Sensors and Actuators B 177 (2013) 898903

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Sensors and Actuators B: Chemical

journal homepage: www.elsevier.com/locate/snb

Synthesis of Pt doped TiO2 nanoparticles: Characterization and application for

electrocatalytic oxidation of l-methionine
Fereshteh Chekin a, , Samira Bagheri b , Sharifah Bee Abd Hamid b
a
b

Department of Chemistry, Islamic Azad University, Ayatollah Amoli Branch, Amol, Iran
Centre for Research in Nanotechnology & Catalysis (NANOCEN), IPS Building, University of Malaya, 50603 Kuala Lumpur, Malaysia

a r t i c l e

i n f o

Article history:
Received 7 October 2012
Received in revised form
29 November 2012
Accepted 1 December 2012
Available online xxx
Keywords:
Pt doped TiO2 nanoparticles
Carbon nanotubes
Methionine
Electrocatalysis

a b s t r a c t
In this research, we reported a novel method for synthesis of Pt doped TiO2 nanoparticles (PtTiO2 )
by solgel assisted method. The synthesized Pt doped TiO2 nanoparticles were characterized using Xray diffraction (XRD), transmission electronic microscopy (TEM) and FT-IR techniques. To investigate
the catalytic efciency of PtTiO2 nanoparticles, the electrooxidation of l-methionine (l-Met) using the
deposited lm of Pt doped TiO2 nanoparticles and carbon nanotubes composite on glassy carbon electrode
(PtTiO2 /CNT/GCE) was studied in buffer solution (pH 7.00) using cyclic voltammetry (CV). Bare GCE
shows an ill-dened oxidation wave around 1.4 V for l-Met whereas PtTiO2 /CNT/GCE shows a welldened oxidation peak at 1.1 V. The modied electrode does not show any fouling effect toward the
oxidation of l-Met. Amperometry method was used to determine l-Met in the concentration range of
0.5100 M with a detection limit of 0.1 M (S/N = 3). The selectivity of the reaction has been assessed
with no interference from tyrosine, lysine, cysteine, tryptophan, alanine and glutathione. The present
modied electrode shows good recovery results for spiked l-Met in human blood serum sample.
2012 Published by Elsevier B.V.

1. Introduction
Titanium dioxide (TiO2 ) with an energy band of about 3.2 eV has
various applications, such as optical coating, dye sensitized solar
cell, and gas sensors [1,2]. TiO2 has three polymorphic forms of
crystal structure: brookite, anatase and rutile. The photocatalytic
activity of TiO2 is dependent on its crystal structure, crystal size distribution, surface roughness, surface hydroxyl group density, etc.
[3]. The photocatalytic activity of TiO2 can be signicantly improved
by doping with noble metals such as platinum (Pt), which acts as
the photogenerated electron acceptor [49]. Thus, under UV illumination, the photogenerated electrons effectively transfer from the
TiO2 surface to the doped Pt particles to suppress the recombination of electrons and holes and promote the transfer of holes on the
TiO2 surface. This produces a longer electronhole pair separation
lifetime, resulting in improved quantum yield and photocatalytic
efciency [10].
Methionine is an essential amino acid with an important role in
biological methylation reactions. It constitutes the main supply of
sulfur in the diet, preventing disorders in hair, skin or nails. Moreover, it helps to reduce cholesterol levels by increasing the lecitin
production in liver, being also a natural chelating agent for heavy
metals. Methionine can be present in real samples at different

Corresponding author.
E-mail address: fchekin@yahoo.com (F. Chekin).
0925-4005/$ see front matter 2012 Published by Elsevier B.V.
http://dx.doi.org/10.1016/j.snb.2012.12.002

concentration level, from near 0.1% (w/v) in some drugs to

105 mol l1 in blood plasma [11]. Methionine deciencies have
been attributed to toxemia, muscle paralysis, hair loss, depression, schizophrenia, parkinsons disease, liver deterioration and
impaired growth [12]. Since methionine cannot be synthesized in
the body it must be obtained from food supplies and pharmaceutical supplements are commercially available [13].
Flow injection [14], chromatography [15], atomic absorption
[16] and colorimetric [17] methods have been employed for the
determination of l-Met. These methods have several disadvantages such as high cost, long analysis time and low sensitivity.
Therefore, these methods were unsuitable for routine analysis.
On the other hand, determination of l-Met by electrochemical
method has several advantages which include high sensitivity
and selectivity and reproducibility. Determination of l-Met using
chemically modied electrodes is one of the attractive methods.
Only few reports were available in the literature for the determination of l-Met which include screen printed graphite macro
electrode [18], carbon electrode modied with ruthenium metallodendrimer multi layers [19], conducting composite electrode
doped with Ru(II) metallodendrimer [20], fullerene-C60 modied
gold electrode [21] colloidal gold-cysteamine modied carbon
paste electrode [22], boron doped diamond and glassy carbon electrodes [23], nickel powder doped carbon ceramic electrode [24]
1,8,15,22-tetraaminophthalocyanato-copper(II) modied glassy
carbon electrode [25]. However, these electrodes have several
drawbacks including tedious preparation.

F. Chekin et al. / Sensors and Actuators B 177 (2013) 898903

899

In the present work, we focused on synthesis and catalytic activity of PtTiO2 system. There are many methods adopted to prepare
Pt doped TiO2 . Pt doped TiO2 nanoparticles by solgel method are
of considerable interest due to its low cost, easy preparation and
industrial viability. The Pt doped TiO2 nanoparticles and carbon
nanotubes composite modied glassy carbon electrode was investigated for the electrochemical oxidation of methionine using cyclic
voltammetry. The present modied electrode shows good results
for determination of l-Met.
2. Experimental
2.1. Materials and apparatus
Titanium tetra isopropoxide with purity 98% was obtained from
Acros Organics. Platinum chloride and l-Met were purchased from
Aldrich. Glacial acetic acid (100%) was purchased from Merck. Carbon nanotubes were purchased from Shenzhen Nano-Technologies
Port Co., Ltd. (China) and were puried using a mixture of sulfuric acid and nitric acid in a composition of 3/2 by volume. Other
reagents were of analytical grade and purchased from Aldrich or
Merck and used as received without further purication.
Bruker D8 powder X-ray diffraction (XRD) was used for determination of crystal phase identication and estimation of the
crystallite size. LEO-Libra 120 microscope was employed for Pt
doped TiO2 nanoparticles transmission electron microscopy (TEM)
images. Fourier transform infrared spectroscopy (FT-IR) studies
were carried out with BRUKER FT-IR spectrometer. OXFORD (INCA
Energy 400) energy dispersive spectroscopy (EDS) was used for the
elemental analysis and chemical characterization of the sample.
2.2. TiO2 nanoparticles precursor solution
The precursor solution was prepared by dissolving titanium
tetra isopropoxide (TTIP) in the glacial acetic acid (AA), followed
by the addition of H2 O. The mol ratio of TTIP:AA:H2 O must be kept
at 1:10:200 in order to produce a clear solution. The solution was
then be stirred for several hours.
2.3. Synthesis of Pt doped TiO2 nanoparticles
The precursor solution was made as above mentioned. Dopant
(Pt) solution was prepared by dissolving platinum chloride into the
deionized water at 60 C. The amount of dopant used in this study
is 5 wt.%. Then, the dopant solution was added drop wise into the
precursor solution for a few minutes. The solution was dried at
the temperature of 80 C overnight. The dried gel was grinded and
calcined in a mufe furnace at 500 C for 5 h.
2.4. Fabrication of PtTiO2 /CNT/GCE
Prior to modication, the bare GCE (geometric area = 0.025 cm2 )
was polished on chamois leather with 0.05 m alumina powder.
Then it was thoroughly sonicated in deionized water and absolute
ethanol, respectively. 1 mg of multi wall carbon nanotube and 1 mg
of synthesized PtTiO2 was dispersed in 5 mL dimethyl formamide
(DMF) with the aid of ultrasonic agitation. The cleaned GCE was
coated by casting 5 L of the PtTiO2 and CNT composite solution
and dried at 50 C in an oven air to remove the solvent.

Fig. 1. XRD patterns of (a) PtTiO2 , (b) TiO2 and (c) PtTiO2 /CNT composite.

the titania samples exist only in anatase phase, with their characteristic diffraction peaks of 2 values at about 25.4 (1 0 1), 37.9
(0 0 4), 48.2 (2 0 0), 54.0 (1 0 5), 55.1 (2 1 1) and 62.9 (2 0 4), respectively. In consequence, the prepared TiO2 and Pt/TiO2 powders are
well-crystallized pure anatase form. From the maximum diffraction peak at Fig. 1 by Scherrers formula (D = K/ cos , where
D is the crystallite size, K the Sherrer constant usually taken as
0.89,  the wavelength of the X-ray radiation (0.15418 nm for Cu
K), and is full width half maximum of diffraction peak measured at 2, the average particle sizes of pure PtTiO2 (Fig. 1a)
and TiO2 (Fig. 1b) powders for (1 0 1) plane, are about 10 nm and
12 nm, respectively. In comparison with XRD pattern of pure TiO2 ,
Pt loaded on TiO2 surface nearly has not inuence on crystalline
structure and particle size. Pt phase has not been detected in the
XRD patterns of Pt/TiO2 powders, possibly because the Pt content
on TiO2 surface is not enough to form clearly crystalline. Also, Fig. 1c
shows XRD patterns of PtTiO2 /CNT composite that has diffraction peaks of TiO2 and Pt/TiO2 . The peak at 2 value of 25 is broad
indicating (0 0 2) phase of CNT and (1 0 1) phase of TiO2 have overlapped.
Fig. 2a and b shows the FT-IR spectra of undoped and doped
TiO2 -NPs in range of 4004000 cm1 which were synthesized via

3. Results and discussion

3.1. Characterization of Pt doped TiO2 nanoparticles
Fig. 1 shows XRD patterns of TiO2 and Pt/TiO2 powders calcined at 500 C under air for 5 h. From the wide angle XRD pattern,

Fig. 2. FT-IR patterns of (a) TiO2 and (b) PtTiO2 .

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F. Chekin et al. / Sensors and Actuators B 177 (2013) 898903

Fig. 3. TEM images of (a) TiO2 , (b) PtTiO2 and (c) PtTiO2 /CNT. The histogram of the diameter distribution of (d) TiO2 and (e) PtTiO2 . (f) EDS pattern of PtTiO2 .

the solgel method. In undoped TiO2 -NPs (Fig. 2a), the peaks at
468 cm1 and 650 cm1 are for O Ti O bonding. The band centered
at 1618 cm1 is characteristic of -H2 O bending. The broad absorption bands between 400 cm1 and 800 cm1 are mainly ascribed
to Ti O and O Ti O exion vibration. However, the vibration
bands between 1300 cm1 and 4000 cm1 are mainly assigned to
the chemisorbed and/or physisorbed H2 O and CO2 molecules on the
surface of the compound. When metal ions are doped to the surface
of TiO2 , the absorption band transforms and simultaneously new
absorption band appears. Upon addition of dopant, a small shift was
detected for the stretching vibration of TiO [26].
TEM micrographs of TiO2 , PtTiO2 and PtTiO2 /CNT composite are shown in Fig. 3. Electron microscopy analyses reveal that
TiO2 (Fig. 3a) and PtTiO2 (Fig. 3b) samples exhibit similar morphology. The presence of differently sized TiO2 grain agglomerates
over the mats of carbon nanotubes is observed (Fig. 3c). It is well
recognized that the TiO2 CNTs bonding can be formed through
some physic/chemical interactions such as Vander Waals force, Hbonding and other bonds. For example, Ti surface atoms on TiO2
may possibly react with the OH and COOH groups on the functionalized MWNTs, and thus the bonding C O Ti or O C O Ti
might form through a dehydration reaction. The size histograms of
the TiO2 (Fig. 3d) and PtTiO2 (Fig. 3e) are shown beside the TEM
images. The histograms show that the main particle size of the TiO2
and PtTiO2 was about 13 and 16 nm, respectively. Energy dispersive X-ray spectroscopy (EDS) of PtTiO2 is shown in Fig. 3f which
conrms the existence of Ti, O and Pt with weight percent.

1.2 V (Fig. 4) exhibits a typical H+ ion electro-adsorption/desorption

region, a double layer charging current region, a Pt pre-oxidation
region and a Pt oxy-species reduction region. In the proton adsorption/desorption region, current peaks observed at 0 V and 0.1 V,
which corresponds to polycrystalline Pt, conrmed the existence
of Pt, as evidenced by EDS, FT-IR and TEM.
The integrated area under the adsorption peak in the CV curve
represents the total charge concerning H+ adsorption, QH , and has

3.2. Electrochemical behavior of PtTiO2 /CNT/GCE

The cyclic voltammetry (CV) curve of PtTiO2 /CNT/GCE in 0.1 M
H2 SO4 solution at 50 mV s1 in a potential window of 0.3 to

Fig. 4. Cyclic voltammograms of PtTiO2 /CNT/GCE in 0.1 M H2 SO4 solution at scan

rate 50 mV s1 .

F. Chekin et al. / Sensors and Actuators B 177 (2013) 898903

Fig. 5. Cyclic voltammograms of GCE in the (a) absence and (b) presence of 0.1 mM
l-Met and (c) as (b) at PtTiO2 /CNT/GCE in 0.1 M PBS solution (pH 7.00) and 0.1 M
KCl at scan rate of 50 mV s1 .

been used to determine electrochemical surface area (ECSA) by

employing the equation [27]:
ECSA [m2 g1 of Pt] =

901

Fig. 6. Currenttime curve of PtTiO2 /CNT/GCE with successive addition of l-Met

to a stirred 0.1 M PBS (pH 7.00). The inset is the calibration curve.

with higher oxidation current and less positive potential for l-Met
at PtTiO2 /CNT/GC electrode was attributed that the oxidation of
l-Met was catalyzed by PtTiO2 /CNT.

QH [C m2 ]
210 [C m

] electrode loading [g of Pt/m2 ]

The ECSA of Pt is determined to be 84.79 m2 g1 for our

PtTiO2 /CNT catalyst, which is higher than for pt nanoparticles functionalized graphene sheets catalyst (32.13 m2 g1 ),
Pt-chemically reduced graphene catalyst (11.50 m2 g1 ), Ptthermally reduced graphene catalyst (20.00 m2 g1 ), PtVulcan
catalyst 30.10 m2 g1 ), Pt-graphene catalyst (44.60 m2 g1 ) and
Ptgraphene oxide catalyst (16.90 m2 g1 ) [28,29].
3.3. Electrochemical determination of l-Met at PtTiO2 /CNT
composite lm modied GCE
We have examined the electrocatalytic activity of PtTiO2 lm
deposited on GCE toward l-Met electrooxidation in buffer solution
(pH 7.00) using cyclic voltammetry (Fig. 5). We obtained higher
oxidation current with less positive potential for l-Met at pH 7.00.
Bare GCE shows an oxidation wave at 1.4 V for l-Met (curve b).
On the other hand, the PtTiO2 /CNT/GCE modied GCE exhibits a
well-dened oxidation wave for l-Met at 1.1 (curve c).
A comparison of the cyclic voltammograms of l-Met at bare
GCE (curve b) and PtTiO2 /CNT/GCE (curve c) demonstrates the
oxidation peak potential of l-Met at PtTiO2 /CNT/GCE occurs at a
potential about 300 mV less positive than at a bare GCE (potential
shift from 1.4 V to 1.4 V). The obtained clear voltammetric signal

3.4. Effect of pH on l-Met oxidation

It well known, the electrochemical behavior of l-Met are dependent on the pH value of the aqueous solution [11,14]. The effect
of pH value on the electrooxidation of l-Met at the surface of
PtTiO2 /CNT/GCE was investigated through the use of different
0.1 M phosphate buffer solutions (pH 3.009.00). The current
response of l-Met at PtTiO2 /CNT/GCE increases from pH 3.00 to
7.00 and then a decrease is obtained at pH values higher than 7.00
(not shown). Therefore, pH 7.00 was chosen as optimum pH and
further studies were performed at pH 7.00.
3.5. Amperometric determination of l-Met
Amperometric method was used to examine the sensitivity
of PtTiO2 /CNT/GCE toward the detection of l-Met. Fig. 6 shows
the amperometric curve obtained for l-Met at PtTiO2 /CNT/GCE
in a constantly stirred 0.1 M PBS (pH 7.00). The dependence of
current response with respect to concentration of l-Met for 3
times experiments was average linear from 0.5 to 100 M with an

Table 1
Analytical parameters for voltammetric determination of l-Met at different modied electrodes.
Electrode

Potential shift (mV)

LDR (M)

LOD (M)

Reference

nAu-Cyst-CPEa
p-4-CuIITAPc-GCEb
CHNM/GCEc
Ni-CCEd
C60 /GEe
PtTiO2 /CNT/GCE

100

300

1100
50500
2451210
290

0.5100

0.59
0.027
160
2
8.2
0.1

[22]
[25]
[29]
[24]
[21]
This work

a
b
c
d
e

Colloidal-gold cysteamine-modied carbon paste electrode.

1,8,15,22-Tetraaminophthalocyanato-copper(II) modied glassy carbon electrode.
Cobalt hydroxide nanoparticles modied glassy carbon electrode.
Ni doped carbon ceramic electrode.
C60 modied gold electrode.

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F. Chekin et al. / Sensors and Actuators B 177 (2013) 898903

Table 2
Recovery test for l-Met in human blood serum samples.

recovery for l-Met in blood serum samples, indicating that the

present method may be used for practical applications.

Sample

Spiked (M)

Found
(M)

Mean recovery
(n = 3)

1
2
3
4

10.0
25.0
50.0
100.0

10.1
24.8
49.8
97.3

101.0
99.8
99.6
97.3

4
3
3
6

detection limit of 0.1 M at PtTiO2 /CNT/GCE, a high sensitivity of

29,085.66 A mM1 cm2 and an correlation coefcient of 0.991
(Fig. 6, inset).
The observed linear range and detection limit of l-Met were
compared with the reported papers and are given in Table 1
[21,22,24,25,30]. As can be seen from Table 1, the present modied
electrode shows better sensitivity than the other modied electrodes. Further, the present modied electrode was highly stable
and no tedious procedure was involved in electrode modication.
3.6. Reproducibility and stability of the PtTiO2 /CNT/GCE
The operational stability of PtTiO2 /CNT/GCE was tested by the
CV method every 2 days in 2 weeks. The response to 0.1 mM l-Met
decreased less than 12% after 2 weeks, so it has good stability. The
fabrication reproducibility of ve electrodes independently made,
showed a RSD of 6.1% for detecting 0.1 mM l-Met. The excellent
reproducibility and stability of PtTiO2 /CNT/GCE may be mainly
attributed to the strong deposition of the PtTiO2 /CNT.
3.7. Recovery test for l-Met in human blood serum samples
The practical application of PtTiO2 /CNT/GCE was tested by
measuring the concentration of l-Met in human blood serum samples. The human blood serum samples were collected from nearby
hospital. 1 mL of the serum sample was diluted to 10 mL of 0.1 M
PBS. The standard addition technique was used to examine the
recovery of l-Met in serum samples. The recovery results were
obtained and the results are summarized in Table 2. The proposed
method showed a good recovery for spiked l-Met in serum samples,
indicating that the present modied electrode could be applied to
determine l-Met in different human uids.
3.8. Interference study
Possible interferences for the detection of l-Met at the
PtTiO2 /CNT/GCE was investigated by the addition of various compounds such as glycine, alanine, ascorbic acid, dopamine, uric
acid, l-cysteine, glutathione, d-penicillamine, cystamine, N-acetyll-cysteine and lysine into pH 7.00 PBS in the presence of 1.0 mM
l-Met. The results showed that these mentioned compounds did
not show interference.
4. Conclusion
In summary, we demonstrated that Pt doped TiO2 nanoparticles can be readily formed by solgel method. The method is simple,
scalable and applicable to a variety of systems. The PtTiO2 has catalytic activity, making it an ideal candidate for sensor applications.
The present study demonstrates the sensitive determination of lMet using the PtTiO2 /CNT modied GCE. The bare GCE showed
an ill-dened oxidation wave for l-Met whereas the modied electrode not only showed a well-dened stable oxidation peak but
also enhanced its oxidation current. Further, using the amperometry method, a detection limit of 0.1 M (S/N = 3) was achieved
for determination of l-Met. The modied electrode showed good

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Biographies
Fereshteh Chekin received her Ph.D. degree in analytical chemistry from Mazandaran University under supervision of Prof. J.B. Raoof in 2010. She joined in Islamic
Azad University as a professor assistant in 2010. Her research interests include
electrochemistry, analytical chemistry, biosensors, nanobiosensors, nanocomposite
materials. Her current research is focused on synthesis of nano materials.
Samira Bagheri received her M.S. in physics (2010) from Iran University. She is now
a Ph.D. student in UM University. She joined in Prof. Sh.B. Abd Hamids group in
2011. Her research is focused on materials and electrochemistry.
Sharifah Bee Abd Hamid received her Ph.D. in chemistry (2011) from Lanzhou University. She joined in UM University as a professor in 1993. Her research is focused
on nanotechnology and catalysis.