000).
CNT-modified GCEs provide a stable and sensitive electro-
chemical response for phenols (Wang et al., 2003), NADH
(Musameh et al., 2002), estrogenic phenolic compounds (Vega
et al., 2007a,b; Agui et al., 2007), ascorbic acid, dopamine
(Wu and Hu, 2004), uric acid (Wu and Hu, 2004) and tetracy-
cline (Vega et al., 2007a).
The main objective of this work was to develop a simple
and sensitive electrochemical sensor for the determination of
RS. Based on the good electrocatalytic activity of MWCNT
modified GCE toward the electrochemical oxidation of RS, a
sensitive electrochemical method has been proposed for the
determination of RS.
2. Experimental
2.1. Chemicals and reagents
Resorcinol was purchased from the MERCK Company. BR
buffer solution was made up of phosphoric acid (MERCK), bo-
ric acid (MERCK), and ice acetic acid from the MERCK and its
pH value was adjusted with NaOH (MERCK). MWCNTs with
purity of >95% (40–60 nm in diameter) were obtained from the
Chinese Academy of Sciences. Generally, pristine MWCNTs
S.M. Ghoreishi et al.
contained 3% amorphous carbon, SWCNTs, and graphite
requiring some purification pre-treatments before electro-ana-
lytical characterization. MWCNTs refluxed under stirring for
5 h in concentrated nitric acid. It has been reported that this
treatment could purify the CNTs and cause carboxylation at
their termini (Tsang et al., 1994; Hiura et al., 1995). A
1.0 · 103 M RS standard solution was simply prepared by dis-
solving RS in deionized water. Working solutions were prepared
with this standard solution and using suitable dilution with a
0.1 M BR buffer solution. BR buffer solution was also used as
the supporting electrolyte.
2.2. Apparatus
Electrochemical measurements were carried out on a M273
electrochemical workstation (EG&G Corporation, USA) with
a conventional three-electrode system. This equipment was
equipped with a platinum plate (Metrohm) as the counter elec-
trode, a saturated calomel electrode (SCE) from Metrohm as
the reference electrode and a MWCNT/GCE as the working
electrode. Solution pH values were determined using a 691
pH meter (Metrohm Swiss made) combined with glass elec-
trode (Metrohm). Deionized water was formed with an ultra-
pure water system (smart 2 pure, TKA, Germany). MWCNT
was dispersed with an ultrasonic bath (SONOREX DIGITAL,
10P, BANDELIN). Data were collected at room temperature.
2.3. Fabrication of the modified electrode
Using ultrasonic agitation, 0.5 mg of purified MWCNTs was
dispersed into 5 ml of redistilled water for 30 min. Prior to
modification, the GCE was polished with 0.05 mm alumina
slurry and then cleaned ultrasonically in double-distilled water.
Subsequently, the GCE was coated with 20 lL of MWCNT
suspension and the solvent was evaporated in air.
2.4. Analytical procedure
Twenty milliliters of 0.1 M BR buffer solution (pH 6.0) contain-
ing a specific amount of standard solution of RS was added to an
electrochemical cell. Electrochemical measurements were carried
out by CV and recorded in the potential range of 0.1–1.0 V at a
scan rate of 20 mV s1. DPV employed the following parameters:
Einitial = 0.3 V, Efinal = 0.9 V, scan rate = 20 mV s1. SWV was
recorded from 0.3 to 0.9 V and the current peak at 0.6 V was mea-
sured. The SWV parameters were as follows: SWV fre-
quency = 80 Hz, pulse height = 100 mV, amplitude = 10 mV.
3. Results and discussion
3.1. Voltammetric behavior of RS at MWCNT/GCE
Fig. 1 shows the cyclic voltammograms (CVs) of 5.0 · 105 M
RS on a bare GCE and MWCNT–GCE in 0.1 M BR buffer
solution (pH 6.0). Compared to the bare electrode, the anodic
peak current of RS increased significantly at the modified
electrode. Also, the oxidation peak potential shifted to the
negative values (Fig. 1a) in contrast to those at the bare elec-
trode (Fig. 1b), which indicated that the modified electrode
has a catalytic effect on the oxidation of RS. The following
reasons might explain the electrocatalytic response of RS on
Voltammetric determination of resorcinol on the surface of a glassy carbon S1565

4 800
y= 0.985 – 0.07x
2 700 R2= 0.9972

0 600

E/mV
I/10-6A

-2 c 500

-4 b 400

-6 300
a
-8 200
0 500 1000 3 4 5 6 7 8 9 10
E/mV pH

Figure 1 Cyclic voltammograms of 5.0 · 105 M RS in 0.1 M Figure 3 The relationship between the pH values (from 4 until 9)
BR buffer (pH 6.0) at scan rate of 20 mV s1 (a) on a MWCNT/ and the anodic peak potentials obtain from SWV at scan rate of
GCE; (b) on bare electrode; (c) absence of RS on a modified 20 mV s1.
electrode.

the surface of MWCNT/GCE. First, the treatment of HNO3
introduced many active groups on the surface of the CNTs,
e.g. ACOOH, AC‚O and AOH. These active groups could
form hydrogen bonds with the AOH groups of the RS, which
weakened the AOH bond energies, and the electrons would be
transferred through O  HAO. Second, due to the unique elec-
tronic structures of the CNTs, they can act as a promoter to
enhance the electrochemical reaction. The huge specific surface
area of CNTs can also increase the effective area of the elec-
trode. So the peak current increased and the oxidation poten-
tial shifted negatively (Ding et al., 2005).
Fig. 1c shows the cyclic voltammogram of the modified
electrode in the absence of RS. The electro-oxidation of RS
is an irreversible process, because no corresponding reductive
peak observed on the cathodic branch.
3.2. Effect of scan rate
the diffusion-controlled process of RS on the surface of
MWCNT/GCE.
The linear regression equation was ipa = 0.9647 + 0.0038
v1/2 (ipa: A, v: mV s1) with the correlation coefficient of
0.9982 (Fig. 2, inset).
3.3. Effect of pH
The electrochemical behavior of RS was investigated over the
pH range from 4.0 to 9.0 in 0.1 M BR buffer solution. Fig. 3
shows the square wave voltammograms of 5.0 · 105 M RS
in 0.1 M BR buffer solution. The peak potential shifted to
the negative values by increasing the pH. The negative shift
in anodic peak potential (Epa) with pH can be described by
the following equation:
Epa ðV versus SCEÞ ¼ 0:985  0:07 pH r ¼ 0:9972 ð1Þ

The oxidation peak current of 4.0 · 104 M RS was measured The slope of the regression Eq. (1) is close to the theory va-
with CV at different scan rates from 20 to 200 mV s1 (Fig. 2). lue of 58.5 mV pH1 for two electrons and two protons pro-
By increasing the scan rate, the heights of oxidation peak were cess (Sun et al., 2010; Wu et al., 2010; Yin et al., 2011),
increased. Also, peak potential shifted toward more positive indicating that the electrochemical redox of RS at MWCNT/
values for oxidation process. Oxidation peak current varied GCE should be a two electrons and two protons process
linearly with the square root of scan rate (m1/2), demonstrating (scheme 1). The relationship between the peak current and
pH was investigated (Fig. 4). As can be seen the peak current
in pH 6.0 is maximum, therefore pH 6.0 was chosen as the
2
optimum pH and this pH was used in all the following exper-
1 iments. After that, the oxidation potential was observed to de-
0 crease by increasing the pH and above pH 9.0, the oxidation
peak current no longer appeared. Therefore a weak acidic
-1
solution was better for the experiments.
I/10-6A

y =0.9647+0.0038x
-2 1.7
2
R = 0.9982

-3
1.6
1.5
3.4. Calibration curve
1.4
I/10 -6A

1.3
-4 1.2
1.1 The relationship between the oxidation peak current and RS
1
-5 0.9 concentration was examined using DPV and SWV methods.
0 30 60 90 120 150 180 210
V 1/2 /mVs -1
-6
0 200 400 600 800 1000
HO OH O O
E/mV
+
-2H +
Figure 2 Cyclic voltammograms of MWCNT/GCE in 0.1 M BR +2H +2e
buffer (pH 6.0) containing 4.0 · 104 M RS at different scan rates.
Inset: The relationship between anodic current and scan rates. Scheme 1 Mechanism of RS oxidation at MWCNT/GCE.
S1566 S.M. Ghoreishi et al.

1.1 -8

1 -9
0.9 -10
0.8 y= 0.154+0.0211x
-11

I/10-6A
R2=0.9994
I/10-6A

0.7 4.5
4
-12 3.5
3
0.6

I/10-6A
2.5
-13 2
1.5
0.5 1
0.5
-14 0
0.4 0 50 100 150 200 250
C/10-6mol L-1
-15
0.3
100 300 500 700 900
0.2 E/mV
3 4 5 6 7 8 9 10
pH Figure 6 SWV of RS at MWCNT/GCE in 0.1 M BR (pH 6.0)
with different concentrations (1.2 · 106 to 1.9 · 104 M). (Inset)
Figure 4 The relationship between the pH values (from 4 until 9) linear relationship between ipa and CRS.
and the anodic peak current obtain from SWV at scan rate of
20 mV s1.

-300
Table 2 Recovery data observed for RS at different concen-
-400 trations. Analysis carried out by SWV.
-500 Sample no. Added (lM) Founded (lM) Recovery (%)
1 4.00 3.89 97.1
-600 2 6.00 5.81 97.3
3 8.00 7.42 93.0
-700 y= 0.024+0.0033x
I/10-6A

2
R =0.9988 4 9.00 9.46 104.0
0.7
-800 0.6

0.5

-900 0.4
I/ 10-6A

0.3
(pH 6.0). Inset in Fig. 5 shows the linear relationship between
0.2
-1000 ipa and CRS. The linear regression equation is expressed as ipa
0.1

0 (lA) = 0.0033c (lM) + 0.024 (r = 0.9988). When the signal-

-1100 0 50 100 150
C/ 10-6 mol L -1
-1200
0 200
Figure 5 Differential pulse voltammograms of RS at various
concentrations (1.2 · 106 to 1.9 · 104 M) MWCNT/GCE in
0.1 M BR (pH 6.0) at electrode with different concentrations.
(Inset) linear relationship between ipa and CRS.
The oxidation peak current was found to be proportional to RS
concentration over the ranges of 1.2 · 106 to 1.9 · 104 M.
Fig. 5 shows the differential pulse voltammograms obtained
for RS at various concentrations in 0.1 M BR buffer solution
200 250
to- noise ratio was 3, the detection limit was 1.1 · 106 M.
Since SWV is one of the popular techniques for carrying
400 600 800 1000 out the analysis in various samples, due to its high sensitivity
E/ mV and multi-analysis capability, it has been utilized in the present
investigation to estimate the detection limit of RS (Goyal et al.,
2009b). Fig. 6 shows the SWV results obtained for the oxida-
tion of different concentrations of RS at the modified
electrode. The linear regression equation is expressed as ipa
(lA) = 0.0211c (lM) + 0.154 (r = 0.9994). When the signal-
to- noise ratio was 3, the detection limit was 4.9 · 107 M,
which is lower than the DPV value of 1.1 · 106 M. Which val-
ues of detection limit is comparable to values reported by other
research groups for electrocatalytic oxidation of RS at the
surface of modified electrodes (Table 1).

Table 1 Comparison of the efficiency of some modified electrodes used in the electro-analysis of RS.
Modified electrodes Detection limit (lmol l1) Dynamic range (lmol l1) Reference
Graphene–chitosan/GCE 0.75 1–550 Yin et al. (2011)
SWNTs/GCE 0.3 0.4–10 Wang et al. (2007)
40–100
MWNTs/GCE 1 5–80 Ding et al. (2005)
MWNTs/multielectrode array 0.6 6–100 Zhang et al. (2009)
MWNTs/GCE 0.49 1.2–190 This work
Voltammetric determination of resorcinol on the surface of a glassy carbon
3.5. Stability of the MWCNT/GCE
The reproducibility of MWCNT/GCE was examined by repeat-
ing the measurement of 4.0 · 104 M RS. After each determina-
tion, the used modified electrode underwent five successive cyclic
voltammetric sweeps between 0.1 and 1.0 V at a scan rate of
20 mV s1 in 0.1 M BR (pH 6.0) to remove any adsorbents and
yield a reproducible electrode surface. The relative standard devi-
ation (RSD) of ten measurements was 2.4%. The long-term
stability of the MWCNT/GCEs was also tested by measuring
the oxidation peak current at a fixed RS concentration of
4.0 · 104 M over a period of 3 weeks. After 3 weeks, the current
response only decreased by 4.4%. These results indicate that the
electrode has excellent reproducibility and long-term stability,
making it attractive for the fabrication of chemical sensor.
3.6. Interferences
The effect of possible interference was investigated by the addi-
tion of other species to a solution containing 1.0 · 105 M RS in
0.1 M BR electrolytes. Each possible contaminant was first
added to yield a concentration identical to that of RS. Subse-
quently, another addition was made so that the interfering con-
centration was 10 times more than RS. Ascorbic acid, uric acid,
penicillin, aspirin, and amoxicillin were tested. Uric acid, peni-
cillin, aspirin and ascorbic acid were found to cause less than a
9% increase in the RS current peak height, even when present in
10-fold excess. The presence of amoxicillin in 10-fold excess of
RS was sufficient to cause a 6% decrease in RS signal.
3.7. Recovery test
We prepared an artificial wastewater by mixing the different
phenolic compounds and drug and the experiments were car-
ried out under optimal conditions. Different concentrations
of RS were added to this artificial wastewater and the RS con-
tents were determined by SWV. Then the recoveries of five
measurements and RSD were calculated and the results are
summarized in Table 2.
4. Conclusions
In this work, the MWCNTs-modified GCE was used for the
determination of RS by SWV and DPV methods, quantita-
tively. The modified electrode exhibited electrocatalytic activ-
ity for the oxidation of RS associated with negative shift in
anodic peak potential. The method provided a simple, conve-
nient and fast route to detect the concentration of RS.
Acknowledgements
The authors are grateful to University of Kashan for support-
ing this work by Grant No. 1591959.
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