Journal of Colloid and Interface Science 490 (2017) 444–451

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Journal of Colloid and Interface Science

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

Regular Article

Evaluation of Thymus vulgaris plant extract as an eco-friendly

corrosion inhibitor for stainless steel 304 in acidic solution by
means of electrochemical impedance spectroscopy, electrochemical
noise analysis and density functional theory
A. Ehsani a,⇑, M.G. Mahjani b, M. Hosseini b, R. Safari a, R. Moshrefi b, H. Mohammad Shiri c
a
Department of Chemistry, Faculty of Science, University of Qom, Qom, Iran
b
Faculty of Chemistry, K.N. Toosi University of Technology, Tehran, Iran
c
Department of Chemistry, Payame Noor University, Iran

g r a p h i c a l a b s t r a c t

a r t i c l e i n f o a b s t r a c t

Article history: Inhibition performance of Thymus vulgaris plant leaves extract (thyme) as environmentally friendly
Received 12 October 2016 (green) inhibitor for the corrosion protection of stainless steel (SS) type 304 in 1.0 mol L
1 HCl solution
Revised 10 November 2016 was studied by potentiodynamic polarization, electrochemical impedance (EIS) and electrochemical
Accepted 15 November 2016
noise measurements (EN) techniques. The EN data were analyzed with FFT technique to make the spec-
Available online 16 November 2016
tral power density plots. The calculations were performed by MATLAB 2014a software. Geometry opti-
mization and calculation of the structural and electronic properties of the molecular system of
Keywords:
inhibitor have been carried out using UB3LYP/6-311++G⁄⁄ level. Moreover, the results obtained from elec-
Green inhibitor
EIS
trochemical noise analysis were compared with potentiodynamic polarization and electrochemical impe-
EN dance spectroscopy. All of the used techniques showed positive effect of green inhibitor with increasing
Stainless steel inhibitor concentration.
Corrosion Ó 2016 Elsevier Inc. All rights reserved.

1. Introduction

Acidic solutions are widely used in industrial processing such

⇑ Corresponding author. as acid pickling, cooling systems, chemical and electrochemical
E-mail address: ehsani46847@yahoo.com (A. Ehsani).

http://dx.doi.org/10.1016/j.jcis.2016.11.048
0021-9797/Ó 2016 Elsevier Inc. All rights reserved.
 A. Ehsani et al. / Journal of Colloid and Interface Science 490 (2017) 444–451
etching, and oil well acidizing [1–4]. Among anticorrosion methods
for protection of stainless steel, corrosion inhibitors due to their
easy application, reasonable cost and their sufficient efficiency
are attracted great attention recently. Inhibitors are chemical sub-
stances which added to a corrosive environment in small concen-
trations. Most of the inhibitors have toxicity compounds that due
to the adverse effects on the environment and human is faced with
a ban on the use of inorganic inhibitors. The safety and environ-
mental issues of corrosion inhibitors arisen in industries has
always been a global concern [5]. Lately researchers have paid
attention to the development of organic and environmentally
friendly inhibitors [3,4,5–9]. Most organic compounds contain
nitrogen, sulfur, oxygen and P-band [10]. These structures with
polar groups can act as active centers that play an important role
in the absorption of the inhibitor on the metal surface [11,12].
There are lots reports on the use of plant extracts as green inhibi-
tors of metals in acid solution [13–18]. The inhibition characteris-
tics of green inhibitors investigated such as Watermelon rind, seed
and peel (WMPE) [14], Curcuma longa extract [16], Aloe Vera leaf
extract [17], Cucumis sativus peel extract [18], Salvia hispanica
[19], Nonetheless, there is still a need for research on other plants
that can be used as inhibitors in industrial applications. There are
reports on the use of Thymus vulgaris (TV) plant extract for corro-
sion protection for different metals in various acid solutions
[20,21]. For example, the protection of copper and a-brass in
HNO3 solution by Thymus vulgaris plant extract based on weight
loss and electrochemical techniques have been reported by Fouda
et al. [22]. Results indicate that inhibition efficiency has increased
with an increase in extract concentration and decrease with an
increase in temperature. Similarly, El Hajjaji et al. [23] have inves-
tigated the effect of the oil of T. vulgaris on mild steel in HCl. The
results obtained reveal that oil reduces the corrosion rate. Ibrahim
et al. [24] showed that Thyme leaves extract have had a good cor-
rosion inhibitor for mild steel in HCl. According to the results,
Thyme leaves extract acted as a mixed type inhibitor on the metal
surface. The electrochemical noise is one of the modern electro-
Fig. 1. Energies (in a.u.) of the occupied/virtual molecular orbitals of the inhibitor molecular system calculated at DFT-UB3LYP/6-311G⁄⁄++ level of theory.
445
chemical techniques [25,26] that has gained popularity in the
recent decades and has emerged as a promising technique for cor-
rosion studies [27]. Electrochemical noise technique is indeed the
spontaneous fluctuations of potential and current with time.
Potential and current measured simultaneously without applying
external perturbation. In this technique two nominally identical
electrodes are connected galvanically through a zero resistance
ammeter (ZRA). The current between two electrodes is measured
by ZRA. Moreover two electrodes, due to short circuit connection
between them, sense similar potential and their potential is mea-
sured toward a standard reference electrode or a third identical
electrode.
Different mathematical approaches have been used for electro-
chemical noise analysis. Among other methods statistical and spec-
tral methods are the most popular approaches in electrochemical
noise analysis [28–30]. Specific parameters such as potential, cur-
rent mean and noise resistance have defined for electrochemical
noise time series characterization. For example determination
and tracing of mean potential and current values can provide use-
ful information about thermodynamics and kinetic of corrosion
process, respectively. The noise resistance, Rn, is another important
parameter that has a physical concept like polarization resistance
and is calculated by division of standard variation of potential on
standard variation of current. It is obtained that noise resistance
variable can be comparable with polarization resistance (Rp) calcu-
lated by linear polarization and electrochemical impedance spec-
troscopy (EIS). The power density spectrums (PSD) are
appreciated curve that used frequently in spectral analysis of elec-
trochemical noise methods. In spectral methods, Time domain
potential and current noise is transferred to frequency domain.
The first and crucial step before noise spectral analysis is data pre-
treatment. In most electrochemical noise measurements is
appeared a DC drift in potential or current noise data, that the
more strong drift is observed in the corrosion potential. The pro-
cess of removing DC trend is called trend removal and its process
is necessary prior to statistical and spectral analysis [28,31].
446 A. Ehsani et al. / Journal of Colloid and Interface Science 490 (2017) 444–451
In this work, inhibition effect of Thymus vulgaris (TV) plant
extract as green inhibitor on corrosion of SS type 304 in 1.0 mol L
1
HCl solution was studied. Electrochemical impedance spectroscopy
(EIS), electrochemical noise measurements (EN) and potentiody-
namic polarization techniques were employed to investigate the
effect of inhibitor concentration on corrosion process. Geometry
optimization and calculation of the structural and electronic prop-
erties of the molecular system of the plant extract (Ph-OH-CH3-
C3H7) have been carried out using UB3LYP/6-311++G⁄⁄ level.
2. Experimental
2.1. Materials
The employed working electrodes were prepared from stainless
steel 304 with composition of Fe, rest; Ni, 10; Cr, 18.5; Mn, 1.8; Si,
0.75; C, 0.08; S, 0.03 and P, 0.04 (wt%). The electrolyte was
1.0 mol L
1 HCl solution, which was prepared from Merck reagents
and distilled water at ambient temperature. Green inhibitor extract
were obtained from the Thymus vulgaris plant and used without
any further purification.
2.2. Methods
Electrochemical noise, electrochemical impedance spec-
troscopy and polarization measurements were used to evaluate
the corrosion behavior of 304 stainless steel in 1.0 mol L
1 HCl
solution in the absence and presence of green corrosion inhibitor
(Thyme vulgaris plant) at different concentrations. The specimens
were connected to a copper wire at one end, and mounted by
epoxy resin with the other end exposed as the WE surface for test.
Before carry out experiments, the WE surface was polished by wet
sanding sheets through 400–1200 grade, cleaned with distilled
water, and degreased with acetone prior to every run. Noise mea-
surements were carried out by electrochemical interface model
1287 solarton for 2 h. Two nominally identical working electrodes
were facing each other vertically in solution at a distance of about
1 cm. The cell was placed in a Faraday cage due to avoid interfer-
ences with external electromagnetic field and stray currents in
during EN measurements. The EIS and potentiodynamic polariza-
tion tests were performed by the potentiostat/galvanostat model
273 A EG&G and SI (HF frequency response analyzer). Standard
Fig. 2. The HOMO (a) and LUMO (b) molecular orbital diagrams of the inhibitor molecular system, calculated at DFT-UB3LYP/6-311G⁄⁄++ level of theory.
electrochemical cell with three electrodes was used for electro-
chemical impedance spectroscopy (EIS) and potentiodynamic
polarization. A SS 304, a graphite rod and Ag/AgCl electrode were
used as working, counter and reference electrode respectively.
Electrochemical experiments sequence of steps was EN, EIS and
polarization measurement. The latter two techniques needed CE
for the tests. Before measures, to achieve steady state, the samples
were immersed for 30 min in their own solutions.
Electrochemical potential and current noise were obtained with
10 Hz sampling frequency. The EN data were analyzed with FFT
technique to make the spectral power density plots. The calcula-
tions were performed by MATLAB 2014a software. EIS measure-
ments were carried out after 30 min of immersion in a solution
of the open circuit potential in the frequency range of 100 kHz–
10 mHz and Nyquist and bode plots data were analyzed by ZView
software. Polarization measurements were performed immedi-
ately after the EIS and were recorded at a scan rate of 10 mV/s.
Power Suite software was used to measure the corrosion current
density and polarization parameters.
3. Results and discussion
3.1. Computational details
Geometry optimization and calculation of the structural and
electronic properties of the molecular system of the plant extract
(Ph-OH-CH3-C3H7) have been carried out using UB3LYP/6-311+
+G⁄⁄ level, Figs. 1 and 2. In addition, starting from the electronic
wave functions, the atomic basins are determined, using density
gradient method and atoms-in-molecule (AIM) theory [32,33].
Also, to local/atomic study molecular/intramolecular charge/
energy transfer mechanism, the details of the contour maps of
the electron density (q(r)) and its Laplacian (r2q(r)), correspond-
ing to atomic electronic kinetic energy and molecular virial forces
(V(r)), in the molecular planes are calculated and plotted in Fig. 3.
Moreover, molecular vibrational frequencies (as IR spectra)
obtained based on harmonic oscillation (HO) approximation for
the optimized structures, Fig. 4. It clears that both electronic and
vibrational properties/characteristics (such as he variations of elec-
tron density, bonding characteristics and atomic displacements)
play the dominant role in the molecular/intramolecular charge/
energy transfer.
 A. Ehsani et al. / Journal of Colloid and Interface Science 490 (2017) 444–451
Fig. 3. The contour maps ((topology of the electronic properties)) of the local electron density (a), Laplacian of electron density (b), electronic kinetic energy (c), and virial
force (d), of the inhibitor molecular system, calculated using AIM theory.
3.2. Potentiodynamic polarization
Fig. 5 shows Tafel curves of SS 304 in 1.0 mol L
1 HCl solution in
the absence and presence of varies concentrations of TV plant
extract. Polarization measurements provide valuable information
about the kinetics of anodic and cathodic reactions. The potentio-
dynamic polarization parameters such as the corrosion rate (CRate),
anodic and cathodic Tafel slopes (ba, bc), corrosion current density
(Icorr), corrosion potential (Ecorr) and polarization resistance (Rp) are
listed in Table 1. These results present that with increasing concen-
tration of TV plant, the corrosion current density decreased. There
is no remarkable shift in corrosion potential (Ecorr) values with
increasing inhibitor concentration. The form of these curves is very
similar either in the cathodic and anodic branches which can sug-
gest that the mechanisms of SS304 electrochemical reactions prob-
ably remain invariant in the present of green inhibitor. The
changes in Tafel slopes confirmed the effect of TV extract on the
both cathodic and anodic reactions. Therefore, the TV plant
447
behaved mixed-type inhibitor. Values of the corrosion inhibition
efficiency (IE) were presented in Table 1 was Obtained as [11]:
Iblank
Iinhibitor
IE ¼  100 ð1Þ
Iblank
where Iblank and Iinhibitor are corrosion current densities in absent and
present of inhibitor, respectively. The IE values shows that the inhibi-
tion is more pronounced with increasing in inhibitor concentration.
3.3. Electrochemical impedance spectroscopy
Electrochemical impedance spectroscopy (EIS) is one of the best
techniques to analyze the properties of the electrochemical sys-
tems [34–40]. The Nyquist plots of EIS are shown in Fig. 6 for SS
304 in 1.0 mol L
1 HCl solution in the absence and presence of var-
ious concentrations of TV plant extract. Fig. 6 shows the electrical
equivalent circuit relevant to analyze the impedance plots. In the
presented equivalent circuit, Rs is the solution resistance and Rct
448 A. Ehsani et al. / Journal of Colloid and Interface Science 490 (2017) 444–451

Fig. 4. The IR spectra of the inhibitor molecular system, calculated at DFT-UB3LYP/6-311G⁄⁄++ level of theory.

[41–48]. The impedance of the constant phase element is defined

as follows:
1
Z CPE ¼ n ð2Þ
Y 0 ðjwÞ
where Y0 is the CPE constant (F cm
2 Sn
1 or snX
1 cm
2), j equals
pffiffiffiffiffiffiffi

1, x is the angular frequency and n is the CPE exponent.
Depending on n, CPE can represent resistance (n = 0, ZCPE = R),
capacitance (n = 1, ZCPE = C), inductive (n = 1, ZCPE = L) or Warburg
impedance (n = 0.5, ZCPE = W). The correct equation to convert the
CPE constant, Y0, into the double layer capacitance, Cdl, is the fol-
lowing equation:

C dl ¼ Y 0 ðxmax Þn
1 ð3Þ

Fig. 5. Polarization curves for SS 304 in 1 M HCl solution in different volume
percent of the inhibitor (0.25–2%).
is the charge transfer resistance. The ideal capacitive behavior is
not observed in this case and hence a constant phase element
(CPE) is introduced in the circuit to give a more accurate fit
where xmax is the angular frequency at which the imaginary com-
ponent of the impedance is maximum. Inhibition efficiencies in
Table 2 were calculated through the following expression:
 
Rin
Rb
IEð%Þ ¼ 100 ð4Þ
Rin
where Rb and Rin represent the charge transfer resistance, before
and after addition of the inhibitor to the corrosion environment,
respectively. As can be seen, Nyquist diagrams have an approxi-
mately semicircular appearance that present the corrosion of SS
304 is controlled by a charge transfer process. As it can be seen
from Table 2, the Rct values increased with increasing of inhibitor

Table 1
Polarization parameters of 304SS in 1.0 mol L
1 HCl solution.

Sample Ecor (mV) Icorr CR (mpy) Tafel slop (mV decade
1) RP IE (%)
(lA cm
2) (kX)
ba bc
Blank
262.04 4.00 8.20 59.30 101.20 4.60 –
0.25%
232.97 2.60 5.30 57.00 104.17 7.77 35.0
0.5%
221.77 2.53 5.15 60.00 115.88 7.90 36.8
1%
228.57 2.44 4.97 55.17 104.86 10.75 39.0
1.5%
230.13 2.36 4.82 45.36 128.17 14.50 41.0
2%
223.07 2.04 4.17 52.96 120.80 21.13 49.0
 A. Ehsani et al. / Journal of Colloid and Interface Science 490 (2017) 444–451 449

with adsorbed inhibitors on the metal surface. As a result, the 304

SS surface protected of acid solution attack [11].

3.4. Electrochemical noise measurements

The obtained potential and current for SS304 electrodes in

1 mol L
1 HCl in the absence and presence of different values of
inhibitor are shown in Fig. 7. The EN signals record during
120 min after an immersion time 30 min. Useful information can
be obtained by visual examination of time records. The EN signals
current time records in absence of inhibitor are in order of 10
5
and in present of inhibitor, in low concentration in order of 10
6
and in high concentration are in order of 10
7 that indicated to a
decrease in current values with increasing of inhibitor concentra-
tion. The statistical analysis of EN data are listed in Table 3. As
can be seen from Fig. 7 the potential and current are oscillated ape-
riodic. The mean values of potential are shifted toward more pos-
itive values with increasing inhibitor concentration, and numbers
Fig. 6. Nyquist plots and equivalent circuit for 304SS in 1 mol L
1 HCl solution in
of birth-death transient are increased. The birth-death transients
absence and presence of different concentration of TV plant at 25 °C.
that can be seen as a sudden increase and decrease in current val-
ues, are attributed to activation controlled process such as meta-
stable pitting. Rn values was increased with increasing of
Table 2
Impedance parameters for 304 SS in 1.0 mol L
1 HCl solution in absence and presence inhibitor concentration. The trend of gn values are in good agree-
of different concentration of T.V plant at 25 °C. ment with g obtained from the polarization method and electro-
chemical impedance spectroscopy. The EN data is also analyzed
Sample RS C  105 n1 Rct IE (%)
(X cm2) (F cm
2) (X cm2) in frequency domain by computing the power spectral density
(PSD). Different methods are used for transforming the time
Blank 1.25 8.40 0.89 2195 –
0.25% 2.87 4.16 0.90 3564 38.40 domain information to a frequency domain, however the fast Four-
0.5% 3.10 4.68 0.92 5200 57.70 ier transformation (FFT) algorithm is applied to obtained PSD plots
1% 1.37 4.48 0.90 5325 58.70 in this study. In this order, for avoiding the integration effect in FFT
1.5% 1.67 2.56 0.89 5337 58.90 method, some extra preparation is needed. In the literatures, Hann
2% 5.12 4.60 0.91 5800 62.15
window with linear de-trending is mostly recommended for pre-
processing of data before transferring them from time domain to
concentration. On the other hand, the Cdl values don’t follow a frequency domain. Fig. 8 shows typical spectral noise resistance
specific trend with increasing the inhibitor concentration. Inhibition plots which are obtained by transformation of trend removed noise
efficiencies increased with increasing the concentration of inhibitor. records. As can be seen, the bode diagrams and PSD diagrams can
The IE values are in good agreement with IE obtained from the be compared to each other, although there is not a clear relation
polarization method. This situation was the result of increasing sur- between them due to the noise of PSD diagrams. In lower fre-
face coverage by the inhibitor and inconsequence a decrease in local quency region, PSD diagrams have lower noise magnitude and they
dielectric constant due to the increase in the thickness of double converge to EIS results that indicate noise technique can provide
layer. This can be attributed to the water molecules replacement useful information especially in lower frequency region.

Fig. 7. EN potential and current records of SS304 in 1.0 mol L
1 HCl solution in absence and presence of different concentrations of T.V plant.
450 A. Ehsani et al. / Journal of Colloid and Interface Science 490 (2017) 444–451

Table 3
Statistical parameters for 304 SS in 1.0 mol L
1 HCl solution.

Inhibitor Emean (mV vs Ag/AgCl) Imean (lA cm
2) rv (mV) rI (lA cm
2) Rn (kX cm2)
Blank 1.00 228.00 46.00 30.80 0.15
0.25% 2.84 3.23 8.86 14.76 0.60
0.5% 3.02 3.84 5.70 13.40 0.43
1% 3.04 1.72 5.92 0.98 6.00
1.5% 3.30 3.52 6.07 0.60 10.17
2% 3.50 1.20 0.98 0.05 20.50

Fig. 8. Comparison between PSD (R) plots and bode diagrams for SS304 with applied Hann windowing in absence and presence of different concentrations of TV plant.

4. Conclusion corrosion inhibition mechanism. A good correlation was observed

The inhibition effects of Thymus vulgaris plant extract on corro-
sion behavior of stainless steel type-304 alloy in 1 mol L
1 HCl
were studied using electrochemical techniques. Inhibition effi-
ciency increases with increasing inhibitor concentration. Tafel results
indicate that Thymus vulgaris plant extract exhibit mixed-type
between the potentiodynamic studies and electrochemical impe-
dance spectroscopy with electrochemical noise measurements.
Hence, it seems that the EN method can be applied as a comple-
mentary quantitative technique to study the corrosion behavior
of inhibitors. Moreover EIS plots indicate the charge transfer resis-
tance increase with increasing concentration of the inhibitor.
 A. Ehsani et al. / Journal of Colloid and Interface Science 490 (2017) 444–451 451

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