Surfaces and Interfaces 20 (2020) 100595

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Surfaces and Interfaces

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Portulaca grandiflora as new green corrosion inhibitor for mild steel T

protection in hydrochloric acid: Quantitative, electrochemical, surface and
spectroscopic investigations
Ahmed A. Fadhila,b, Anees A. Khadomb,*, Salima K. Ahmedc, Hongfang Liua,*, Chaoyang Fua,*,
Hameed B. Mahoodd
a
Key laboratory of Material Chemistry for Energy Conversion and Storage (Ministry of Education), Hubei Key Laboratory of Material Chemistry and Service Failure, School
of Chemistry and Chemical Engineering, Huazhong University of Science and Technology (HUST), 1037 Luoyu Road, Wuhan 430074, PR China.
b
Department of Chemical Engineering, College of Engineering, University of Diyala, Baquba City 32001, Diyala governorate, Iraq
c
Department of Chemistry, College of Science, University of Diyala, Baquba City 32001, Diyala governorate, Iraq
d
Department of Chemical and Process Engineering, Faculty of Engineering and Physical Sciences, University of Surrey, Guildford GU2 7XH, UK.

A R T I C LE I N FO A B S T R A C T

Keywords: The inhibition action of the Portulaca grandiflora leaf (PGL) extract against corrosion on N80 carbon steel was
Corrosion tested under 0.5 M HCl acidic conditions at variable temperatures and inhibitor concentrations. The performance
Green inhibitor behaviour of PGL was evaluated by weight loss and electrochemical techniques including polarisation mea-
Acid surement, open circuit potential, and electrochemical impedance spectroscopy. The analysis results of Fourier
Electrochemical measurement
transform infrared spectroscopy, ultraviolet spectra, and surface morphology strongly support the corrosion
SEM
FTIR
rates results. The obtained outcomes show that the inhibitor can effectively inhibit the corrosion of carbon steel
in acidic media with a maximum inhibition efficiency of 95% at high levels of temperature (60 °C) and inhibitor
concentration (20 mL/L). The adsorption of PGL on the steel surface followed that according to the Langmuir
isotherm model. The heat of adsorption values increased from -17.71 kJ mol-1 to -22.03 kJ mol-1 as the tem-
perature increased from 30 to 60°C suggests a mixed-mode of adsorption on the metal surface.

1. Introduction possible alternatives to synthetic materials, many studies have been

Since the Industrial Revolution, the environmental degradation of
metals and alloys has been a serious problem worldwide, affecting the
economy of the industrial sector as well as infrastructure and archi-
tecture as well as ancient and modern art. Exposure to corrosive en-
vironments (e.g. acidic and alkaline solutions) and interaction with
oxidative environments result in degradation of metallic materials,
whereby the metal returns to its ore form. Generally, corrosion sup-
pression in metals can be accomplished by using different techniques
e.g. anti-corrosion coatings [1], the application of corrosion inhibitors
[2], and cathodic protection [3]. However, the use of these techniques
on a commercial scale creates ecological toxins and risk to human
health [4,5]. Therefore, significant research has been conducted on eco-
friendly anticorrosion agents over the past few decades with a focus on
environmental protection. In this regard, special attention has been
paid to the use of natural compounds, particularly extracts with anti-
oxidant properties to protect various alloys and metals. To develop
conducted in the field of ‘green’ corrosion inhibition because such
techniques are eco-friendly, inexpensive, non-toxic, easily formulated,
and renewable [6–9]. Extracts of plants have shown significant in-
hibitive action [10] and pose limited or no negative ecological hazards
[11]. Many previous works have demonstrated the suitability of plant
extracts for use as corrosion inhibitors on steel in HCl. For example,
Ficus tikoua leaf extract has shown an efficiency of 95.8% for carbon
steel [12], and bitter kola leaf extract has an efficiency of 90% [13].
Moreover, the leaf extracts of Glycyrrhiza glabra and Xanthium stru-
marium and the juices of peaches and kiwis have demonstrated effi-
ciencies of 88% [14], 94.8% [15], 91% [16], and 96.1% [17], respec-
tively, against corrosion. These anticorrosion materials are extracted
from plants and usually contain polar functional groups such as NH2,
CHO, and carbonyl groups or heteroatoms such as N2, O2, P, and S,
which are considered to be highly effective corrosion inhibitors
[18–20].
Bidi et al., [21] studied the effect of Hyalomma tick extract as a new

E-mail addresses: aneesdr@gmail.com (A.A. Khadom), liuhf@hust.edu.cn (H. Liu), cyfu@hust.edu.cn (C. Fu).
⁎
Corresponding authors.

https://doi.org/10.1016/j.surfin.2020.100595
Received 8 April 2020; Received in revised form 18 June 2020; Accepted 2 July 2020
Available online 24 July 2020
2468-0230/ © 2020 Elsevier B.V. All rights reserved.
A.A. Fadhil, et al.
green corrosion inhibitor for carbon steel in 1 M HCl solution. Corrosion
kinetic parameters were evaluated using polarization and electro-
chemical impedance spectroscopy (EIS) methods. It was found that
maximum inhibition efficiency was 95% at an inhibitor concentration
of 3 g/L. Hyalomma tick extract adsorption on the steel surface acted as
a mixed inhibitor following Langmuir adsorption isotherm. Berrissoul
et al. [22] investigated the corrosion inhibition of mild steel in hy-
drochloric acid solution by Lavandula mairei Humbert extract as an
eco-friendly inhibitor. The corrosion inhibition efficiency increased
with the increase of Lavandula mairei Humbert extract concentration
up to 92% obtained at 303 K for a 0.4 g/ L concentration. Fouda et al.
[23] investigated the effectiveness of Tilia cordata extract as a green
corrosion inhibitor for carbon steel in 1 M HCl. The results showed that
Tilia cordata has corrosion inhibition efficiency of 96% at 300 mg L−1.
Charge transfer resistance increases while both the capacitance of the
double layer and corrosion current values decrease with increasing the
extract concentration. Pitchaipillai et al. [24] studied the ethanolic
extract of Kleinia grandiflora leaves as a corrosion inhibitor for mild
steel in acidic medium using mass-loss analysis, potentiodynamic po-
larization measurements, EIS, FTIR, SEM, UV, and XRD analysis. The
inhibition efficiency was observed to increase with increasing con-
centration of the extract. The results indicate that the Kleinia grand-
iflora leaf extract can serve as an effective inhibitor for the corrosion of
mild steel in an acidic medium. Satapathy et. al., [25] investigated the
effect of different concentrations of Justicia gendarussa extract as a
corrosion inhibitor for mild steel in 1 M HCl medium. The maximum
percentage inhibition was 93% at 150 ppm inhibitor concentration and
25°C. Furthermore, Justicia gendarussa extract obeys the Langmuir
adsorption isotherm.
Portulaca grandiflora, commonly known as moss rose, rose moss, or
sun plant, is a small, herbaceous annual plant that belongs to the
Portulacaceae family. It is widespread and may contain complex or-
ganic materials such as phenols, ascorbic acid, and gallic acid [26]. It is
a very common, available and priceless plant in Diyala governorate/
Iraq. In the present work, P. grandiflora leaf (PGL) was first extract and
evaluated as a corrosion inhibitor for mild steel in HCl. Gravimetric
measurements and electrochemical analysis are used to estimate the
performance of the inhibitor. In addition, adsorption of PGL on a steel
surface is investigated using atomic force microscopy (AFM), Fourier
transform infrared (FTIR) spectroscopy, and scanning electron micro-
scopy (SEM).
2. Experimental
2.1. Materials
The following components of the N80 steel along with their weight
percentages were used in the present work: C, 0.16; Mn, 0.397; Si, 1.59;
Al, 0.005; P, 0.005; S, 0.014; Cu, 0.022; Cr, 0.202; Ni, 0.12; and Mo,
0.087. Prior to experimentation, the steel electrode was thoroughly
cleaned with grade 800–1500 sandpaper; washed ultrasonically with
deionised water, acetone, and ethanol; and dried. In addition, 37% HCl
supplied by Sigma Aldrich and ultrapure water were used to prepare a
0.5 M HCl solution that acted as a corrosive environment. The corrosion
rate of N80 steel was evaluated in the presence and absence of PGL as a
corrosion inhibitor at different temperatures of 30, 40, 50, and 60°C and
inhibitor concentrations of 0, 5, 10, 15, and 20 mL/L. All of the ex-
periments were performed in triplicate, and the average value was
taken to ensure the maximum reproducibility of the results.
2.2. Preparation of inhibitor
Fresh PGL samples were collected from different areas of Diyala
Province in Iraq, and were cleaned first with tap water and then with
distilled water to remove any remaining waste products or mud. The
PGL was dried for 72 h in a desiccator at 60°C and was then ground to
2
Surfaces and Interfaces 20 (2020) 100595
powder. Afterwards, 150 g of powdered PGL was refluxed with ethanol
at 65°C for 24 h. The refluxed products were then filtered, and the
filtered solution was stored in a desiccator until the time of use. The
PGL was added at amounts of 5, 10, 15, and 20 mL for each litre of 1 M
HCl.
2.3. Electrochemical measurement
Electrochemical measurements were conducted using a CHI760E
electrochemical workstation in a conventional three-electrode corro-
sion cell. The counter and working electrodes were composed of Pt and
N80 steel, respectively. A saturated calomel electrode (SCE) was used as
a reference electrode. PGL at concentrations of 0, 5, 10, 15, and 20 mL/
L was added to the 0.5 M HCl corrosive solution. The N80 steel speci-
mens were coated with epoxy resin, leaving a working surface area of
0.8 cm2. Against the SCE, the electrode potential was measured, and the
polarisation curves were recorded at a scanning rate of 1 mV/s with
various potentials from the detected open circuit potential (OCP), fol-
lowing 1200 s of immersion. The anodic and cathodic curves of the
linear Tafel region were extrapolated to the corrosion potential to
achieve the corrosion current densities. The polarisation was evaluated
from the lower cathodic potential of -800 mV to the anodic potential of
200 mV. Electrochemical impedance spectroscopy (EIS) assessment was
conducted at a frequency range 100 kHz–0. 01 Hz with a single am-
plitude perturbation of 5 mV at OCP with the scan rate of 1 mV/s. The
polarisation map was further analysed by using software, and the im-
pedance estimation was determined by using ZSimpWin data analysis
software. All the experiments were performed at temperatures of 30,
40, 50, and 60°C.
2.4. Weight loss measurement
Rectangular test samples of N80 steel 50 mm × 10 mm × 3 mm in
length, width, and thickness, respectively (Tangshan Xincheng Iron and
Steel Co., Ltd., China), were used with the same chemical composition
as that mentioned in Section 2.1. The samples were cleaned with tap
water, rinsed with distilled water, and dried with a clean tissue. Then,
they were immersed in alcohol and acetone, dried again with a clean
tissue, and stored in a desiccator on a bed of silica gel until the time of
use. The sample size was measured to an uncertainty of 0.01 mm by
using electronic Veriner calipers and was weighed using an electronic
balance with uncertainty of 0.0001 g. The steel samples were fully
immersed in 500 mL of a 0.5 M HCl solution with and without the
inhibitor. The samples were immersed under specific conditions of in-
hibitor concentration and temperature for 24 h. After each test, the
corrosion products were removed, and the steel samples were cleaned
as described above. The corrosion rates [gm m−2 day−1 (gmd)] were
determined in the presence and absence of PGL.
2.5. Surface morphology diagnosis measurement
The morphology of the N80 steel surface was observed using an
SEM instrument (SU 8010, Hitachi, Japan) and an atomic force mi-
croscope (SPM 9700, Shimadzu, Japan). The morphology measurement
was conducted before and after immersing the N80 steel specimens in
0.5 M HCl solution without and with PGL for 24 h under minimum and
maximum conditions (i.e. 30°C, 5 mL and 60°C, 20 mL, respectively).
FTIR spectroscopy was performed using pure PGL and PGL adsorbed
on the N80 steel specimens. The PGL inhibitor was mixed with KBr
powder and was then transferred onto a pallet for FTIR characterisation
using a spectrometer (Vertex 70, Bruker, Japan) with 400–4000 cm−1
wave numbers.
The UV spectra were obtained for 20 mL/L PGL in 0.5 M HCl using a
spectrophotometer (UV-1800, UV–vis, Shimadzu, Japan). The spectra
were recorded in two different cases: 1) using inhibited acidic solution
before immersion of the N80 steel specimens and 2) after immersion of
A.A. Fadhil, et al.
Fig. 1. OCP–time curves for N80 steel in 0.5 M HCl solution without and with different concentrations of PGL at different temperatures.
the specimens for 24 h at 30°C.
3. Results and discussion
3.1. Open circuit potential results
The variation in OCP, that is, the potential generated on N80 steel
electrodes in 0.5 M HCl versus standard calomel electrode (SCE) po-
tential, with time (1200 s) for the PGL is shown in Fig. 1 A–D. The open
circuit potential (EOCP) against the time curves were approximately
linear with and without PGL which indicates a stable steady state po-
tential in both cases. However, the EOCP in the presence of the inhibitor
moved in a negative direction, which specifies complete dissolution and
surface removal of the oxide layer and the adsorption of inhibitor
molecules on the surface of the steel [27, 28].
3.2. Polarisation results
Fig. 2 A–D shows polarisation diagrams of the steel in the inhibited
and uninhibited 0.5 M HCl solutions at various levels of PGL content
and temperature. The current density of the metal was significantly
reduced in the presence of PGL. The polarisation parameters in the
presence and absence of PGL are listed in Table 1. As shown in Fig. 2
and Table 2, the PGL molecules pushed the current density towards
lower values without affecting the general behaviour of the Tafel lines,
which indicates the blocking of active sites on metal surfaces by PGL
molecules and hence retardation of steel corrosion [29]. The active site
blocking might be attributed due to PGL adsorption via their electron
rich adsorption centres. The polarisation curves show that in the in-
hibited solutions, the values of both the anodic and cathodic Tafel
slopes were affected by the presence of PGL as compared with the case
3
Surfaces and Interfaces 20 (2020) 100595
of the inhibitor-free solution. This indicates that the PGL essentially
behaved as mixed-type inhibitors. Furthermore, the shape of anodic
curves revealed that some compounds were formed at the metal sur-
face, which may be attributed to the formation of component-iron (II)
complex on the steel surface [30]. Another important criterion is a shift
in the corrosion potential (Ecorr), which that gives important informa-
tion about the type of inhibitor. A value higher than −85 mV indicates
that the inhibitor has a certain inhibitive behaviour for either anodic or
cathodic reactions. In the present case, a shift of less than −85 mV was
observed, which suggests that PGL can be distinct as a mixed-type [31].
That is, the PGL molecules were adsorbed in both the anodic and
cathodic sites, which reduced the main anodic reaction of the steel
dissolution, and the cathodic reaction in acidic media (O2 reduction and
evolution of H2). These results agreed with the work of Cao [32]; the
blocking of active sites on a metal surface or electro-catalytic effect of
the inhibitor or its reaction products accompany with corrosion po-
tential change.
The value of inhibition efficiency according to the polarisation
measurements (%IEP) listed in Table 1 can be determined by using Eq.
(1):
iocorr − i corr
%IEP = × 100
iocorr (1)
o
where 1icorr and icorr represent the corrosion current densities in ab-
sence and presence of PGL, respectively. The inhibition efficiency in-
creased with an increase in the PGL concentration owing to an increase
in the steel surface coverage by the adsorption of the PGL.
3.3. Electrochemical impedance spectroscopy
Analysis based on EIS provides significant information on the
A.A. Fadhil, et al.
Fig. 2. Polarization curves for N80 steel in 0.5 M HCl solution without and with different concentrations of PGL at different temperatures.
properties of the steel surface and the electrode kinetics processes. In
this study, EIS for steel in inhibited and uninhibited acid (0.5 M HCl)
was performed under different conditions; the results for the examined
PGL are shown in the Nyquist diagram at in Fig. 2A–D. The impedance
curves were similar and displayed a single semicircle at high frequency.
Corrosion process due to charge transfer can be predicated from pre-
sence of capacitive loop with high frequency [33]. As the PGL con-
centration increased, the semicircle diameter also increased, which
indicates high inhibition performance of the PGL. Electrochemical
Workstation software (CHI760E) was used for estimating the R (QR)
equivalent circuit, as shown in Fig. 5. In this equivalent circuit, Rs and
Rct represent the solution resistance and the resistance of charge
transfer, respectively. The non-ideal capacitor or constant phase ele-
ment (CPE) of the steel–solution interface can be obtained from Q and n
(exponential coefficient). The double layer commonly behaves as a CPE
rather than a pure capacitor. CPE is substituted for the capacitor to fit
the semicircle for precision. The admittance and impedance of the CPE
are shown in Eqs. (2) and (3), respectively:
YCEP = Yo (jω)n ,
1 cording to Eq. (5) [38]:
ZCPE = ,
Yo (jω)n
where j represents the imaginary root, ɷ represents the angular fre-
quency, Yo represents the extent of the CPE, and n is the deviation
parameter with regard to the phase shift signifying the microscopic
oscillation of the steel surface. The CPE can be an inductor for n equal
to −1, resistor for n equal to zero, Warburg impedance for n equal to
Surfaces and Interfaces 20 (2020) 100595
0.5, or capacitor for n equal to 1 [34]. The impedance increased and the
admittance decreased upon an increase in the inhibitor concentration,
as represented by Eqs. (2) and (3). Table 2 shows the parameters of
impedance values resulting from the equivalent circuits, which fit the
experimental data. Furthermore, the results in Table 2 specify that the
Rct values increase with an increase in the PGL concentration; the re-
verse was detected for CPE. Such results are usually attributed to the
growth in the thickness of the PGL molecular layer on the steel surface
[35]. These findings agree with the results of the polarisation in-
vestigations. Eq. (4) can be used to evaluate the double-layer capaci-
tance (Cdl) [36]:
Cdl = Yo (ωmax )n − 1, (4)
where ɷmax = 2πfmax and fmax are the maximum frequency value of the
impedance spectrum imaginary component. At each temperature, Cdl
decreased in the presence of PGL, which can be attributed to the con-
sistent replacement of H2O molecules by the adsorbed molecules of PGL
on the interface of the metal and the solution [37]. Addition of the
inhibitor increases the amount of adsorbed molecules and the protec-
(2)
tive layer thickness, which leads to decreases in the Cdl values, ac-
(3) ε ε0 A
Cdl = ,
d (5)
where A is the electrode effective surface area, d is the protection film
thickness, ɛo is the vacuum permittivity, and ɛ is the corrosive solution
dielectric constant.
The PGL efficiency according to EIS measurement (IEI%) can be
4
A.A. Fadhil, et al. Surfaces and Interfaces 20 (2020) 100595

Fig. 3. Nyquist plots for N80 steel in 0.5M HCl solution without and with different concentrations of PTT at different temperatures.

Table 1
Electrochemical parameters from polarization measurements for steel in 0.5 M
HCl acid at different conditions.
C (mL/L) T (°C) Icorr (mA/ Ecorr βa (mVdec−1) -βc (mVdec−1) %IEP
cm2) (mV)

Blank 30 6.48 -485 173.4 148.2 -

5 0.83 -480 129.2 122.6 87.1
10 0.56 -492 96.8 121.2 91.3
Fig. 4. Corresponding equivalent circuit used to fit the EIS experimental data. 15 0.46 -474 94.6 146.8 92.2
20 0.38 -463 86.4 155.5 94.3
Blank 40 17.21 -475 198.9 192.1 -
evaluated by Eq. (6) [39]: 5 3.22 -502 146.2 141.9 81.3
10 1.41 -500 112.8 149.2 91.8
R ct − R oct 15 1.23 -483 101.3 106.3 93.1
% IEI = × 100,
R ct (6) 20 1.15 -482 93.7 163.4 93.8
Blank 50 39.82 -468 186.5 225.7 -
5 7.32 -492 143.4 135.2 81.6
where Rct and R°ct represent the charge transfer resistance in the pre-
10 4.32 -491 120.1 148.5 89.1
sence and absence of PGL, respectively. The %IEI enhanced with an 15 3.45 -421 109.3 108.8 91.1
increase in the PGL concentration. The numerical values of %IEI are 20 2.15 -478 103.1 123.4 94.6
comparable with those of the electrochemical polarisation measure- Blank 60 56.88 -477 251.8 269.1 -
ments (%IEP). The Bode and phase angle figures for steel in the unin- 5 8.65 -486 204.7 201.5 84.6
10 5.15 -496 177.1 168.4 90.9
hibited and inhibited 0.5 M HCl solution are shown in Figs. 6A–D. The 15 3.75 -493 134.5 143.2 93.4
Bode diagrams show one time constant. Over the range of full fre- 20 2.72 -486 121.2 144.2 95.2
quency, the impedance modulus increased with an increase in the PGL
concentration at each constant temperature. Additionally, the fre-
quency range with the supreme phase angle became greater as the PGL 3.4. Measurement of weight loss
concentration increased.
The results of weight loss for steel in the 0.5 M HCl acidic solution at
various temperatures and PGL concentrations are summarised in

5
A.A. Fadhil, et al. Surfaces and Interfaces 20 (2020) 100595

Table 2
Electrochemical parameters form EIS measurements for steel in 0.5M HCl solution at different conditions.
C (mL/L) T (°C) Rs (Ω.cm2) Yo (μ Ω−1 sn cm−2) n Rct (Ω.cm2) Cdl (μF.cm−2) IE%

Blank 30 0.9 303.8 0.91 22.2 338.1 -

5 1.5 208.2 0.87 195.4 125.7 88.6
10 1.2 134.6 0.86 320.8 107.8 92.8
15 1.4 87.8 0.88 365.6 92.21 93.9
20 1.6 67.5 0.85 472.1 84.62 95.2
Blank 40 2.4 609.1 0.79 20.2 450.5 -
5 1.3 340.1 0.83 108.7 157.1 81.4
10 0.9 195.3 0.79 266.3 104.3 92.4
15 1.7 208.7 0.79 348.9 93.41 93.2
20 2.5 162.9 0.92 443.4 85.52 94.4
Blank 50 1.5 591.5 0.81 18.1 501.4 -
5 1.1 332.8 0.85 91.6 128.7 80.2
10 0.9 144.2 0.84 152.4 79.01 88.1
15 2.3 109.3 0.78 297.3 70.1 92.9
20 1.7 89.4 0.81 394.7 67.31 94.2
Blank 60 1.6 584.3 0.89 12.7 580.8 -
5 0.7 408.7 0.86 77.5 136.7 83.8
10 1.8 315.9 0.78 149.3 102.3 91.4
15 2.1 221.1 0.82 276.8 91.55 94.4
20 1.3 101.8 0.74 357.4 82.42 95.4

Table 3. The values of the corrosion rate and weight loss percentage
inhibition efficiency (%IEW) were calculated by sing Eqs. (7) and (8),
respectively:
weightloss(g)
CR = , inhibitor molecules adsorbed on the surface of the metal. In addition, C
area(m2) × time(day)
CR o − CRi
%IEW = × 100,
CRi
where CRi and CRo represent the corrosion rate in the absence and
presence of PGL in acidic solutions, respectively. It is clear that in the
uninhibited and inhibited 0.5 M HCl, the rate of corrosion increased
with an increase in temperature. However, at a certain temperature, the
corrosion rate of the steel decreased with an increase in the con-
centration of PGL. The % IEW improved at higher PGL concentrations.
Table 3 presents data showing the effect of PGL concentration and
temperature on the performance of the inhibitor. The %IEW increased
with an increase in temperature until approaching a maximum value of
95.1%, which is ascribed to an increase in the chemisorption of the PGL
molecules on a metal surface. The adsorption of an inhibitor on a steel
surface represents an important step in understanding the inhibitor
performance in acidic solutions. One conclusion is that reaction of the
corrosion was prevented over areas protected by adsorbed PGL mole-
cules, which means that corrosion reactions commonly occur on PGL-
free active sites [40]. As compared with many other plant extracts, PGL
represents a significant inhibitor for steel in 0.5 M HCl. Table 4 shows
some examples of plants extracts, inhibitors efficiencies vary from 61 to
98.56% within the studied range of inhibitors concentrations (0.1 – 200
g/L, which is approximately equal to mL/L since the density of 0.5 M
HCl ≈1.01g/mL) and temperature (25 – 60 °C) [41 –50]. In other
words, PLG shows significant performance (95.1% inhibitor efficiency
at 20 mL/L and 60 °C) and the adsorption behaviour was also com-
parable.
The coverage of the surface data (ϴ = 0.01% IEW) is highly valu-
able for understanding the mechanism of adsorption. Adsorption iso-
therms represent the relation between the surface coverage and in-
hibitor concentration at a constant temperature. The Langmuir
adsorption isotherm is widely used and assumes that a metal surface
contains a fixed number of adsorption sites, with each site accom-
modating only one adsorbed molecule on the metal surface. In Fig. 7, C/
ϴ versus C shows linear plots for the Langmuir adsorption isotherm.
The high linearity lines indicate that the adsorption process obeys the
Langmuir adsorption isotherm as shown in Eq. (9):
C 1
= + C,
θ K (9)
where the degree of adsorption is represented by the adsorption equi-
librium constant (K). Higher values of K relate to a greater number of
(7)
represents the PGL concentration. In Fig. 7, the Langmuir adsorption
lines are approximately at unity with high correlation coefficients (R2).
This means that each active site occupies one inhibitor molecule on the
(8) metal surface. The standard adsorption free energy (ΔGads) was eval-
uated using the following equation (Eq. 10) [51]:
1 ΔGads ⎞
K= exp ⎛− ,
55.5 ⎝ RT ⎠ (10)
where the number 55.5 is the water concentration in the solution ex-
pressed in units of molarity (approximately 999 mL/L), R is the gas
constant (8.314 J/mol K), and T is the absolute temperature (K). The
adsorption parameters are listed in Table 5. A negative value of ad-
sorption heat indicates a spontaneous and stable PGL layer on the steel
surface. It is widely accepted in the literature that a value of ΔGadso up
to -20 kJ mol−1 assumes the physical adsorption of inhibitor molecules
on a metal surface; higher values are related to chemical adsorption
[52, 53]. In the present work, the values of ΔGadso increased from
-17.71 kJ mol−1 to -22.03 kJ mol−1 as the temperature increased from
30°C to 60°C. This means that at lower temperatures, the adsorption is
caused by electrostatic interaction between the charged steel surface
and the charged PGL molecules, which reflects physical adsorption. As
the temperature increases, the adsorption could be attributed to elec-
tron transfer from the PGL molecules to the steel surface, which reflects
chemical adsorption. Therefore, the adsorption might be mixed mode,
i.e. a physical and chemical adsorption mechanism.
Inhibitor activity and kinetics can be studied by evaluating the ac-
tivation energy (Ea) in the absence and presence of PGL. The Ea for both
corrosion and corrosion inhibition process of metal in HCl at different
temperatures were evaluated by using an Arrhenius-type equation [54]:
Ea
C R = A exp(− ).
RT (11)
The linear form of Eq. 11 can be written as
Ea
ln(CR) = ln A − .
RT (11a)
In Eq. (11) and (11a), CR is the rate of corrosion, A is the constant or
modified frequency factor of the Arrhenius equation, and R is the uni-
versal gas constant. Eq. (11a) can be plotted as the natural logarithm of

6
A.A. Fadhil, et al.
Fig. 5. Bode plots for N80 steel in 0.5M HCl solution without and with different concentrations of PTT at different temperatures.
the corrosion rate [ln (CR)) against reciprocal of absolute temperature
(1/T), as shown in Fig. 8. The slopes and intercepts of the lines of Ar-
rhenius equations can be used to estimate the values of Ea and A, re-
spectively. Table 6 illustrates the Ea and A for the metal corrosion re-
actions in inhibited and uninhibited acidic solutions. The Ea in the
absence of PGL was higher than the values the inhibited solution. The
reduction in the value of Ea appears to be unreliable, which could be
attributed to an increase in the surface area covered by the PGL mo-
lecules at elevated temperatures [55]. Other explanations suggest that
an inhibitor in a corrosive acidic solution alters the reaction kinetics of
the corrosion process by suggesting different reaction paths with lower
Ea [56]. PGL is consists of complex organic materials, such as sterols,
7
Surfaces and Interfaces 20 (2020) 100595
carotenoids, polyphenolic acids, flavonoids, polysaccharides, reducing
agents [57]. It is rich with polar functional groups and/or heteroatoms,
which are considered to be highly effective anti-corrosion materials.
This variety of organic compounds can be adsorbed on metal active
sites with lower Ea.
As shown in Table 5, the A values in presence of PGL were lower
than those of the PGL-free solution, which is favourable for inhibiting
the corrosion rate. These results agree with many of those in the lit-
erature, which indicate that the rise in A increases the metal corrosion
rate [58].
A.A. Fadhil, et al. Surfaces and Interfaces 20 (2020) 100595

Fig. 5. (continued)

Table 3
Corrosion rate data for steel in 0.5 M HCl acid at different conditions.
C (mL/L) T (°C) Rate of Corrosion (gmd) %IEW

Blank 30 728.7 0
5 105.6615 85.5
10 85.2579 88.3
15 56.8386 92.2
20 42.9933 94.1
Blank 40 896.3 0
5 124.5857 86.1
10 76.1855 91.5
15 60.9484 93.2
20 49.2965 94.5
Blank 50 1126.7 0
5 154.3579 86.3
10 93.5161 91.7
15 73.2355 93.5
20 60.8418 94.6
Blank 60 1365 0
5 117.39 91.4
Fig. 6. Langmuir adsorption isotherms of PGL on the steel surface in 0.5 M HCl 10 99.645 92.7
solution at different temperatures. 15 83.265 93.9
20 66.885 95.1

3.5. Fourier transform infrared measurements

The diagnosis of materials and compounds can be evaluated using
Fourier transform infrared (FTIR) [59–64]. Furthermore, the type of
organic inhibitor bonding in the adsorption on steel surfaces can be
evaluated [65]. Thus, FTIR analysis was conducted on both pure PGL
powder (i.e. before mixing with HCl) and the powder of the adsorbed
film collected from the steel surface after 24 h of immersion in the HCl
containing 20 mL/L PGL at 60°C. As shown in Fig. 8, the FTIR spectrum
of the PGL powder after immersion shifted to higher transmittance
compared with that before immersion. The band located at about 2900
cm−1 can be attributed to C-H stretching vibration, and the band at
1700 cm−1 was caused by the C=C and C=N stretching vibration. The

8
A.A. Fadhil, et al. Surfaces and Interfaces 20 (2020) 100595

Table 4
Comparison of PGL with some other plant extracts for mild steel in 0.5M HCl
Inhibitor Max. %IE Concentration (g/l) Temperature (°C) Adsorption isotherm Adsorption type

PGL 95.1 20 60 Langmuir Mixed

Cardiospermum halicacabum leaf extract 98.56 200 30 Langmuir Chemical [41]
Crataegus oxycantha 66 0.4 30 Langmuir Physical [42]
Prunus avium 61 0.4 30 Langmuir Physical [42]
glycine max leaves extract 91.07 2 35 Langmuir Physical [43]
Sinapis alba 88 0.1 50 Langmuir Chemical [44]
kernel cake powder (Elaeis guineensis Jacq.) 87 1.77 25 Langmuir Chemical [45]
Luffa cylindrica Leaf Extract 87.89 1 60 Langmuir Physical [46]
Pimenta dioica leaves extract 98.52 130 35 Langmuir N/A [47]
Arthrospira platensis extract 66 0.25 25 Langmuir Physical [48]
Dillenia pentagyna 92.29 1.2 35 Langmuir Mixed [49]
Terminalia catappa 78.07 6 27 Langmuir Physical [50]

Table 6
Parameters of activation for corrosion reaction of steel in 0.5M HCl at different
PGL concentrations.
C (mL/L) A (gmd) Ea (kJ/mol)

0 806129.75 17.71
5 7115.28 12.89
10 4536.91 11.11
15 727.78 5.54
20 713.37 4.67

Fig. 7. Arrhenius plots of steel N80 in uninhibited and inhibited 0.5M HCl.

Table 5
Parameters of adsorption of PGL at different temperatures.
T (°C) K (L/mL) ΔGads (kJ/mol)

30 1.13 -17.71
40 1.45 -18.94
50 1.48 -19.61
60 2.87 -22.04
Average value 1.73 -20.00

Fig. 9. UV spectrum of PGL powder before and after immersion for 24 h in

0.5M HCl at 60 °C.

wide band at 3400 cm−1 is related to O-H or N-H stretching. In con-

trast, the absorption bands at about 1500 cm−1 and 1100 cm−1 can be
attributed to the structure vibration of the aromatic ring. These results
indicate that the PGL adsorption layer contains N2 atoms or alcohol in
the functional groups (N-H, O-H, C=C, C=N, and C-N) and the aro-
matic ring. The shifts of FTIR spectrum of the protection layer of the
metal surface compared with that of the inhibitor powder are often
attributed to the creation of a PGL–Fe2+ complex on a steel surface
[66].

3.6. UV measurement

UV measurement offers significant and traditional techniques for

identifying a metal complex [67]. The UV–visible absorption spectra of
the 20 mL/L PGL inhibitor were obtained before and after 24 h of
Fig. 8. FTIR spectrum of PGL powder before and after immersion for 24 h in immersion of the steel specimens. Fig. 9 shows the UV–visible absorp-
0.5M HCl at 60 °C. tion spectra for both cases. The absorption spectrum of PGL before the

9
A.A. Fadhil, et al. Surfaces and Interfaces 20 (2020) 100595

Fig. 10. SEM of steel N80 in uninhibited and inhibited 0.5M HCl.
A. Before test
B. After test at 30 °C in absence of inhibitor.
C. After test at 30 °C in presence of 20 mL/L inhibitor PGL.
D. After test at 60 °C in absence of inhibitor.
E. After test at 60 °C in presence of 20 mL/L inhibitor PGL.

metal immersion showed three bands in the UV region that could have
formed due to π-π* and n- π* transitions with a considerable charge
transfer. After 24 h of immersion of the steel samples, the change in the
absorption position indicates a complex formation between the PGL and
the surface of steel. In addition, significant deviation was noted in the
shape of the UV spectra before and after the specimen immersion,
which indicates the possibility of forming an inhibitor layer over the
steel surface.

10
A.A. Fadhil, et al.
3.7. Surface morphology measurement
Scanning Electron Microscopy (SEM) was used widely to study the
surface morphology of metals and alloys [68–71].After 24 h of steel
immersion in 0.5 M HCl in the absence and presence of 5 ppm and 20
ppm PGL at two temperature levels (30°C and 60°C), the surface mor-
phology of the surface was studied using SEM. Fig. 10A shows the steel
samples before the test with no observed damage. The unprotected steel
surface at 30°C (Fig. 10B) showed clear damage due to the corrosive
solution attack. Generally, moderately smoother morphologies were
noted than those observed when uninhibited solution was used. The
surfaces were inhibited by PGL at 30°C and 60°C (Fig. 10C and E). At
elevated temperatures, coarser surfaces were detected (Fig. 10D). Ac-
cording to the above observations, the PGL layer protected the surface
of metal and had a lower permeability for the HCl solution in com-
parison with that of the unprotected surface. Therefore, the steel sur-
face was successfully covered by the addition of the PGL inhibitor,
which confirms the gravimetrical and electrochemical studies.
4. Conclusions
The following points were concluded from the present work:
1. The addition of PGL to a 0.5 M HCl solution led to a significant
decrease in the corrosion rate of N80 steel. A maximum inhibition
efficiency of 95% at high levels of temperature and inhibitor con-
centration was obtained.
2. The performance of PGL increased with the concentration of the
inhibitor, which is ascribed to the formation of a protective layer
spontaneously adsorbed on the steel surface.
3. The potential at steady-state conditions was attained after nearly
1200 s.
4. All corrosion rate measurements including polarisation, EIS, and
weight loss studies proved that the PGL inhibitor acted as a mixed-
type inhibitor.
5. After immersion of steel samples for 24 h in the inhibited hydro-
chloric acid corrosive solution, FTIR investigations revealed that the
spectrum shifted to a higher transmittance.
6. The SEM micrographs show that the damage to steel surface can be
ascribed to deterioration by corrosion. The addition of PGL to the
aggressive media decreased the corrosion rate of the steel.
Data availability
All data are available in present paper.
CRediT authorship contribution statement
Ahmed A. Fadhil: Data curation, Software. Anees A. Khadom:
Data curation, Writing - review & editing. Salima K. Ahmed: .
Hongfang Liu: Visualization, Investigation. Chaoyang Fu:
Visualization, Investigation. Hameed B. Mahood: Writing - review &
editing.
Declaration of Competing Interest
We wish to confirm that there are no known conflicts of interest
associated with this publication and there has been no significant fi-
nancial support for this work that could have influenced its outcome.
Acknowledgments
This research has been supported by the National Natural Science
Foundation of China (51171067, 51475177).
11
Surfaces and Interfaces 20 (2020) 100595
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