electroanalytical studies on the corrosion inhibition behavior of guava (psidium guajava) leaves...
TRANSCRIPT
Electroanalytical studies on the corrosion inhibitionbehavior of guava (Psidium guajava) leaves extracton mild steel in hydrochloric acid
K. K. Anupama • Joseph Abraham
Received: 21 August 2012 / Accepted: 10 November 2012
� Springer Science+Business Media Dordrecht 2012
Abstract Corrosion inhibition behavior of the extract of guava (Psidium guajava)
leaves towards mild steel in HCl media have been studied by polarization, EIS,
adsorption and surface studies at different temperatures. Polarization studies showed
that this extract has good inhibition efficiency (IE) and acts as a mixed-type
inhibitor. As the concentration of the extract increases, the IE also increases,
whereas with respect to temperature the corrosion inhibition shows a reverse trend.
Keywords Mild steel � Acid solutions � EIS � Polarization � Acid inhibition
Introduction
Mild steel being a low cost material is widely used in industries. In petrochemical
industries, corrosion of mild steel is a major problem due to severe attack by
hydrochloric acid when used as a cleaning agent, through chemical reactions [1].
The use of acid is inevitable in industries, as acid solutions are generally used for the
removal of undesirable scale and rust in several industrial processes [2]. Corrosion
inhibition of these metals is mainly achieved through the use of inhibitors. The
inhibitory action of any inhibitor compound is decided by factors such as the
presence of heteroatoms, electronegative functional groups, conjugated double
bonds, presence of aromatic rings, etc. [3].
However, the use of corrosion inhibitors has several limitations as it may be
hazardous when they have to be used somewhere like in a pipeline. The toxic effect
does not only affect living organisms but also poison the environment [2]. The
inhibition performance of plant extracts is normally ascribed to the presence in their
composition of complex organic species such as tannins, alkaloids, nitrogen base,
K. K. Anupama � J. Abraham (&)
Department of Chemistry, University of Calicut, Calicut University P O, Calicut, Kerala, India
e-mail: [email protected]
123
Res Chem Intermed
DOI 10.1007/s11164-012-0923-0
carbohydrates, and proteins [4, 5]. Several authors have investigated and reported
natural corrosion inhibitors like Areca catechu [1], Clematis gouriana [3], olive
leaves [6], henna [7], Rauvolfia serpentina [8], Andrographis paniculata [9],
Oxandra asbeckii [10], Mentha leaves [11], Zenthoxylum alatum [12], Iris tenuifolia[13], Spondias mombin [14], Spirulina platensis [15], Withania somnifera [16],
Piper guineense [17], Buddleia perfoliata [18], Lavandula multifida [19], and argan
hulls [20].
The present work is devoted to examining the extract of guava (Psidium guajava)
leaves as an inhibitor for corrosion of mild steel in HCl media. The guava plant
(P. guajava L.; Myrtaceae) is widely cultivated in tropical and temperate regions of the
O
O
Fig. 1 Structure of typicalflavonoid
Fig. 2 Polarization curves of mild steel corrosion in a 0.5 N, b 1 N, c 1.5 N, d 2 N HCl in absence andpresence of different concentrations of P. guajava water extract at 30 �C
K. K. Anupama, J. Abraham
123
world. Native to Central America, they are small trees with reddish-brown bark and
tough leaves [21]. Phytochemical screening has shown that the extract contains an
appreciable amount of flavonoids and tannins amongst others [22]. Recent phytochem-
ical screening of P. guajava leaves showed tannins in aqueous extract, and anthocyans,
alkaloids, flavonoids (Fig. 1), and steroids/terpenoids in ethanol extract [23].
Experimental
Inhibitor preparation
Fresh guava leaves were collected and identified. They were then sun-dried for
7 days and made into a fine powder. A sample of 2.5 g of powdered leaves were
then extracted with 500 ml of double-distilled water to make P. guajava water
extract. A second sample of 2.5 g of powdered guava leaves were also extracted
with 500 ml of distilled ethanol.
Specimen preparation
Mild steel specimens of composition C (0.2 %), Mn (1 %), P (0.03 %), S (0.02 %),
and Fe (98.75 %) were used. The steel specimens with an exposed area of 1 cm2
were used for electrochemical studies.
Fig. 3 Polarization curves of mild steel corrosion in a 0.5 N, b 1 N, c 1.5 N, d 2 N HCl in absence andpresence of different concentrations of P. guajava alcohol extract at 30 �C
Electroanalytical studies on the corrosion inhibition behaviour
123
Medium
The medium for the study was made using reagent grade HCl (Merck, Germany)
and distilled water. All tests were performed in aerated medium at room temperature
and atmospheric pressure.
Electrochemical measurements
The electrochemical studies were made using a three-electrode cell assembly at room
temperature. Mild steel of 1 cm2 exposed surface area was the working electrode.
Platinum sheet with 1 cm2 surface area was used as the auxiliary electrode and
saturated calomel electrode as the reference electrode. All the electrochemical
measurements were carried out using a Gill AC computer controlled work station
(model no: 1475; ACM, UK). Prior to the electrochemical measurements, a
stabilization period of 60 min was allowed, to attain a stable value of Ecorr [9].
Table 1 Polarization data for mild steel corrosion in different concentrations of HCl without and with
P. guajava water extract
Acid
concentration
(N)
Inhibitor
concentration
(ml)
-Ecorr
(mV)
ba
(mv/dec)
bc
(mv/dec)
Icorr
(mA cm-2)CR
(mm/year)
%IE
0.5 Blank 443.20 108.74 156.52 2.31 26.75 –
2 452.93 89.43 193.96 1.04 12.04 55
4 460.76 78.48 129.3 0.37 4.30 83.9
6 458.69 52.69 87.85 0.36 4.18 84.4
8 465.30 54.61 103.72 0.27 3.10 88.4
10 469.40 59.51 105.93 0.25 2.87 89.3
1 Blank 479.15 168.95 228.11 3.37 39.02 –
2 477.03 160.08 225.15 2.89 33.55 14
4 494.85 81.14 149.09 0.56 6.48 83.4
6 510.35 42.95 75.63 0.26 3.00 92.3
8 507.10 60.44 115.56 0.08 0.88 98
10 497.92 71.58 134.86 0.27 3.11 92
1.5 Blank 459.24 56.92 117.78 0.69 8.05 –
2 468.19 49.44 91.04 0.51 5.88 26.8
4 480.49 48.66 82.61 0.45 5.19 35.3
6 474.97 51.40 78.43 0.30 3.53 56.2
8 477.25 29.94 49.57 0.23 2.66 56.9
10 476.53 44.79 83.49 0.14 1.67 79.2
2 Blank 437.40 80.14 232.3 1.49 17.38 –
2 448.90 68.53 134 1.32 15.35 11.7
4 451.00 70.28 367.6 0.88 10.25 41
6 448.50 64.15 150.7 0.74 8.62 50.4
8 454.80 57.36 134.3 0.63 7.33 57.8
10 456.01 57.93 185.6 0.50 5.81 66.4
K. K. Anupama, J. Abraham
123
The linear polarization study was carried out from a cathodic potential -250 mV
versus Ecorr to an anodic potential of ?250 mV versus Ecorr with a scan rate of
1 mV/s. The linear Tafel segments of the anodic and cathodic curves were
extrapolated to corrosion potential to obtain the corrosion current densities using
which inhibition efficiency (IE) was calculated.
EIS measurements were carried out with amplitude of 10 mV in a frequency
range from 10 kHz to 0.1 Hz. The impedance diagrams are given in the form of
Nyquist plots. The charge transfer resistance values were obtained from the
diameter of the semicircles of the Nyquist plots.
Scanning electron microscopy (SEM)
The specimens for surface morphological examination were immersed in acid
containing an optimum concentration of inhibitors and blank solution for 4 h. Then,
they were removed, rinsed quickly with acetone, and dried. The analysis was
Table 2 Polarization data for mild steel corrosion in different concentrations of HCl without and with
P. guajava alcohol extract
Acid
concentration
(N)
Inhibitor
concentration
(ml)
-Ecorr
(mV)
ba
(mv/dec)
bc
(mv/dec)
Icorr
(mA cm-2)
CR
(mm/year)
%IE
0.5 Blank 443.2 108.74 156.52 2.31 26.75 –
2 454.4 84.31 160.96 0.92 10.64 60.2
4 470.1 78.24 169.13 0.57 6.62 75.3
6 464.3 69.73 172.81 0.45 5.17 80.7
8 471.9 63.80 156.62 0.16 1.90 92.9
10 473.6 66.90 157.33 0.13 1.47 94.5
1 Blank 479.1 168.9 228.11 3.37 39.02 –
2 481.4 88.7 195.57 1.87 21.68 44.4
4 465.4 75.49 174.91 0.95 11.05 71.7
6 473.6 77.80 175.75 0.77 9.03 77.1
8 470.2 62.42 154.44 0.37 4.36 89.0
10 482 53.58 140.97 0.18 2.14 94.6
1.5 Blank 459.2 56.92 117.78 0.69 8.05 –
2 490.2 46.20 86.73 0.44 5.49 37.2
4 456.2 48.9 136.38 0.30 3.50 56.5
6 473.3 52.40 133.6 0.19 2.24 72.2
8 458.5 50.10 91.73 0.18 2.06 74.3
10 475.2 43.86 101.6 0.16 0.88 76.6
2 Blank 437.4 80.14 232.39 1.49 17.38 –
2 448.5 61.85 172.20 1.01 11.64 32.9
4 454.1 58.45 513.40 0.93 10.8 37.9
6 445.6 61.95 158.30 0.75 8.75 49.6
8 444.3 59.3 147.30 0.49 5.76 66.8
10 450.4 49.02 203.50 0.25 2.89 83.3
Electroanalytical studies on the corrosion inhibition behaviour
123
performed on a scanning electron microscope (model SU6600, serial no. HI-2102-
0003) at an accelerating voltage 20.0 kV. All micrographs of the specimen were
taken at 9500 magnification.
Atomic force microscopy (AFM)
Mild steel strips of size 4.8 9 1.9 cm2 were used for AFM studies. The specimens
were immersed in blank solution and also in 1 N HCl containing an optimum
concentration of inhibitors, for 4 h. The specimens were cleaned and dried before
conducting AFM studies.
Results and discussion
Potentiodynamic polarization measurements
The potentiodynamic polarization curves for steel corrosion in HCl having different
concentrations, without and with the inhibitor, i.e. P. guajava water and alcoholic
extracts at 30 �C, are shown in Figs. 2 and 3. The corrosion parameters obtained
from polarization curves such as corrosion potential (Ecorr), corrosion current
Fig. 4 Nyquist plots for mild steel corrosion in a 0.5 N, b 1 N, c 1.5 N, d 2 N HCl in the absence andpresence of different concentrations of P. guajava water extract at 30 �C
K. K. Anupama, J. Abraham
123
densities (Icorr), and anodic and cathodic Tafel slopes (ba and bc) are given in
Tables 1 and 2.
IEs were calculated using the equation,
% IE ¼ Icorr � Icorr�Icorr
� 100 ð1Þ
where Icorr and Icorr� are the uninhibited and inhibited corrosion current densities,
respectively.
From Tables 1 and 2, it can be seen that Icorr values are decreasing with
increasing inhibitor concentration, which evidently shows corrosion inhibition.
From Figs 2 and 3, it is evident that P. guajava extracts retard both cathodic and
anodic processes, which is also supported by the data given in Tables 1 and 2. Both
ba and bc values have changed, and it can be seen that there is no regular
displacement pattern in the Ecorr values which shows that both the inhibitors act as
mixed type. According to Ferreira and others [24, 25], if the displacement in
corrosion potential is more than 85 mV with respect to the corrosion potential of the
blank, the inhibitor can be seen as a cathodic or anodic type [26].
Fig. 5 Nyquist plots for mild sample corrosion in a 0.5 N, b 1 N, c 1.5 N, d 2 N HCl in the absence andpresence of different concentrations of P. guajava alcohol extract at 30 �C
Electroanalytical studies on the corrosion inhibition behaviour
123
Electrochemical impedance spectroscopy
The corrosion behavior of steel in HCl media with different concentrations was also
studied using the EIS technique. Nyquist plots, as can be seen from Figs 4 and 5, are
not perfect semicircles which may be explained as the result of surface
inhomogeneity. The impedance spectra exhibit a single semicircle for a particular
concentration. The diameter of the circle increases with the increase in inhibitor
concentration. The single semicircle indicates that the charge transfer takes place at
the electrode/solution interface, and corrosion of mild steel is increased by the
charge transfer process.
From Tables 3 and 4, it can be seen that Rct values increase with the increase in
inhibitor concentration, showing that the mild steel surface is protected by the
inhibitor. Cdl values show an opposite trend, i.e. a decrease with increasing
thickness of the protective layer formed on the mild steel surface [15]. The
Table 3 Electrochemical impedance data for mild steel corrosion in different concentrations of HCl in
absence and presence of guava–water extract
Acid
concentration (N)
Inhibitor
concentration
(ml)
Rct (X cm2) Cdl
(lF/cm2)
Icorr
(mA cm-2)
CR
(mm/year)
%IE
0.5 Blank 8.03 537 3.24 37.65 –
2 21.12 378 1.23 14.32 61.9
4 30.71 196 0.84 9.84 73.9
6 43.56 185 0.59 6.94 81.6
8 47.17 91.3 0.55 6.41 82.9
10 66.05 81.9 0.39 4.57 87.8
1 Blank 6.54 719 3.98 46.18 –
2 7.55 358 3.45 40.05 13.4
4 35.43 147 0.74 8.53 81.5
6 96.36 143 0.27 3.13 93.2
8 228.1 59.7 0.11 1.33 97.1
10 74.49 138 0.35 4.05 91.2
1.5 Blank 7.91 452 3.29 38.22 –
2 10.80 320 2.41 28.00 26.8
4 12.32 166 2.11 24.54 35.9
6 17.53 220 1.48 17.25 54.9
8 35.66 95.9 0.73 8.49 77.8
10 43.07 13.3 0.61 7.02 81.6
2 Blank 7.88 468 3.31 38.34 –
2 8.91 354 2.93 33.94 11.5
4 13.33 154 1.96 22.68 40.9
6 15.36 275 1.69 19.68 48.7
8 17.99 216 1.45 16.81 56.2
10 22.02 170 1.18 13.73 54.2
K. K. Anupama, J. Abraham
123
maximum IE obtained for both P. guajava water extract and alcohol extract reaches
more than 90 %. It can be seen that these results are in agreement with those
obtained from polarization studies.
IEs were calculated using the equation,
%IE ¼ Rct� � Rct
Rct
� 100 ð2Þ
where Rct and Rct� are the charge transfer resistances in the absence and presence of
inhibitors, respectively.
Observing the results obtained from electrochemical studies, it may be assigned
that the IE increases gradually with the addition of each 2 ml of the extracts up to
the highest concentration of the extracts used, i.e. 10 ml, and that even at the lowest
inhibitor concentration, i.e. 2 ml of the extract, there is considerable IE. Thus,
P. guajava leaves have proven to be a good inhibitor against mild steel corrosion in
HCl. An important fact to be noted is that the quantity of P. guajava leaves used to
Table 4 Electrochemical impedance data for mild steel corrosion in different concentrations of HCl in
absence and presence of guava–alcohol extract
Acid concentration
(N)
Inhibitor concentration
(ml)
Rct
(X cm2)
Cdl
(lF/cm2)
Icorr
(mA cm-2)
CR
(mm/year)
%IE
0.5 Blank 8.03 537 3.24 37.65 –
2 17.27 378 1.51 17.51 51.6
4 40.85 196 0.64 7.4 79.5
6 44.85 185 0.58 6.78 81.2
8 149.9 91.3 0.17 2.01 94.4
10 164 81.9 0.16 1.84 94.9
1 Blank 6.54 719 3.98 46.18 –
2 12.63 388 2.06 23.94 48.2
4 23.81 183 1.09 12.7 72.5
6 33.67 150 0.77 8.98 80.6
8 50.74 117 0.51 5.95 87.1
10 105.50 84.6 0.25 2.86 93.8
1.5 Blank 7.91 452 3.29 38.20 –
2 14.79 228 1.76 20.40 46.5
4 22.81 161 1.14 13.20 65.3
6 29.69 151 0.87 10.10 73.4
8 33.66 176 0.77 8.90 76.5
10 41.37 106 0.63 7.30 80.9
2 Blank 7.88 468 3.31 38.34 –
2 11.28 306 2.31 26.80 30.1
4 12.63 212 2.06 23.90 37.7
6 16.04 223 1.62 18.80 50.8
8 22.4 197 1.16 13.40 64.9
10 34.6 130 0.75 8.73 77.2
Electroanalytical studies on the corrosion inhibition behaviour
123
prepare the extract is very small in the whole volume of the solvent (about 2.5 g in
500 ml of double-distilled water and distilled ethanol). The results obtained also
show that the P. guajava alcohol extract exhibits better inhibitive capacity than the
P. guajava water extract, which may be attributed to the nature of the substances
extracted with the solvents [27].
Adsorption studies
Adsorption isotherms provide information regarding the mode of inhibition on the
metal surface. The adsorbed layer combats the action of the corrosive media (HCl)
and enhances the protection of the metal surface [8]. Frequently used isotherms are
the Langmuir, Temkin and Frumkin isotherms. The dependence of h (degree of
surface coverage) as a function of inhibitor concentration was graphically tested for
these isotherms. The best fit was obtained for the Frumkin adsorption isotherm, for
both the inhibitors, with the correlation coefficient (R2) value close to unity (Figs. 6,
7).
The Frumkin isotherm equation (Eq. 3) is obeyed when a plot of log [h/C (1 - h)]
versus h produces a straight line with the slope equal to 2a
0.3
0.4
0.5
0.6
0.7
0.8
0.9
1.0 R2=0.98653lo
g{ θ
/c(1
-θ)}
θ
-1.0
-0.5
0.0
0.5
1.0
1.5
2.0 R2=0.97803
log
{θ/c
(1- θ
)}
θ
-0.4
-0.2
0.0
0.2
0.4
0.6
0.8R2=0.99866
log
{θ/c
(1-θ
)}
θ
0.60 0.65 0.70 0.75 0.80 0.85 0.90 0.0 0.2 0.4 0.6 0.8 1.0
0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 0.1 0.2 0.3 0.4 0.5 0.6 0.7
-0.8
-0.6
-0.4
-0.2
0.0
0.2
0.4
R2=0.98783
log
{θ/c
(1-θ
)}
θ
(a) (b)
(c) (d)
Fig. 6 Frumkin adsorption isotherms for mild steel in a 0.5 N, b 1 N, c 1.5 N, d 2 N HCl with differentconcentrations of P. guajava water extract
K. K. Anupama, J. Abraham
123
logh
Cð1� hÞ ¼ 2:303logKFrum þ 2ah ð3Þ
where a is the lateral interaction term describing the molecular interaction in the
adsorbed layer, KFrum is the desorption–adsorption equilibrium constant, and C is
the concentration of the inhibitor. The Frumkin adsorption theory assumes the
adsorption of a multimolecular layer where there is an adsorbate–adsorbent inter-
action. And this fact is almost confirmed from the best fitting isotherm (Figs. 6, 7)
obtained for the P. guajava extract adsorption on mild steel.
The Frumkin adsorption isotherm also accounts for the inhomogeneity on the
surface of the steel specimen, which is an advantage over the Langmuir adsorption
isotherm in explaining the equilibrium reactions.
Scanning electron microscopy (SEM)
Scanning electron microscope images were recorded (Fig. 8) to establish the
interaction of inhibitor molecules with the metal surface. Figure 8a indicates the
finely polished characteristic surface of the mild steel and shows some scratches
0.0
0.2
0.4
0.6
0.8
1.0
1.2
1.4 R2=0.97121
log
{θ/c
(1- θ
)}
θ
0.0
0.2
0.4
0.6
0.8
1.0
1.2
R2=0.97486
log
{ θ/c
(1-θ
)}
θ
-0.1
0.0
0.1
0.2
0.3
0.4
0.5
0.6
0.7 R2=0.9986
log
{θ/c
(1-θ
)}
θ
0.5 0.6 0.7 0.8 0.9 1.0 0.4 0.5 0.6 0.7 0.8 0.9 1.0
0.45 0.50 0.55 0.60 0.65 0.70 0.75 0.80 0.85 0.3 0.4 0.5 0.6 0.7 0.8
-0.4
-0.2
0.0
0.2
0.4
0.6R2=0.99864
log
{θ/c
(1-θ
)}
θ
(a) (b)
(c) (d)
Fig. 7 Frumkin adsorption isotherms for mild steel in a 0.5 N, b 1 N, c 1.5 N, d 2 N HCl with differentconcentrations of P. guajava alcohol extract
Electroanalytical studies on the corrosion inhibition behaviour
123
which must have arisen during polishing. Figure 8b reveals that the immersed
specimens were highly damaged in the presence of 1 N HCl, due to direct acid
attack. Figure 8c, d shows the formation of a protective film over the metal surface
by P. guajava alcohol and water extracts, respectively. These images well exhibit
the better IE of the P. guajava alcoholic extract when compared to the aqueous one,
agreeing with the results of the electrochemical measurements.
Atomic force microscopy (AFM)
AFM is a powerful technique for surface morphological studies providing
information about the influence of inhibitors on corrosion at the metal–solution
interface. The three-dimensional AFM images are given in Fig. 9a–d. Figure 9a
displays the surface topography of an uncorroded metal surface for which the
average roughness value (Ra) was obtained as 16 nm. Figure 9b displays the
corroded metal surface showing severe damage due to exposure to acid, the Ra value
for which was obtained as 41 nm. Figure 9c, d displays the steel surfaces which
were immersed in 1 N HCl containing optimum concentrations of P. guajavaalcohol and water extracts, respectively. The Ra values obtained for P. guajavaalcohol inhibitor and P. guajava aqueous inhibitor are 12 and 21 nm, respectively,
which are lower than those obtained for the steel surface in the uninhibited
Fig. 8 SEM images of a mild steel, b mild steel in 1 N HCl, c mild steel in 1 N HCl ? 10 ml P. guajavaalcohol extract, and d mild steel in 1 N HCl ? 10 ml P. guajava water extract
K. K. Anupama, J. Abraham
123
environment. This clearly shows that a compact protective film of the inhibitor is
formed on the metal that keeps the surface smooth.
Conclusion
• Psidium guajava acts as a better inhibitor for corrosion of mild steel in HCl
medium. With increasing concentration of the inhibitor, the IE also increases.
• Impedance measurements revealed the increase in charge transfer resistance and
the decrease of double layer capacitance with increasing inhibitor concentration.
• Polarization data suggest that P. guajava acts as a mixed-type inhibitor.
• Adsorption studies revealed that the adsorption pattern of P. guajava inhibitor
obeys the Frumkin adsorption isotherm, suggesting a multimolecular layer
adsorption.
• SEM images shows that a protective layer is formed on the metal surface by the
inhibitor molecules.
Fig. 9 AFM images of a mild steel, b mild steel in 1 N HCl, c mild steel in 1 N HCl ? P. guajavaalcohol extract and d mild steel in 1 N HCl ? P. guajava water extract
Electroanalytical studies on the corrosion inhibition behaviour
123
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