Arabian Journal for Science and Engineering

https://doi.org/10.1007/s13369-019-04270-2

RESEARCH ARTICLE - CHEMISTRY

Surface Adsorption and Corrosion Resistance Performance of Acacia

concinna Pod Extract: An Efficient Inhibitor for Mild Steel in Acidic
Environment
Rajesh Haldhar1 · Dwarika Prasad1   · Nishant Bhardwaj1

Received: 15 May 2019 / Accepted: 25 November 2019

© King Fahd University of Petroleum & Minerals 2019

Abstract
The object of this study is to experimentally evaluate the inhibition properties of Acacia concinna (A. concinna) extract
in a 0.5 M sulphuric acid media for mild steel. The protective film-formation study was done using UV–Vis spectroscopy.
Surface film composition and morphology were examined by scanning electron microscope and atomic force microscope.
Electrochemical impedance spectroscopy (EIS) and potentiodynamic spectroscopy (PDS) were carried out to explain the
combined (cathodic and anodic) nature and cathodic dominance of A. concinna. Results of electrochemical analyses showed
that 250 mg/L inhibitor concentration had the highest performance and efficiency (proved to be 94% by EIS and 92% by PDS
results). The formed film in this sample showed the highest hydrophobicity and literally no obvious forms of corrosion. The
theoretical results showed the comparative adsorption of phytochemicals on the steel. All acquired outcomes confirmed that
A. concinna extract can develop an efficient protective layer and resist the corrosion procedure.

Keywords  EIS · PDS · Green corrosion inhibitor · SEM · AFM · Acacia concinna

1 Introduction inhibitor is eco-friendly, biodegradable, and non-toxic. It is

easily accessible from our surrounding, hence cost-effective
We lose almost 75,000 billion USD per year due to corro- [8–11]. Reason to choose 0.5 M sulphuric acid was due to
sion across the world, which equals to a 3.4% global GDP. In this being the lowest concentration with a significant cor-
India, around 1670 billion USD is lost due to corrosion per rosion rate which does not damage the electrochemical
year, which equals to 4.2% GDP of the country [1]. Steel is workstation. A few investigations were reported by differ-
effectively accessible with its exceptional mechanical prop- ent scientists utilizing such materials as an efficient corro-
erties in manufacturing procedure and construction [2]. The sion inhibitor for various metals in different media. How-
principal issue with utilizing steel is its lower corrosion- ever, majority of corrosion inhibitors gave good inhibition
resistance nature, as it gets rapidly corroded when comes performance at higher inhibitor concentration. On the other
into contact with an acidic medium, for example, sulphuric hand, synthetic inhibitors can significantly inhibit corrosion,
acid [3]. It is notable that the acidic solutions are broadly but are costly.
utilized in different industrial processes for pickling, descal- A. concinna pod is a climbing shrub, belonging to the
ing, and cleaning. The inhibitor forms a protective film on Mimosaceae family and commonly known as Shikakai.
the surface of the steel using their π-electrons framework These are usually available all around India and East Asian
and heteroatoms, for example, O, P, S, N [4–7]. The inhibitor continent. A. concinna contains Acacia acid, Acacidiol, and
adsorption on MS surface is either physical (physisorption) Acacigenin-B as its main phytochemical constituents [12,
or chemical (chemisorption).The plant-extract corrosion 13]. Figure 1 represents A. concinna and its main secondary
metabolites.
The present work is aimed to examine the extract of A.
* Dwarika Prasad concinna for corrosion inhibition behaviour in 0.5 M sul-
[email protected] phuric acid corrosive medium which relies on electrochemi-
1
Department of Chemistry, Shri Guru Ram Rai University, cal methods followed by weight-loss estimates. Adsorption
Dehradun 248001, India of A. concinna extract and protective film formation on

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 Arabian Journal for Science and Engineering

O
H
H

COOH

OH

H
O

(a) (b)

O
H
O
C
O
H
O H

COOH

OH

H
H O

(c) (d)

Fig. 1  a A. concinna pods image and their main chemical components, b Acacia acid, c Acacidiol, and d Acacigenin-B

the surface of steel were examined using AFM and SEM conditions. From this technique, around 9% of yield was
which give important information about the surface mor- obtained, with a pH value of 7.5. 1 cm × 1 cm × 0.03 cm
phology. UV–Vis spectroscopy was used to examine the steel coupons were utilized in weight-loss estimates. The
adsorption. The theoretical study is an add-on to compare chemical composition of steel coupon was recorded as
the film-formation activeness of the main phytochemical. (wt%) Ni = 0.27, Si = 0.39, Cr = 0.45, Cu = 0.43, P = 0.12,
Using A. concinna is an eco-friendly, cost-effective corro- C = 0.08, Mn = 0.43, and balance Fe. The steel coupons
sion inhibitor. were abraded with different grades of emery papers
(100–1200) and then washed with acetone followed by
distilled water, dried in oven, and then placed in a desic-
2 Experimental Studies cator. The corrosive solution was prepared by diluting sul-
phuric acid to 0.5 M. The corrosive media were prepared
2.1 Preparation of Extract and Electrochemical Cell at different concentrations (50–250 mg/L) by diluting A.
concinna extract with 0.5 M sulphuric acid.
Dry A. concinna, as verified by Dr. A. A. Bhatt at Lovely
Professional University, Punjab (INDIA), were thoroughly
washed with tap water followed by sterile distilled water 2.2 Weight‑Loss Measurement
and then dried under shade. Their leaves were crushed to
a powdered form. Static extraction was performed using This measurement was taken according to the ASTM stand-
approximately 350  g of dry A. concinna in methanol ard G 31–72 for 24 h [14]. All evaluations were carried out
(350 ml) in a round-bottom flask connected to a Soxhlet at 298 ± 0.5 K thermostat. The average value was taken by
apparatus for 94 h at 69 °C. The filtrate was gathered and repeating the experiment three times. The following formula
concentrated utilizing the rotary evaporator at controlled was employed to obtain the corrosion rate:

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Arabian Journal for Science and Engineering

K×W Rct − Roct

CR = . (1) IE(%) = × 100. (6)
A×t×𝜌 Rct
The effectiveness of the inhibition was obtained by apply- The efficiency of corrosion inhibition (IE %) in the electro-
ing the following formulas: lytes was calculated by Eq. 6 on the basis of EIS test results
[16].
CR0 − CRi
IE(%) = × 100 (2)
CR0 YCPE = Y0 (j𝜔)n (7)

( )
CR0 − CRi 1
ZCPE = [(j𝜔)n ]−1 (8)
𝜃= (3) Y0
CR0

where the surface coverage values denoted by θ, CRi  , and

( )n−1
Cdl = Y0 𝜔��m (9)
CR0 are used for the corrosion rate of the MS coupons in
the inhibitor and blank solutions, respectively. Adsorption o
Cdl − Cdl
isotherms between C and C/θ are shown in Fig. 4. The value 𝜃= . (10)
of slope and regression coefficient (R2) close to 1 suggests a
o
Cdl
monolayer adsorption on the MS surface [15]. This can be
described by following equation:
2.4 Surface Investigations
C 1
= +C (4)
𝜃 Kads For the surface examination, AFM, followed by SEM, micro-
graphs of the pre-treated surfaces of MS coupons in 0.5 M
where C represents inhibitor concentration, Kads represents sulphuric acid, in the presence and absence of inhibitor extract
the equilibrium adsorption constant, and θ represents the (500 mg/L), at 298 ± 0.5 K were taken.
surface coverage.
2.5 UV–Visible Spectroscopic Studies
2.3 CH‑Instrumental Studies
Shimadzu UV-1800 spectrophotometer with a range of
The electrochemical techniques (Tafel: polarization estima- 200–400 nm was used for recording the absorption spectra.
tions and EIS: impedance spectroscopy) were performed by The UV–Vis measurement was taken at 298 K.
using the CHI760C electrochemical workstation. MS cou-
pons (1 cm2) were immersed in 0.5 M sulphuric acid solu- 2.6 Theoretical Studies
tion along with a mixture of different concentrations of A.
concinna extract for 60 min. At 298 ± 0.5, the values of open Theoretical studies were done for a deeper understanding of
circuit potential (OCP) with respect to the saturated calomel the adsorption mechanism. Quantum chemical calculations
electrode (SCE) were noted. Corrosion inhibition measure- were performed as theoretical studies. It is a well-known fact
ments through EIS techniques were applied in a cell with that the plant extracts have several phytochemical constitu-
SCE as the reference electrode, steel as a working electrode, ents. For theoretical examinations, we followed the existence
and platinum as the counter electrode. Scanning frequencies of three main phytochemicals in A. concinna extract. For theo-
from 100 kHz to 0.01 Hz are used for obtaining the Nyquist retical studies, density functional theory (DFT) at a B3LYP
and Bode plots. A 5 mV signal amplitude perturbation at function was used 6-31G+(d,p) basis set utilizing Hyperchem
OCP was considered in EIS measurement. The polariza- 8.0 software. Followings equations have been used to calculate
tion plots were obtained in the potential range of − 250 to different quantum chemical parameters [17].
+ 250 mV with respect to corrosion potential (Ecorr) and a
scan rate of 1 mV/s. EIS and polarization tests were repeated ΔE = ELUMO − EHOMO (11)
three times to get the average values. For the calculation of
inhibition efficiency, following equations were used: 1(
(12)
)
𝜂= ELUMO − EHOMO
2
i0corr − iicorr
IE (%) = × 100 (5)
i0corr 1(
(13)
)
𝜒 =− ELUMO + EHOMO
2

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 Arabian Journal for Science and Engineering

𝜒 − 𝜒inh for example, C=O. These results reveal some clear evidences
ΔN = ( Fe (14) about the possibility of complex formation between iron and
)
2 𝜂Fe − 𝜂inh
phytochemicals of A. concinna extract [18].
1
𝜎= (15) 3.2 Weight‑Loss Experiment and Adsorption
𝜂
Parameters
𝜂
ΔEBack Donation = − (16) The weight-loss technique is the important and easiest pro-
4
cedure to calculate corrosion-inhibition efficiency of the
natural corrosion inhibitor at different concentrations.
𝜋 = −𝜒 (17) Table 1 shows that with the increment of inhibitor con-
where 𝜒inh and 𝜂inh represent the electronegativity and hard- centration the corrosion rate gradually decreases and the
ness of inhibitor molecule, whereas 𝜒inh and 𝜂Fe mean the inhibition ability increases. This happens because of the
electronegativity and hardness of iron, respectively. adsorption of phytochemicals on the MS surface. When
inhibitor concentration is zero, the highest corrosion rate
(11.33 mm year−1) was observed; on the other hand, when
3 Results and Discussion the concentration of inhibitor was highest (250 mg/L), the
lowest corrosion rate (1.32 mm year−1) was observed. The
3.1 Spectroscopic Studies highest corrosion inhibition effectiveness of 91.13% was
achieved at 250 mg/L. For further confirmation of adsorp-
UV–Vis absorption spectrum (Fig. 2) was obtained for solu- tion mechanism of A. concinna, Langmuir isotherms were
tions containing the extract of A. concinna in 0.5 M sulphu- used.
ric acid, before and after the corrosion test, to detect the In the previous study, M. fragrans showed 83.27% inhibi-
presence of organic compounds and identify the possible tory effect at 500 mg/L with Kads (9.95 Lg−1) [19] whereas
adsorption of phytochemicals on the steel surface. Maxi- A. concinna showed a 94% inhibitory effect at 250 mg/L
mum values of intense absorption peaks recorded for solu- with Kads (41.09 ­Lg−1), which confirms its better perfor-
tion containing A. concinna extract and 0.5 M sulphuric acid mance in the same corrosive medium (Fig. 3).
appeared at 278 nm. The peak assigned at 278 nm corre-
sponded to the n − π* transitions attributed to the functional 3.3 Potentiodynamic Polarization Technique (Tafel)
groups of phytochemicals present in the A. concinna extract,
The corrosion rates of the inhibitor concentrations and polar-
ization curves are provided after 1 h immersion time of the
MS coupons (Fig. 4). The lowest corrosion current density
was recorded at 250 mg/L concentration of A. concinna
extract which confirmed its highest inhibitory effect. The
slight shift of Tafel slope towards cathodic side shows the
predominant cathodic inhibitory action of the A. concinna
extract. Cationic and anion reaction rates at the surface of
steel are explained by the curves of different concentrations
of sample. It is found that the cathodic reaction was highly

Table 1  Corrosive properties obtained by weight-loss experiments of

mild steel in 0.5 M H
­ 2SO4 without and at different concentrations of
A. concinna for 24 h at 298 K
Inhibitor concentra- CR (mm year−1) Inhibition effi- θ
tion (mg/L) ciency (%)

0 11.33 – –
50 1.93 82.94 0.8294
100 1.76 84.44 0.8444
150 1.53 86.45 0.8645
200 1.15 89.76 0.8976
Fig. 2  UV–Vis spectra of A. concinna extract after and before the
250 1.00 91.13 0.9113
corrosion test

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Arabian Journal for Science and Engineering

affected, that is, the rate of releasing hydrogen gas at cath-

ode decreased resulting in a reduced rate of corrosion. The
displacement of corrosion potential of inhibitor with respect
to the blank is within the range of 0–85 mV, indicating that
the inhibitor behaved as a mixed type of inhibitor. Tafel pro-
vided various parameters such as corrosion current density
(icorr), corrosion potential (Ecorr), anodic Tafel slope (βa), and
cathodic Tafel slopes (βc) [20–26].
Table 2 shows that at 250 mg/L inhibitor concentration
(C) maximum decrement in icorr. The changes in the position
of anodic and cathodic sides explain the types of inhibi-
tion effects. The change in the value of βa and βc signifi-
cantly explains the combined cathodic and anodic effects
of inhibitor. This indicates that both iron dissolution and
hydrogen evolution reactions were affected by adsorption
of active components of S. chirata extract. In the previ-
ous study, M. fragrans showed 87.42% inhibitory effect
Fig. 3  The Langmuir adsorption isotherm (C/θ vs. C) by measuring at 500 mg/L with icorr (112.00 μA cm−2) [19] whereas S.
the weight loss of the extract A. concinna for mild steel surface in chirata showed 92.73% inhibitory effect at 250 mg/L with
0.5 M ­H2SO4 at a temperature of 298 K for 24 h
icorr (68.35 μA cm−2), which confirms its better performance
towards the same corrosive medium.

3.4 Electrochemical Impedance Spectroscopy (EIS)

For impedance spectroscopy, MS coupons were exposed

to the corrosive solution protected by A. concinna extract
[27–32]. Nyquist and Bode plots were provided by EIS
analysis and are presented in Fig. 5. Figure 5 shows that the
solution inhibited with 250 mg/L A. concinna extract pro-
vided capacitive loops with larger diameter. The enlargement
of capacitive loop using the A. concinna extract was greater
than the blank. A concentration of 250 mg/L A. concinna
extract leads to the highest enlargement in the capacitive
loop, implying maximum inhibition effect of corrosion natu-
ral corrosion inhibitor. Electrochemical parameters include
polarization resistance (Rp), solution resistance (Rs), double-
layer capacitance (Cdl), and phase shift (n) of inhibitor layer.
According to Fig. 5 and Table 3, the use of a mixture of
Fig. 4  Polarization curves of A. concinna on mild steel in 0.5  M 250 mg/L A. concinna extract gives the maximum corrosion
­H2SO4 for a concentration range of 0–250 mg/L extract at 298 K for
1h inhibition efficiency of 94% and the highest enlargement
of Rp [33]. The surface corrosion diminished significantly
in the presence of aggressive solution. Hence, it can be

Table 2  Polarization parameters Inhibitor −Ecorr (mV Icorr (μA ­cm−2) βa (mV/dec) −βc (mV/dec) Inhibition θ
for mild steel in 0.5 M H
­ 2SO4 concentration vs. SCE) efficiency (%)
without and with different (mg/L)
concentrations of A. concinna
at 298 K 0 465 890.90 141.66 164.26 – –
50 461 138.60 53.23 138.56 84.44 0.8444
100 465 101.90 49.20 132.34 88.56 0.8856
150 459 90.60 45.47 131.42 89.83 0.8983
200 462 74.48 48.27 132.06 91.63 0.9163
250 455 64.75 37.84 152.13 92.73 0.9273

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 Arabian Journal for Science and Engineering

Fig. 5  a An equivalent circuit, b Nyquist and Bode (c) plots of mild steel in 0.5 M H
­ 2SO4 solution in the absence and presence of A. Concinna
extract for 1 h

Table 3  EIS parameters of mild

Concentration of Rct (Ω ­cm2) Rs (Ω ­cm2) Cdl (µF ­cm−2) n Inhibition effi- θ
steel in 0.5 M ­H2SO4 without
inhibitor (mg/L) ciency (%)
and at different concentrations
of A. concinna at 298 K  0 15.71 1.22 269.49 0.57 – –
50 102.59 1.73 130.39 0.87 84.68 0.8468
100 128.44 1.72 126.84 0.89 87.76 0.8776
150 170.42 1.96 95.60 0.94 90.78 0.9078
200 242.20 1.69 144.76 0.96 93.51 0.9351
250 313.00 1.54 76.59 0.97 94.98 0.9498

deduced that blocking the active sites via extract compo- molecules of A. concinna extract is the main reason for the
nents protected the metal surface from corrosion attacks, Cdl decrement, and therefore, corrosion inhibition effect
and because shape of semicircles is same the mechanism increases. The obtained results show chemisorption of A.
of corrosion does not change during the process. Another concinna extract on the MS surface with the help of coor-
result that can be perceived from Table 3 is the decrement of dination bond formation. This is due to sharing of hetero-
Cdl value in the presence of A. concinna extract. This shows atomic non-bonding electrons of A. concinna phytochemical
that the molecules of inhibitor successfully adsorbed on the to the vacant d orbital of Fe. The physisorption process is
metal surface and decreased the local dielectric constant. due to electrostatic interaction between protonated phyto-
By enhancing the extract concentration, the surface cov- chemical and anionic steel surface. These results confirm the
erage was improved based on suitable physisorption and synergic inhibition effect of A. concinna extract on steel in
chemisorption of phytochemicals of A. concinna extract 0.5 M sulphuric acid solution [36–38]. In a previous study,
[34, 35]. The replacement of water molecules with inhibitive M. fragrans showed 87.88% inhibitory effect at 500 mg/L

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Arabian Journal for Science and Engineering

with Rct (128.88 Ω cm2) [39] whereas A. concinna showed 0.5 M sulphuric acid for 24 h. The SEM and AFM images
94% inhibitory effect at 250 mg/L with Rct (313.00 Ω cm2), of MS surface were badly corroded by the sulphuric acid. In
which confirms its better performance towards the same cor- this case, maximum surface roughness (138.81 nm) appears
rosive medium. due to formation of iron hydroxide and oxide on the metal
surface, while Fig. 6c displays the AFM and SEM images of
3.5 AFM and SEM Studies the MS specimens dipped for the same period of time inter-
val in 0.5 M sulphuric acid solution containing 250 mg/L
Figure 6a displays the AFM images along with SEM micro- of A. concinna extract with a lower surface roughness
graph of polished MS with a smooth surface and minimum (32.37 nm), because of blocking of active site and protect-
surface roughness (2.99 nm). Figure 6b displays the AFM ing metal from oxide and hydroxide formation or corrosion.
and SEM images of MS coupon dipped in a solution of The surface roughness value of steel was drastically reduced

Fig. 6  AFM and SEM micro-

graphs of the surface of mild
steel after 24 h immersion
at 298 K in 0.5 M ­H2SO4. a
Abrade mild steel, b without
inhibitor, and c with inhibitor
(250 mg/L)

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 Arabian Journal for Science and Engineering

after adding extract in aggressive media. This result supports main phytochemical components. Figure 7 shows the opti-
the weight-loss data, where, in the presence of 250 mg/L mized, HOMO, and LUMO orbitals of the Acacia acid,
inhibitor concentration, highest inhibition efficiency was Acacidiol, and Acacigenin-B.
observed [16, 39–41]. Table 4 shows a high value of EHOMO for Acacigenin-
B (− 0.19 eV) indicating its high capacity to donate the
electrons to steel. Acacigenin-B has the lowest values
4 Computational Study Explanation of E LUMO (− 4.73  eV) showing the highest capacity to
accept electrons from Fe. Acacigenin-B (4.54 eV) shows
Plant extracts have lots of phytochemical components. the lower value of ΔE indicating its strong influence of
There are three main components of A. concinna selected the [Fe-Acacigenin-B] complex. Figure 8 shows the sug-
for the theoretical study as per literature. A. concinna pod gested mechanism for the adsorption procedure on the MS
contains Acacia acid, Acacidiol, and Acacigenin-B as the surface.

Acacia acid HOMO LUMO

Acacidiol HOMO LUMO

Acacigenin-B HOMO LUMO

Fig. 7  Optimized structures and frontier molecular orbital density distributions (HOMO & LUMO) of Acacia acid, Acacidiol, and Acacigenin-B
obtained by DFT/B3LYP/6-31G+(d,p) method

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Arabian Journal for Science and Engineering

Table 4  Quantum chemical parameters calculated for the Acacia acid, Acacidiol, and Acacigenin-B molecules by the method DFT/B3LYP/6-
31G+(d,p)
Molecule EHOMO (eV) ELUMO (eV) ΔE (eV) ΔN (e) ΔEBack-Donation η (eV) σ ­(eV−1) χ (eV) π (eV)
(eV)

Acacia acid − 7.07 0.53 7.61 0.49 − 0.95 3.80 0.26 3.26 − 3.26
Acacidiol − 9.00 − 2.68 6.32 0.18 − 0.79 3.16 0.31 5.84 − 5.84
Acacigenin-B − 4.73 − 0.19 4.54 0.99 − 0.56 2.27 0.43 2.46 − 2.46

Fig. 8  Suggested mechanism
of adsorption behaviour of the
Acacigenin-B molecule on a
mild steel surface

5 Conclusion • AFM observations show that 250 mg/L of A. concinna

extract sample on steel had the lowest roughness in com-
• The anti-corrosive film of A. concinna extract on MS sur- parison with blank.
face in 0.5 M sulphuric acid was analysed by UV adsorp- • The electrochemical investigation revealed that 250 mg/L
tion studies. had the highest corrosion inhibition in the 0.5 M sulphu-
• SEM micrographs revealed that almost no obvious corro- ric acid solution. Efficiencies of about 94% through EIS
sion products formed at 250 mg/L of A. concinna extract and 92% through PDS technique were calculated for this
sample on the surface of the steel. sample.

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 Arabian Journal for Science and Engineering

Acknowledgement  The authors are grateful to Dr. Gurmeet Singh, extract for steel in 0.5 M H­ 2SO4. J. Fail. Anal. Prev. 18, 957–968
Ex-HOD of Department of Chemistry at University of Delhi, Delhi, (2018)
India, for offering the laboratory resource for impedance workstation. 16. Zahra, S.; Ramezanzadeh, M.; Bahlakeh, G.; Ramezanzadeh, B.:
Use of Rosa canina fruit extract as a green corrosion inhibitor for
mild steel in 1 M HCl solution: a complementary experimental,
Compliance with Ethical Standards  molecular dynamics and quantum mechanics investigation. J. Ind.
Eng. Chem. 69, 18–31 (2019)
Conflicts of interest  The authors declare that there are no conflicts of 17. Haldhar, R.; Prasad, D.; Saxena, A.; Kumar, A.: Experimental and
interests. theoretical studies of Ficus religiosa as green corrosion inhibi-
tor for steel in 0.5 M H­ 2SO4 solution. Sustain. Chem. Pharm. 9,
95–105 (2018)
18. Haldhar, R.; Prasad, D.; Saxena, A.: Armoracia rusticana as
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