Effect of Equisetum arvense extract as corrosion inhibitor of A36 steel in sulfuric acid solution

Abstract

The Equisetum arvense extract was prepared by the maceration technique and experimentally tested as a corrosion inhibitor of A36 steel in 0.5 M sulfuric acid at room temperature. The corrosion resistance was estimated by the determination of the polarization curves, linear polarization resistance (LPR) and electrochemical impedance spectroscopy (EIS). In order to study the effect of the Equisetum arvense extract on the superficial morphology of metal, scanning electronic microscopy (SEM) was used. The results indicated a decrease of about two orders of magnitude in the corrosion rate, an increase in polarization resistance and a greater efficiency of inhibition by increasing the concentration of extract. The corrosion mechanism was mainly controlled by charge transfer from metal to the environment through the double electrochemical layer. The SEM images corroborated the results obtained in the corrosion tests, at higher concentration of extract less metal surface damage was observed.

Full text

Received: 21 February 2018
|
Accepted: 1 June 2018
DOI: 10.1002/maco.201810119
ARTICLE
Effect of Equisetum arvense extract as corrosion inhibitor of A36
steel in sulfuric acid solution
Gladiola I. Ramírez-Peralta
1
|
Ulises León-Silva
2
|
Maria E. Nicho Díaz
1
|
María G. Valladares-Cisneros
3
1
Centro de Investigación en Ingeniería y
Ciencias Aplicadas, ICCBA, Universidad
Autónoma del Estado de Morelos,
Universidad 1001, Col. Chamilpa, C.P.
62210 Cuernavaca, Morelos, México
2
Instituto Nacional de Electricidad y
Energías Limpias, Reforma 113, Col.
Palmira, C.P. 62490 Cuernavaca, Morelos,
México
3
Facultad de Ciencias Químicas e
Ingeniería, Universidad Autónoma del
Estado de Morelos, Av. Universidad 1001,
Col. Chamilpa, C.P. 62209 Cuernavaca,
Morelos, México
Correspondence
Ulises León-Silva, Instituto Nacional de
Electricidad y Energías Limpias, Reforma
113, Col. Palmira, C.P. 62490, Cuernavaca,
Morelos, México.
Email: ulises.leon@ineel.mx
The Equisetum arvense extract was prepared by the maceration technique and
experimentally tested as a corrosion inhibitor of A36 steel in 0.5 M sulfuric acid at
room temperature. The corrosion resistance was estimated by the determination of
the polarization curves, linear polarization resistance (LPR) and electrochemical
impedance spectroscopy (EIS). In order to study the effect of the Equisetum
arvense extract on the superficial morphology of metal, scanning electronic
microscopy (SEM) was used. The results indicated a decrease of about two orders
of magnitude in the corrosion rate, an increase in polarization resistance and a
greater efficiency of inhibition by increasing the concentration of extract. The
corrosion mechanism was mainly controlled by charge transfer from metal to the
environment through the double electrochemical layer. The SEM images
corroborated the results obtained in the corrosion tests, at higher concentration
of extract less metal surface damage was observed.
KEYWORDS
A36 steel, corrosion inhibitor, Equisetum arvense, sulfuric acid
1
|
INTRODUCTION
It is very important to protect the metal in structures and
equipment against corrosion in transport, industries, residen-
tial areas, malls, hospitals, universities, buildings, home, etc.
In the oil industry one of the major problems is the use of acids
for chemical cleaning and pickling to remove oxide scales
from the metal surface.
[1]
The efforts to control corrosion have allowed the
development of techniques for this purpose, of which we
have: design of materials or components, selection of
materials, passivators, or inhibitors, coatings, cathodic
protection, pH adjustment, among others. In this work, we
are concerned about talking about inhibitors. Thus, inhibitors
are substances or mixtures that in low concentration and in
aggressive environment inhibit, prevent or minimize the
corrosion.
[2]
Generally, the mechanisms of the inhibitor are:
the inhibitor adsorbs on metal surface to form a protective
barrier and thereby decreases the anodic and/or cathodic
reactions responsible for the corrosion process
[3]
; the
inhibitor reacting with a potential corrosive component
present in aqueous media to form a complex product.
[4]
Organic extracts containing functional groups with
oxygen, nitrogen, sulfur atoms in a conjugate system have
been reported as efficient inhibitors.
[5]
The advantages of
organic inhibitors are low cost of processing, biodegradabil-
ity, and absence of heavy metals or other toxic compounds
which pose great hazard to the environment.
[6]
Numerous
investigations have been reported, for example: Lycium
shawii, Teucrium oliverianum, Ochradenus baccatus,
Materials and Corrosion. 2018;1–7. www.matcorr.com © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim
|
1

Anvillea garcinii, Cassia italica, Artemisia sieberi,
Carthamus tinctorius, and Tripleurospermum auriculatum
extracts inhibited the corrosion of mild steel in acidic media
through adsorption and act as mixed inhibitors.
[7]
The
Zenthoxylum alatum plant extract reduces effectively the
corrosion of mild steel in 5% aqueous hydrochloric acid
solution.
[8]
The Hyptis suaveolens leaf extract was found
efficiently inhibit the corrosion process of mild steel in 1 M
sulfuric acid, and inhibition efficiency increased with
increasing extract concentration.
[9]
The Hibiscus sabdariffa
extract showed good inhibiting property for mild steel
corrosion in 1.2 N sulfuric acid.
[10]
The Ananas sativum
extract retarded the corrosion of aluminium, the efficiency of
this plant extract increases with the increase in its concentra-
tion and temperature.
[11]
The extract of Dodonaea viscosa
leaves acted as an effective corrosion inhibitor of mild steel in
1 M hydrochloric acid and 0.5 M sulfuric acid. The inhibition
efficiency increased with increase in concentration of the
inhibitor and decreased with temperature.
[12]
The Acalypha
torta extract leaves acted as a mixed type inhibitor for the
mild steel in 1 M hydrochloric acid.
[13]
The Hibiscus
sabdariffa extract suppressed the corrosion reaction in 2 M
hydrochloric acid and 1 M sulfuric acid solutions.
[14]
The
banana peel extract functioned as mixed type inhibitor for
carbon steel. It had excellent inhibition efficiency (IE) of 98%
at Zn
2+
(15 ppm) determined by the weight loss method.
[15]
In the present work, the Equisetum arvense extract as
corrosion inhibitor of A36 steel in 0.5 M sulfuric acid was
studied. The Equisetum arvense is a primitive wild plant,
descendant of the enormous trees of the Palaeozoic era. The
name of the genus, Equisetum, derives from the Latin: equus
(horse) and seta (horsehair). This plant has a high content of
mineral salts, mainly silica, some of them water soluble; is
distributed throughout the temperate zones of the north
hemisphere. Two chemo-types have been identified, one in
Europe and the other in Asia and North America, which can
be distinguished chemically by the presence of characteristic
flavonoids (isoquercitrina as possible antioxidant) in the
sterile stems.
[16]
2
|
EXPERIMENTAL SECTION
2.1
|
Material and reagents
The following materials and reagents were used for the
preparation of Equisetum arvense extract and the electrolytes
for corrosion tests: methanol (MW 32.04 g mol
−1
, 99.8%),
sulfuric acid (MW 98.08 g mol
−1
, 97.7%), ethyl alcohol (MW
46.07, 99.5%), and distilled water (MW 18.02 g mol
−1
).
ASTM A36 steel (C 0.2, Mg 0.48, P 0.008, S 0.026, and Si
0.06%) was used to elaborate the samples for the corrosion
tests.
2.2
|
Preparation of plant extract and stock
solution
A total of 200 g of dried Equisetum arvense plant (leaves and
stems) were immersed in methanol for 72 h, at room
temperature and in the dark. The solution was filtered and
the excess solvent was removed under reduced pressure in a
rotary evaporator at 40 °C. The constant weight of the
recovered residue was 4.8 g. The percentage yield was
calculated using the following equation:
%Yield ¼Extract gðÞ=Dry plant gðÞ½100 ð1Þ
The percentage yield was 2.4%. The product obtained was
dissolved in methanol to obtain a stock solution. From the
stock solutions, inhibitor test solutions were prepared at the
following concentrations: 0, 80, 240, 320, and 400 ppm using
excess sulfuric acid as solvent at room temperature (24 °C
approximately). For the corrosion inhibition study 0.5 M
sulfuric acid was used.
2.3
|
Preparation of the A36 steel electrodes
for electrochemical corrosion
The procedure used to prepare working electrodes for
performing electrochemical tests has been previously
reported
[17]
and consist as follows: A copper wire was
welded to the steel sheets using a portable welder
(Thermocouple Attachment Unit). Steel sheets with an
exposure area of 1 × 1 cm
2
were encapsulated with acrylic
resin. A treatment of the exposed side of the steel sheets was
carried out by polishing to a mirror finish with different
grades of emery papers (100, 400, 600, and 1200). The
substrates were washed with water, degreased with ethyl
alcohol, and dried with warm air.
2.4
|
Parameters for electrochemical tests
The corrosion electrochemical tests were carried out in
0.5 M sulfuric acid using a standard three-electrode cell:
electrodes prepared previously (section 2.3) as working
electrodes, saturated calomel electrode (SCE) as reference
electrode and graphite rod as counter electrode. The tests
were performed at room temperature (approximately 24 °C)
and controlled by a Gill 8 AC potentiostat/galvanostat.
For the polarization curves the potential range used was
−1500 to 2000 mV with respect to the free corrosion
potential (E
corr
) at a scan rate of 1 mV s
−1
. Linear
polarization resistance (LPR) curves were obtained by
sweeping the potential region between ±10 mV with
respect to E
corr
, using a scan rate of 1 mV s
−1
,every
20 min for 24 h. Electrochemical impedance spectro-
scopy (EIS) tests were carried out at E
corr
using an
2
|
RAMÍREZ-PERALTA ET AL.

alternating current (AC) potential amplitude of 10 mV, a
frequency interval of 0.1 Hz to 30 kHz with 100 readings
per decade.
2.5
|
Surface morphology
The study of the surface morphology for the A36 steel
immersed in sulfuric acid with and without Equisetum
arvense extract was carried out using a scanning electron
microscope (SEM, Karl Seizz DSM100).
3
|
RESULTS AND DISCUSSION
3.1
|
Polarization curves, linear polarization
resistance and electrochemical impedance
spectroscopy
Figure 1 shows the polarization curves of A36 steel with
and without Equisetum arvense extract in 0.5 M sulfuric
acid. Passivation zones were observed for all systems
between 0.5 V and 1.6 V. The passivation is due to the
formation of a protective layer which makes more
difficult the access of the electrolyte to corrode the
underlying metal.
[18]
The corrosion current density (I
corr
)
of A36 steel decreased when the extract concentration
was increased, thus, the system with 400 ppm showed a
decrease of two orders of magnitude in I
corr
with respect to
steel without extract (reference). In addition, with the
system of 400 ppm the corrosion potential (E
corr
)was
shifted towards more noble potentials with respect
to the reference. The other systems showed I
corr
and E
corr
values similar to those obtained with the reference. The
E
corr
,I
corr
, and inhibition efficiency (IE
cpt
)valuesby
polarization test for the systems are given in Table 1. A
positive shift of the E
corr
due to the presence of
Equisetum arvense extract indicated that this organic
compound is an effective suppressor of the anodic
dissolution reaction,
[19]
which could be related to the
formation of a protective layer.
[20]
On the other hand, the
negative shift of E
corr
indicated the acceleration of
anodic dissolution of the oxide layer.
[21]
The parameters
of E
corr
and I
corr
were determined by extrapolation
of the cathodic polarization curve and anodic polarization
curve, and IE
cpt
was calculated from the following
equation
[22]
:
IEcpt %ðÞ¼1Icorr=I0
corr

100 ð2Þ
where I
0corr
and I
corr
are corrosion current densities in absence
and presence of Equisetum arvense extract, respectively.
The increase in the inhibition efficiency with the
increase in the extract concentration could be attributed
to changes in adsorption-desorption equilibria.
[23]
In the
case of the system at 80 ppm, the difference in efficie-
ncies (Table 1) could be due to the fact that the
polarization test lasted approximately 30 min, probably at
this time, the extract at 80 ppm concentration is not fully
absorbed on the metal surface. However, for the LPR test,
which lasted 24 h, the extract had sufficient time to
be fully absorbed on the metal surface and thus show its
corrosion-inhibiting effect. The differences in efficiency
could also be due to the applied potential, which in
the case of potentiodynamic curves is greater than in the
LPR tests causing different effects in the electroc-
hemical system.
Figure 2 shows the change in polarization resistance
(R
p
) over time for A36 steel in presence and absence of the
Equisetum arvense extract in 0.5 M sulfuric acid. It can be
seen that increasing the extract concentration increased the
R
p
values. In the case of the concentrations of 320 and
400 ppm there was an increase of one order of magnitude
with respect to the values obtained in the reference. After
4 h of testing, all systems showed R
p
values greater than the
reference. The R
p
values increased as the inhibition
approached the maximum when the metal apparently
stopped corroding.
[24]
The increase of R
p
values with the
increase of the extract concentration is due to the adsorption
of the organic molecule on the metal surface.
[25]
The
corrosion inhibition can be attributed to the adsorption of
organic molecules at the metal solution interface.
[26]
The
Equisetum arvense contains twenty-five compounds identi-
fied in its oil, some of which could be absorbed on the
surface of the metal.
[27]
In this study, eight major
components were identified (Table 2). According to the
literature,
[28–30]
fatty acids (3–6 in Table 2) and β-Sitosterol
FIGURE 1 Polarization curves of A36 steel with and without
Equisetum arvense extract in 0.5 M sulfuric acid
RAMÍREZ-PERALTA ET AL.
|
3

(8 in Table 2) are the main responsible for the reduction of
the corrosion rate.
The R
p
values and the inhibition efficiency by LPR test
(IE
LPR
) are given in Table 2. The IE
LPR
was calculated from
the following equation:
IELPR %ðÞ¼ RpiðÞRp=RpiðÞ

100 ð3Þ
where R
p
and R
p(i)
are the polarization resistance of A36 steel
in absence and presence of Equisetum arvense extract,
respectively.
Figure 3 shows the Nyquist plots for A36 steel in
presence and absence of the Equisetum arvense extract in
0.5 M sulfuric acid. The semicircles appearance of the
diagrams in the figure indicates that the corrosion of A36
steel is controlled by a charge transfer process.
[25,31]
The
small inductive loop in low frequencies is usually related to
an adsorbed intermediate species formed during the
dissolution of the metal.
[32]
The inductive loop was
attributed to active dissolution of the carbon steel, through
intermediate species FeOH
ads
, according to Eq. (5) of the
mechanism
[33]
:
Fe þH2O→FeOHads þHþþeð4Þ
FeOHads →FeOHþsol þeð5Þ
FeOHþsol þHþ→Fe2þsol þH2Oð6Þ
The size of the semicircles increased as the extract
concentration rised and therefore the inhibition efficiency
increased, indicating that the corrosion process was con-
trolled. The shape of the diagrams was similar for all systems,
indicating that no change occurred in the corrosion mecha-
nism after inhibitor addition.
[34]
The corresponding Bode plot (phase angle vs. fre-
quency) presented in Figure 4 shows two time constants,
one in high-frequency at approx. 1000 Hz related to the
semicircle observed in high-frequency in the Nyquist plot
(double electric layer) and other in low-frequency, valley
at approx. 0.2 Hz related to the loop observed in the
Nyquist plot.
The impedance diagrams were fitted by a simple Randles
circuit (Figure 5). This circuit consists of R
s
solution
resistance, R
ct
charge transfer resistance, and C
dl
double
layer capacitance. A constant phase element (CPE) is used
instead of a pure capacitor in order to take into consideration
the electrode surface heterogeneity resulting from the surface
(roughness, dislocations, impurities, inhibitors adsorption
and porous layer formation).
[35]
The CPE allows to get a more
accurate fit of experimental data set
[34]
and its impedance is
given by Eq. (7):
ZCPE ¼A1iωðÞ
nð7Þ
where Ais proportionality coefficient, ωis the angular
frequency, and iis the imaginary number, nis an exponent
related to the phase shift and can be used as a measure of
surface irregularity.
[36]
The value of C
dl
, can be calculated for
a parallel circuit composed of a CPE (Q) and R
ct
, according to
the following equation
[37]
:
Cdl ¼QRct1n

1=nð8Þ
TABLE 1 Values of electrochemical parameters from polarization curves and linear polarization resistance
Extract concentration I
corr
(mA cm
−2
)E
corr
(V) IE
cpt
(%) R
p
(Ohms cm
2
)IE
LPR
(%)
0 ppm 0.07 −0.42 –36 –
80 ppm 0.13 −0.48 −80 94 61
240 ppm 0.06 −0.67 15 98 63
320 ppm 0.05 −0.65 29 312 88
400 ppm 2.6 E-4 0.03 99 280 87
FIGURE 2 R
p
as a function of time for A36 steel with and
without Equisetum arvense extract in 0.5 M sulfuric acid
4
|
RAMÍREZ-PERALTA ET AL.

TABLE 2 Compounds identified from gas chromatography–mass spectrometry of Equisetum arvense extract.
Compound
Retention time
(min)
Amount
(%) Fragmentation peaks
2,3-dihydro-2,5-dihydroxy-6-methyl-4H-pyran-
4-one (1)
9.56 13.99 13, 126, 115, 101, 72, 55, 43
5-hydroxymethyl-2-furancarboxaldehyde (2) 10.74 4.79 109, 97, 81, 69, 53, 41, 29
Hexadecanoic acid, methyl ester (3) 18.94 2.07 239, 227, 213, 185, 171, 143, 129, 115, 97, 87, 74,
55, 43
Hexadecanoic acid (4)
19.38 14.85 227, 213, 199, 185, 176, 157, 143, 129, 115, 97, 83, 73, 60, 43
9,12-octadecadienoic acid, methyl ester (5)
20.59 1.11 263, 234, 220, 193, 178, 164, 150, 136, 123, 109, 95, 81, 67, 55, 41
9,12,15-octadecatrienoic acid, methyl ester (6) 21.10 18.63 236, 194, 171, 149, 135, 121, 108, 93, 79, 67, 55, 41
Campesterol (7) 32.25 6.29 382, 367, 315, 289, 255, 213, 187, 145, 107, 95, 81,
55, 43
β-Sitosterol (8) 37.03 9.68 396, 381, 329, 303, 273, 255, 231, 159, 145, 107, 81,
55, 43
TABLE 3 Values of electrochemical parameters from EIS in 0.5 M H
2
SO
4
.
Extract concentration R
s
(Ωcm
2
)R
ct
(Ωcm
2
)C
dl
(µF cm
−2
)Q(s
n
Ω
−1
cm
−2
)IE
EIS
(%)
0 ppm 1.53 56 2.53 × 10
−4
9.8 × 10
−1
–
80 ppm 1.15 63 2.55 × 10
−4
9.7 × 10
−1
11
240 ppm 1.13 224 1.24 × 10
−4
8.6 × 10
−1
75
320 ppm 2.8 246 1.57 × 10
−4
9.7 × 10
−1
77
400 ppm 2 251 1.99 × 10
−4
8×10
−1
78
FIGURE 3 Nyquist plots for A36 steel with and without
Equisetum arvense extract in 0.5 M sulfuric acid
FIGURE 4 Bode diagrams for A36 steel with and without
Equisetum arvense extract in 0.5 M sulfuric acid
RAMÍREZ-PERALTA ET AL.
|
5

The inhibition efficiency by electrochemical impedance
spectroscopy (IE
EIS
) was calculated from the following
equation
[33]
:
IEEIS %ðÞ¼Rct iðÞ Rct =Rct iðÞ

100 ð9Þ
where R
ct
and R
ct (i)
are the charge transfer resistance of A36
steel in absence and presence of the Equisetum arvense
extract, respectively. The R
ct
,C
dl
, and IE
EIS
values are shown
in Table 3.
Table 3 shows that the R
ct
values increase with the
increase in the extract concentration and as a result the
inhibition efficiency increases to 78%. An increase
in R
ct
values indicates a higher metal surface area covered
by the inhibitor as a result of an increase in inhib-
itor concentration.
[38]
This increase in R
ct
confirmed
that a charge transfers process controls the corrosion of
steel.
[37]
The decrease in C
dl
values is due to the
inhibitor adsorption on the metal surface leading to the
formation of film or complex from acidic solution.
[39]
Results obtained from EIS measurements were in
good agreement with those obtained from DC corro-
sion tests.
3.2
|
Surface morphology of the A36 steel
The surface morphology of A36 steel in presence and
absence of the Equisetum arvense extract in 0.5 M sulfuric
acid was characterized. In order to demonstrate that at
higher concentrations there is less damage by corrosion,
images of the reference and at 320 and 400 ppm were
obtained. It can be seen that for steel without extract
(Figure 6a) the metal surface had the most amount of cracks
and microcracks. However, the A36 steel in presence of
320 ppm of extract decreased the surface damage
(Figure 6b) and at 400 ppm of extract the metallic surface
was more regular, homogenous and smooth (Figure 6c).
Less damage was observed when increasing the extract
concentration.
4
|
CONCLUSIONS
The effect of Equisetum arvense extract as a corrosion
inhibitor for A36 steel in 0.5 M sulfuric acid was investigated.
This extract was obtained by the maceration technique of
leaves and stems. Corrosive tests showed that the Equisetum
arvense extract in 320 and 400 ppm concentrations acted as a
good corrosion inhibitor for A36 steel. The extract was
adsorbed on the metal surface and at 400 ppm decreased the
corrosion rate two orders of magnitude with respect to the
FIGURE 6 SEM images of the A36 steel in absence a) and
presence of the Equisetum arvense extract b) 320 ppm, and c)
400 ppm
FIGURE 5 The simple Randles circuit used to fit EIS spectra
6
|
RAMÍREZ-PERALTA ET AL.

reference (steel without extract). The anodic current of metal
oxidation decreased when the concentration of Equisetum
arvense extract increased indicating that this extract inhibits
corrosion by inhibiting anodic reaction. By increasing the
extract concentration in the medium, the values of the
polarization resistance increased, thus decreasing the corro-
sion rate. According to the results obtained in electrochemical
impedance, the mechanism that mainly controlled the
reaction was charge transfer. All the corrosion tests were
congruent in their results, showing the tendency that the
higher the concentration of the inhibitor, the greater the
protection against steel corrosion. The corrosion tests were
corroborated by SEM microscopy. Thus, with the 400 ppm
concentration of Equisetum arvense extract a homogeneous
and less damaged surface was observed.
ORCID
UlisesLeón-Silva http://orcid.org/0000-0003-0924-9980
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How to cite this article: Ramírez-Peralta GI,
León-Silva U, Nicho Díaz ME, Valladares-Cisneros
MG. Effect of Equisetum arvense extract as
corrosion inhibitor of A36 steel in sulfuric acid
solution. Materials and Corrosion. 2018;1–7.
https://doi.org/10.1002/maco.201810119
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