International Journal of Mechanical Engineering and Technology (IJMET)

Volume 9, Issue 11, November 2018, pp. 829–841, Article ID: IJMET_09_11_084
Available online at http://www.iaeme.com/ijmet/issues.asp?JType=IJMET&VType=9&IType=11
ISSN Print: 0976-6340 and ISSN Online: 0976-6359

© IAEME Publication Scopus Indexed

EVALUATION OF GROUNDNUT LEAVES

EXTRACT AS CORROSION INHIBITOR ON
MILD STEEL IN 1M SULPHURIC ACID USING
RESPONSE SURFACE METHODOLOGY (RSM)
Olawale, O.*
Department of Chemical Engineering, Landmark University, Omu-Aran, Kwara State, Nigeria.

Idefoh, C. K
Department of Chemical Engineering, Landmark University, Omu-Aran, Kwara State, Nigeria.

Ogunsemi, B.T
Department of Mechanical Engineering, Landmark University, Omu-Aran,Kwara,state,Nigeria.

Bello, J. O
Department of Chemical Engineering, Landmark University, Omu-Aran, Kwara State, Nigeria.
*coressponding author

ABSTRACT
The inhibiting effects of Groundnut Leaves Extract (GLE) on corrosion of Mild Steel
in 1M H2SO4 acidic media was investigated in this study. The effect of the concentration
of inhibitor (0.2 - 1.0 g/l), time (3 – 5 days) and temperature (40 60 ) on corrosion
rate and Inhibition efficiency were investigated using Response Surface Methodology
(RSM). The Phytochemical analysis of the GLE was performed; the result showed that
organic constituents were present which made the Groundnut Leaves Extract a good
inhibitor. Mathematical models were derived for the groundnut leaves extract. The
optimum conditions obtained were temperature 49.72 OC, time 5 days and inhibitor
concentration of 0.29 g/l while the optimum Inhibition Efficiency at this optimum
condition was predicted to be 85.9%. The outcome of the ANOVA test confirmed a
confidence level of 95%. Gravimetric experiment was carried out at these optimum
conditions to validate the predicted optimum values. The obtained experimental value of
86.3% agreed closely with that obtained from the regression model. The micrographs
result of Scanning Electron Micrographs analysis showed that passive layer of film was
formed on the surface. This study has revealed that Groundnut Leaves Extract is a good
inhibitor for the corrosion of Mild steel in 1M H2SO4 solution.
Keywords: Corrosion Inhibition, Groundnut Leaves Extract, Inhibition Efficiency,
Optimization.

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 Olawale, O, Idefoh, C. K, Ogunsemi, B.T and Bello, J. O

Cite this Article Olawale, O, Idefoh, C. K, Ogunsemi, B.T and Bello, J. O, Evaluation of
Groundnut Leaves Extract as Corrosion Inhibitor on Mild Steel in 1m Sulphuric Acid Using
Response Surface Methodology (Rsm), International Journal of Mechanical Engineering
and Technology, 9(11), 2018, pp. 829–841.
http://www.iaeme.com/IJMET/issues.asp?JType=IJMET&VType=9&IType=11

1. INTRODUCTION
Corrosion is the destruction of material by a reaction with its environment. The petroleum
industry is one of the most affected by corrosion due to the presence of numerous corrosive
substances in the crude oil, which affect equipment and pipelines from the extraction of crude oil
to the transportation of final products [1].
Corrosion Inhibitors are chemicals that react with a metallic surface or the environment the
surface is exposed to; resulting in giving the surface a certain level of protection [2]. Inhibitors
slow corrosion processes by either increasing the anodic or cathodic polarization behavior [3]
reducing the diffusion of ions to the metallic surface or increasing the electrical resistance of the
metallic surface [4]. This practice have exploration has been centered on the utilization of green
chemistry; which incorporates plant extracts that contain many organic compounds such as amino
acids, alkaloids, pigments and tannins used as green alternatives for the toxic and hazardous
compounds. Furthermore, due to the biodegradability, eco-friendliness, low cost and easy
availability of the extracts of some common plants and plant products they have been studied as
corrosion inhibitors for various metals and alloys under different environmental conditions. The
environment may be liquid, gas or mixture of solid and liquid [5]
The use of inhibitors has been widely explored to decrease corrosion of mild steel used in
acidic environments because they form various types of films in several ways; by adsorption, by
the formation of bulky precipitates, and by the formation of a passive layer on the metal surface.
The inorganic salts and organic compounds, which are proven as good inhibitors have limited
solubility and toxic properties, because they contain nitrogen, sulfur or oxygen. Aware of that,
researchers orient their corrosion inhibition studies toward human health and safety consideration
awareness. These environmentally friendly inhibitor sources are natural products which are non-
toxic, cheaply processed, biodegradable and readily available in plenty and are sometimes
regarded as agro-waste. In this regard, plant-based inhibitors such as Red Peanut skin [6] Jatropha
stem [7]; Rice husk [8], Bitter Kola Stem [9] and Pawpaw leaves [10] among several others have
recorded varied levels of success; research efforts are still ongoing to search for other green
inhibitor alternatives. This present work is tailored to the use of Groundnut Leaves Extract as
eco-friendly source to produce green corrosion inhibitor for mild steel. Furthermore, using this
agricultural waste will provide two advantages to the environment. The volume of agro waste
could be reduced and the low cost inhibitor could be easily produced for reducing the pollution
problems arising from structural steel corrosion. The aim of this research is to determine the
inhibition efficiency of the groundnut leaves extract as a corrosion inhibitor on mild steel in
Sulphuric ( ) solution.

2. EXPERIMENTAL
Response Surface Methodology (RSM) is a statistical tool used to investigate the interaction
between several illustrative variables and one or more response variables. The process of RSM
includes designing of a series of experiment sufficient and reliable measurement of the response
and developing a mathematical model of the second order response surface with the best fittings.
The Software Design Expert (6.0.8) was used to analyze the data.
The mathematical empirical model is defined as:

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 Evaluation of Groundnut Leaves Extract as Corrosion Inhibitor on Mild Steel in 1m Sulphuric Acid
Using Response Surface Methodology (Rsm)

= + + + + +
Where : is the response or dependent variable: and are the independent
variables , , , , , are the regression coefficients. The theory and applications of
RSM are highlighted in the literature [11].

3. EXPERIMENTAL DESIGN
A central composite design of 20 experimental runs which included 3- operating variables was
established for the experiments used for studying the effect of: temperature of the solution, Time
of exposure and Inhibition Concentration of extract on corrosion parameters using GLE.
The Factor levels with the corresponding real values are shown in Table 1 while the Design
Matrix is shown in Table 2 The matrix for the three variables was varied at 3 levels (-1, 0 and
+1). As usual the experiments were performed in random order to avoid systematic error
The following steps in RSM considered for this study
1. Design of experiment using Central Composite Design (CCD) to obtain the points
where the experimental run was performed.
2. Experimental observation of the corrosion inhibition effects of the various factors at
the design points.
3. Obtaining a mathematical model expressing the relationship between the process
factors and the percentage inhibition efficiency.
4. Prediction of the Optimum values of the process for the maximum inhibition
efficiency using RSM.
5. Experimental verification.
The RSM was used to analyze the responses. The ANOVA and graphical analyses of the
inhibition efficiency and corrosion rate were carried out. The mathematical models in terms of
coded factors were obtained. The models in terms of coded factors were used to make predictions
about the response for given levels of each factor. Optimum inhibition parameters were also
obtained.

3.1. Preparation of Mild Steel Coupon

Mild Steel, obtained from the Mechanical Engineering laboratory was cut into Coupons of 2 cm
by 2 cm in dimension with thickness of 0.2 cm and a hole 0.2cm drilled in the middle, cleaned
with emery paper to expose the shiny surface, degreased with acetone to remove any oil
impurities, washed with distilled water and then dried in air and stored in a desiccator., The
coupons were weighed and recorded as the initial weight of the mild steel before being exposed
to the corrosion media containing inhibitor.

3.2. Preparation of Plant Extract

The groundnut leaves (GL) used was collected from Landmark University Teaching and
Research farm and dried for five (5) days under a shield, then grinded to fine powder and kept
for further analysis. For every extraction process conducted 30grams of the ground groundnut
leaves was measured and extracted using the Soxhlet extractor for 4hours using 180g of ethanol.
After extraction, the samples were then re-extracted to remove the ethanol. The filtrates obtained
were be used to prepare inhibitor concentrations in sulphuric ( corrodents.

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 Olawale, O, Idefoh, C. K, Ogunsemi, B.T and Bello, J. O

3.4. Phytochemical Analysis

The Groundnut Leaves Extract (GLE) was first grinded; then subjected to phytochemical analysis
to check the secondary metabolites: alkaloids, flavonoids, tannins, steroids and saponins present.
The result of the phytochemical analysis is shown below in Table 3.

3.5. Weight Loss (gravimetric)

Weight loss measurements was conducted under total immersion using 250 ml capacity beaker
containing prepared solution at 40 to 60 which was maintained in a thermostatic water bath.
The Mild Steel Coupons were weighed and dropped in the corrodent. The coupons were retrieved
with time variables of (3 -5 days); exact Temperature of the solution and the inhibitor
concentrations (0.2 – 1.0 g/l) in extract for each run were followed using the design matrix format
in Table 3. After each exposure time, the mild steel coupons were removed, washed thoroughly
to remove the corrosion product with emery paper, rinsed with distilled water and then dried in
acetone. The mild steel was re-weighed to determine the weight loss, in gram by the difference
of mild steel weight before and after immersion. The corrosion rates ( / ℎ) in the absence
and presence of the studied inhibitors were determined. Weight loss was calculated by finding
the difference between the weight of each coupon before and after immersion;

∆W = (1)
Where is the weight before immersion; is the weight after immersion. While the
corrosion rate ( / ℎ) in absence and presence of inhibitors was calculated using equation (2).
"#
!= $% (2)
Where Δ& is the weight loss (g) after exposure time t (days), A is the area of the specimen
( ) and t is the time of exposure in days, and CR is the corrosion rate at each exposure time.
Inhibition efficiency was calculated as

#* +#,
'(% = #*
× 100 (3)
Where, & and & are the weight loss values in presence and absence of inhibitor,
respectively. A is coupon; t is time of exposure, '( % are the inhibition efficiency.
Morphological observations of the corroded Mild Steel samples were carried out using
Scanning Electron Microscopy (SEM).

4. RESULTS AND DISCUSSION

4.1. Evaluation of Regression Model for Inhibition Efficiency (%I.E)
The correlation between the experimental process variables and the inhibition efficiency was
evaluated using the Central Composite Design (CCD) modeling technique.
The effect of inhibition on inhibition efficiency in 0.1M is presented in Table 4 which
showed the weight loss of the coupons, corrosion rate and inhibition efficiency. It showed that
inhibition efficiency has increased since the concentration of the extract (inhibitor) is not directly
visible in it.
The correlation between the experimental process variables and the inhibition efficiency was evaluated
using the Central Composite Design modeling technique. A polynomial quadratic regression equation of
the form was derived

= + + + / / + + 0 + 1 / + 2 + 3 / + 4 / (4)

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 Evaluation of Groundnut Leaves Extract as Corrosion Inhibitor on Mild Steel in 1m Sulphuric Acid
Using Response Surface Methodology (Rsm)

Where fitted between the response (% inhibition efficiency(Y)) and the process variables:
time ( ), temperature ( ), and inhibitor concentration ( /). The final response equation for in
terms of coded is as given:
= 54.94 + 2.10 10.42 + 2.51 / + 12.95 28.55 + 8.20 / + 4.19
15.79 / + 9.34 / (5)
Furthermore, Table 5 presented the analysis of variance (ANOVA).The degree of freedom
(DF), Fisher test (F-test) and probability values (p-value) are 9, 4.22 and 0.0173 respectively. The
p-value is less than 0.05, which implied that the model is significant. The ANOVA results showed
that the quadratic model is suitable to analyze the experimental data. To develop a statistically
significant regression model, the significance of the regression coefficients was evaluated based
on the p-values. The coefficient terms with p-values more than 0.05 are insignificant and are
removed from the regression model. The analysis in Table 5 showed that the linear, quadratic and
interaction effects of temperature and inhibition concentration are significant model terms. The
model reduces to Equation 6 after eliminating the insignificant coefficients
= 54.94 10.42 28.55 15.79 / (6)
The analysis of variance indicated that the quadratic model was significant and adequate to
represent the actual relationship between inhibition efficiency and the significant model variable
as predicted by small p-value. This means that the model is a good representation of variation in
the experimental data. The adequate correlation between the experimental values of the
independent variable and predicted values further showed the accuracy of the model. The
significant and adequacy of the established model was further collaborated by high value of the
coefficient of determination of 79.17% as shown in Table 5 that gives the reason to conclude
that the model is appropriate.
However; in Table 5, shown as ANOVA for the corrosion inhibition of Mild Steel in
by Groundnut Leaves Extract; the “Pred R- squared” implies that the overall mean is a better
predictor of the inhibition efficiency than the current model. Since “Adeq Precision” measures
the signal to noise ratio; a ratio greater than 4 is desirable and from the ANOVA we have a ratio
of 8.279. Furthermore; Regression Coefficient and significance of Response Surface Quadratic
is shown in Table 6

4.2. Experimental Validation

The optimum level of 85.97%. Predicted by the software was validated, to confirm if significant
or not as seen in Table 6. However; experimental value of 86.30% agreed closely with that
obtained from regression model. Furthermore, Table 7 showed the experimental value, predicted
value with the residual for the 20 experimental runs obtained from the CCD.

Table 6 Optimum parameters for the corrosion inhibition process

Optimum parameters Optimum inhibition efficiency (%)
Inhibitor concentration (g/l) 0.29 85.97
Temperature ( ) 49.72
Time (days) 5

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 Olawale, O, Idefoh, C. K, Ogunsemi, B.T and Bello, J. O

Table 7 Diagnostic case statistics of inhibition efficiency

Coded variables
Run / Experimental value Predicted value Residual
1 -1 0 -1 39.20 51.10 -11.90
2 1 0 -1 86.30 78.50 7.80
3 -1 1 0 15.60 3.21 12.39
4 1 1 -1 42.60 47.36 -4.76
5 -1 0 1 70.60 69.02 1.58
6 1 0 1 17.70 33.27 -15.57
7 -1 1 1 47.50 58.48 -10.98
8 1 1 1 48.20 39.48 8.72
9 -1 0 0 74.70 65.79 8.91
10 1 0 1 73.80 69.99 3.81
11 0 -1 1 54.90 36.81 18.09
12 0 1 0 10.60 15.97 -5.37
13 0 0 -1 57.10 60.63 -3.53
14 0 0 1 81.90 65.65 16.25
15 0 0 0 50.70 54.94 -4.27
16 0 0 0 50.70 54.94 -4.27
17 0 0 0 50.70 54.94 -4.27
18 0 0 0 50.70 54.94 -4.27
19 0 0 0 50.70 54.94 -4.27
20 0 0 0 50.70 54.94 -4.27

4.3. Surface Response Plots for Inhibition on Mild Steel

The interactive effects of the process variables on the IE (%) were studied by plotting a three
dimensional surface curve against any two independent variable, while keeping the other variable
constant. The 3D curves are shown in Fig 1 – Fig 3. It showed in Fig 1 that at a given inhibitor
concentration inhibition efficiency increased with decrease in time, but also decreased with
increase in temperature.
However; Fig 2 showed that inhibition efficiency increases with increase in inhibitor
concentration but decreases with an increase in time
Nevertheless; increase in temperature with increase in inhibitor concentration but decrease in
inhibition efficiency was observed in Fig 3, this could be attributed to the fact that the longer the
metal stay in the acid the more it corrodes

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Evaluation of Groundnut Leaves Extract as Corrosion Inhibitor on Mild Steel in 1m Sulphuric Acid
Using Response Surface Methodology (Rsm)

Figure 1 Effects of time and temperature on inhibition efficiency of GLE on Mild Steelat constant
inhibitor concentration of 0.60g/l

Figure 2 Effects of time and inhibitor concentration on inhibition efficiency of GLE on Mild Steel at
constant temperature 50°C

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 Olawale, O, Idefoh, C. K, Ogunsemi, B.T and Bello, J. O

DESIGN-EXPERT Plot

inhibition efficiency
X = B: temp.
Y = C: inhib. conc

Actual Factor
A: time = 4.00 70
57

e f f.
43

inhibit ion
29
15

1.00
60
0.80
55
0.60
50
C: inhib. conc0.40 45
B: temp.
0.20 40

Figure 3 Effects of temperature and inhibitor concentration on inhibition efficiency of GLE on Mild
Steel at constant time of exposure 4 days.

5. EVALUATION OF REGRESSION MODEL FOR CORROSION RATE

The correlation between the experimental process variables and the corrosion rate was evaluated
using the Central Composite Design (CCD) modeling technique. A polynomial quadratic
regression equation of the form:
= + + + / / + + 0 + 1 / + 2 + 3 / + 4 / (7)
Was used, where fitted between the response (Corrosion rate (Y)) and the process variables:
time ( ), temperature ( ), and inhibitor concentration ( /). The final response equation for in
terms of coded is as given:
= 59.45 11.52 + 23.93 4.65 / 8.58 + 0.17 16.73 / 8.73 +
8.02 / 5.69 / (8)
Table 5 showed: degree of freedom (DF), Fisher test (F-test) and probability values (p-value)
are 9, 7.16 and 0.0025 respectively.
From Table 8, the ANOVA result showed that the quadratic model is suitable to analyze the
experimental data, develop a statistically significant regression model; the significance of the
regression coefficients was evaluated based on the p-values. The coefficient terms with p-values
more than 0.05 are insignificant and are removed from the regression model. The model reduces
to Equation (9) after eliminating the insignificant coefficients
= 59.45 11.52 + 23.93 (9)
The analysis of variance indicated that the quadratic model was significant. This means that
the model is as a good representation of variation in the experimental data. The adequate
correlation between the experimental values of the independent variable and the predicted
variables further showed the adequacy of the model. The significance and adequacy of the
established model was further collaborated by the high value of the coefficient of determination
(! is 86.57% in Table 8; it showed that it is close to the "Adj R-Squared" of 0.7448 as one
might normally expect. Furthermore, since “Adeq Precision” measures the signal to noise ratio;

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 Evaluation of Groundnut Leaves Extract as Corrosion Inhibitor on Mild Steel in 1m Sulphuric Acid
Using Response Surface Methodology (Rsm)

a ratio greater than 4 is desirable and from the ANOVA with a ratio of 10.521 and this therefore
makes the use of groundnut leaves extract as a corrosion inhibitor on Mild Steel in 1M
very effective and the model appropriate.
The analysis in showed that the linear, quadratic and interaction effects of temperature and
inhibition concentration are significant model.

Table 8 ANOVA for the corrosion inhibition of Mild Steel in => ?@A by Groundnut Leaves Extract
ANOVA for Response Surface Quadratic model; corrosion rate
Analysis of variance table [Partial sum of squares]
Degree of P-value
Sum of Mean of
Source freedom F- values
squares squares Prob > F
(DF)
Model 11253.65 9 1250.41 7.16 0.0025 Significant
(time) 1326.41 1 1326.41 7.60 0.0203
(temperature) 5724.53 1 5724.53 32.79 0.0002
/ (inhibitor 216.60 1 216.60 1.24 0.2914
concentration)
202.60 1 202.60 1.16 0.3067
0.081 1 0.081 4.650E-004 0.9832
/ 769.54 1 769.54 4.41 0.0621
609.70 1 609.70 3.49 0.0912
/ 514.56 1 514.56 2.95 0.1168
/ 258.78 1 258.78 1.48 0.2514
Residual 1745.96 10 174.60
Lack of fit 1745.96 5 349.19
Pure error 0.000 5 0.000
Cor. Total 12999.61 19
Std. Dev. 13.21 R- squared 0.8657
Mean 46.88 Adj R- squared 0.7448
C.V% 28.19 Pred. R-squared 0.3858
Press 7984.12 Adeq. Precision 10.521

5.1. Surface Response Plots for corrosion rate on Mild Steel

The interactive effects of the process variables on the corrosion rate were studied by plotting a
three dimensional surface curve against any two independent variable, while keeping the other
variable constant. The 3D curves are shown in Fig 4 – Fig 7 respectively. Fig 4 showed the plot
of predicted versus experimental. It showed that the plots were reasonably distributed near to the
straight line indicating a good relationship between the experimental and predicted values of the
response, and that the underlying assumptions of the analysis were appropriate. It also showed
that the selected quadratic model was adequate in predicting the response variables for the
experimental data. The predicted versus experimental plot gave a linear graph. The graph (3-D
surface plot) in Fig 5 to Fig 7 showed the relationship between the factors and corrosion rate
response of the designed experiment.
Fig 5, showed that corrosion rate increased with increase in temperature and also increased
with increase with time; while Fig 6 showed that corrosion rate decreased with increase in
inhibitor concentration and also increases with an increase in time, as shown in Fig 7, but
decreases with an increase in inhibitor concentration. This assumed physical adsorption.

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 Olawale, O, Idefoh, C. K, Ogunsemi, B.T and Bello, J. O

Furthermore; the Groundnut Leaves Extract obeys the mechanism of physiorption with the
inhibition efficiency increasing with increase in inhibition concentration but decreases with time
and temperature.

Figure 4 Plot of Predicted values versus the Actual Experimental values for corrosion rate of GLE on
Mild Steel

Figure 5 Effects of time and temperature on corrosion rate of GLE on Mild Steel

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 Evaluation of Groundnut Leaves Extract as Corrosion Inhibitor on Mild Steel in 1m Sulphuric Acid
Using Response Surface Methodology (Rsm)

Figure 6 Effects of time and inhibitor concentration On corrosion rate of GLE on Mild Steel at Constant
temperature’

Figure 7 Effects of temperature and inhibitor concentration on corrosion rate Rate of GLE

6. DISCUSSION ON SCANNING ELECTRONS MICROGRAPHS (SEM)

ANALYSIS
The micrographs revealed that in the absence of inhibitor, the surface was strongly damaged, due
to corrosion while in the presence of inhibitor there was a much smaller damage on the surface
as shown in Fig 8. This was attributed to the formation of a good protective film on the Mild Steel
surface. Furthermore, in Fig 9, it was observed that the damage was very minute which showed
a better protective film

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 Olawale, O, Idefoh, C. K, Ogunsemi, B.T and Bello, J. O

Figure 8 The SEM micrographs for mild steel In 1.0M in the absence of corrosion Inhibitor (blank)

Figure 9 SEM micrograph of Mild steel mild steel exposed to 1.0M with corrosion inhibitor 0.29. G/l
extract

Figure 10 SEM micrographs for mild steel exposed to 1.0M with corrosion inhibitor GLE;
validated after prediction.

7. CONCLUSION
Groundnut Leaves Extract (GLE) shows an outstanding ability to provide improved corrosion
resistance of Mild Steel in acidic medium (1.0M of H2SO4). An optimal operating condition for
inhibition efficiency of 85.9% was observed. The validation of the model was carried out at this
optimal process conditions; time: 5 days, temperature: 49.72 and inhibitor concentration:
0.29 g/l to validate the predicted optimum value.
The experimental value of 86.3% agreed closely to that gotten from the Response Surface
Methodology. The inhibitive ability of the GLE depends on protective oxide layer formed on the

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 Evaluation of Groundnut Leaves Extract as Corrosion Inhibitor on Mild Steel in 1m Sulphuric Acid
Using Response Surface Methodology (Rsm)

mild steel by adsorption due to the presence of alkaloids, tannins, and steroids. It can be
concluded be used to reduce metal dissolution in acidic media

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