Optimization Study of Eggshell Extract as Inhibitor of Mild Steel Corrosion in a 30 wt% NaCl Solution

Oyewole, O.; Adeoye, J. B.; Lucas, M.; Olugbemi, W.; Oyewole, O.; Adeoye, J. B.; Lucas, M.; Olugbemi, W.

doi:10.4152/pea.2024420204

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Portugaliae Electrochimica Acta

versão impressa ISSN 0872-1904

Port. Electrochim. Acta vol.42 no.2 Coimbra abr. 2024 Epub 31-Jan-2024

https://doi.org/10.4152/pea.2024420204

Research Article

Optimization Study of Eggshell Extract as Inhibitor of Mild Steel Corrosion in a 30 wt% NaCl Solution

O. Oyewole¹²

J. B. Adeoye²

M. Lucas¹²

W. Olugbemi¹³

^¹SGD9: Industry, Innovation and Infrastructure, Landmark University,Omu- Aran, Kwara State, Nigeria

^²Department of Chemical Engineering, College of Engineering, Landmark University,Omu- Aran, Kwara State, Nigeria

^³Chemical Engineering Department, Abubakar University, Zaria, Nigeria

Abstract

Corrosion is a major challenge faced in industries, which has to be addressed by using inhibitors. The aim of this study was to investigate ESE as I of MS in a 30 wt% NaCl solution. ESE was subjected to Pc analysis, to identify the presence of active ingredients that would create a good CI. CI of ESE at different C was investigated using WL, PDP, SEM, FTIR and EDXS techniques, to characterize MS samples. The best process level from the experimental design was observed at T of 24.4 ºC, IT of 6 days and ESE C of 0.4 g/L, with IE (%) of 95.5 %. The presence of metabolites in ESE was confirmed by Pc analysis, which suggested the extract was a good I. Results from PDP and WL techniques were in good agreement. SEM, FTIR and EDS data revealed that the optimal process level produced more protective film on the MS surface. It was concluded that ESE acted as a good and environmentally friendly I.

Keywords: CR; EDXS; FTIR; IE (%); optimization; PDP; SEM; WL

Introduction

The increase in corrosion costs has brought about major financial problems to oil, refinery and petroleum industries, which has fostered research for I that are also eco-friendly ¹. Corrosion is the spontaneous oxidation of most metals. It causes metals and alloys deterioration or destruction by chemical or electrochemical means ². Acids and chlorides are among the main sources of MS corrosion, which is a major concern in academia and industry. Furthermore, in industries like gas production and offshore oil, seawater environments are frequently used. While corrosion is most commonly associated with metals, it affects all kinds of materials. MS is a popular structural material in sugar, petrochemical, brewery, agricultural, paper, textile and marine industries, for making reaction vessels, pipes and tanks ³, since it is cheap and has usable properties. It has a carbon content of up to 0.25%, among other elements, which allows its use in several products, such as structural beams, automobile bodies, kitchen appliances and cans treatment ⁴. The only concern for MS is its low resistance against corrosion, particularly in acidic/saline environments. Over the years, efforts have been made to develop effective organic I in various corrosive conditions, which generally have O, N and S heteroatoms that have higher basicity and electron density. The active centres for the adsorption process onto the metal surface are O, N, P and S. IE (%) is commonly measured in the following order: O < N < S < P ⁵. Researchers are still searching for the best and most cost-effective I. Most natural-based I are environmentally safe chemicals that can be discarded ⁶. Various plant extracts/animal wastes are able to reduce corrosion with promising efficacy. Some of them are: Mangifera indica⁷^,²⁵; Eucalyptus LE ⁸; Mangifera ficus tikoua LE ⁹; Saraca ashoka aqueous seed ¹⁰; Tinospora crispa extract ¹¹; Bitter kola leaf ¹²; Gentiana olivieri extracts ¹³; calcinated ES ¹⁴; Mango extract ¹⁵; Luffa cylindrica LE ¹⁶; Dioscorea septemloba¹⁷; Pterocarpus santalinoides LE ¹⁸; Pomegranate peel plant extracts ¹⁹; Paederia Foetida LE ²⁰; Katemfe LE ²¹; CNE ²²; Corchorus Olitorus LE ²³; and Ficus extrasperata extract ²⁴.

This research was tailored to use ES for preventing corrosion, because it is a readily available and eco-friendly waste. The goal of the study was to optimize ESE as I on MS in a 30 wt% NaCl solution.

Materials and methods

MS preparation

MS employed in this experiment came from the mechanical workshop at Landmark University in Omu-Aran, Kwara State, Nigeria. MS dimensions were 2.2 by 1.9 cm, thickness of 0.2 cm, with a 0.1 cm hole drilled in the middle. MS was cleaned with emery paper, in order to expose the shiny surface, thereafter rinsed with distilled water and degreased with acetone, for removing any oil contaminants and then placed in a desiccator.

ESE preparation

ES were provided by Landmark University Pastries and dried for three days. Then, they were crushed and stored for extraction. In each procedure, 35 g ES powder were placed in a Soxhlet extractor with 300 mL ethanol, for 3 h. The solution was then concentrated and used to make the C of ESE in 30 wt% NaCl.

Corrosive medium preparation

The corrosive medium was prepared by adding 300 g NaCl to 1000 mL distilled water.

WL method

A beaker containing the prepared solution in a thermostatic water bath was used to evaluate WL for all the experimental runs predicted by BB design. T ranges used in this study were from 24.1 to 30.6 ºC, in a thermostatic water bath. This range was determined based on a 10-year survey conducted by ²⁴, which revealed that T of seawater in Nigeria fluctuates from 24.1 to 30.6 ºC (https://www.seawatertemperature.com). C of ESE was from 0.4 to 0.8 g/L, and IT was 3-15 days. MS coupons were weighed before and after immersion, using software-generated variations in IT, T and C of ESE, for each run.

Eq. (1) was used to compute WL of MS.

()

where MS weight before and after immersion in 30 wt% NaCl is W_b and W_a, respectively.

CR was calculated using eq. (2).

()

where ∆W is MS coupon WL without and with ESE, t is IT and A is the alloy area.

IE(%) was calculated using eq. (3).

()

Pc analysis

ES were subjected to Pc analysis, in order to identify the presence of some active ingredients that would create a good CI.

Experimental design

Three variables (T, IT and C of ESE) generated 17 experimental runs by BB design. Table 1 shows the experimental ranges (low and high). Table 2 depicted the experimental design interactions.

Table 1: Experimental ranges (low and high).

Name and symbol	Units	Low	High
T = A	℃	24.4	30.6
IT = B	Days	3	15
Amount = C of Extract	(g/L)	0.3	0.8

Table 2: Variables interactions for 17 experimental runs.

Run	T (℃)	IT (days)	C of ESE (g/L)
1	27.5	9	0.6
2	24.4	15	0.6
3	30.6	15	0.6
4	24.4	6	0.4
5	27.5	15	0.8
6	27.5	9	0.6
7	24.4	9	0.8
8	30.6	9	0.8
9	24.4	3	0.6
10	27.5	15	0.4
11	27.5	3	0.4
12	27.5	9	0.6
13	27.5	9	0.6
14	30.6	3	0.6
15	27.5	3	0.8
16	27.5	9	0.6
17	30.6	9	0.4

Surface characterization

FTIR

FTIR analysis was used to assess MS in a 30 wt% NaCl solution: without ESE; with ESE, of highest IE (%) (as determined by the experimental design); and via optimal process levels (validated).

SEM

SEM technique was employed to study MS morphology and best process variables in a 30 wt% NaCl solution: without ESE; with ESE at the highest IE(%) (as determined by the experimental design); and via optimal process levels (validated).

EDS

EDS revealed MS elemental components in a 30 wt% NaCl solution: without ESE; with ESE, at its highest IE(%) (as determined by the experimental design); and via optimal process levels (validated).

Electrochemical techniques

PDP study

A potentiostat was used to measure PDP plots for MS specimens in 30 wt% NaCl with various C of ESE. A magnetic stirrer was used to keep the test solution at a constant T of 24.4 ºC. After being polished, the samples were degreased with acetone, and rinsed. E_corr extrapolation to the linear component gave I_corr. Steady-state OCP was accomplished by determining the electrochemical system unchanged at the IT end. Furthermore, to obtain PDP data, the V was from -250 to +250 mV, at a SR of 1 mV/s.

Results and discussion

Discussion of Pc analysis results

ESE is a powerful CI, since it contains proteins, which are a type of amino acid, which backed up findings from ²²^,²⁵. Pc analysis results are shown in Table 3.

Table 3: Results of Pc analysis.

Components	Percentage
N	0.93%
Protein	5.79%
Fat	1.5%
Moisture content	0.5%
Ash	90%

Results of WL measurements

Tables 4-6 show the results of experiments generated with BB design. The best process level was observed in experimental run 4 with: IT of 9 days; T of 24.4 ºC, C of ESE at 0.4 g/L; and IE(%) of 95.65%. Furthermore, lowest CR was also found in experiment run 4.

Table 4: Results from the experimental runs with WL response.

Run	T (ºC)	IT (days)	C of ESE (g/L)	WL (g)
1	27.5	9	0.6	0.004
2	24.4	15	0.6	0.013
3	30.6	15	0.6	0.009
4	24.4	6	0.4	0.002
5	27.5	15	0.8	0.005
6	27.5	9	0.6	0.004
7	24.4	9	0.8	0.013
8	30.6	9	0.8	0.007
9	24.4	3	0.6	0.005
10	27.5	15	0.4	0.006
11	27.5	3	0.4	0.01
12	27.5	9	0.6	0.004
13	27.5	9	0.6	0.004
14	30.6	3	0.6	0.004
15	27.5	3	0.8	0.005
16	27.5	9	0.6	0.004
17	30.6	9	0.4	0.008

Table 5: Results from the experimental runs with CR response.

Run	T (ºC)	IT (days)	C of ESE (g/L)	CR g/cm²/days
1	27.5	9	0.6	0.0015873
2	24.4	15	0.6	0.0003095
3	30.6	15	0.6	0.0002142
4	24.4	6	0.4	3.3333E05
5	27.5	15	0.8	0.0001190
6	27.5	9	0.6	0.0015873
7	24.4	9	0.8	0.0001444
8	30.6	9	0.8	0.0002777
9	24.4	3	0.6	0.0001666
10	27.5	15	0.4	0.0001428
11	27.5	3	0.4	0.0011904
12	27.5	9	0.6	0.0015873
13	27.5	9	0.6	0.0015873
14	30.6	3	0.6	0.0047619
15	27.5	3	0.8	0.0005952
16	27.5	9	0.6	0.0015873
17	30.6	9	0.4	0.0003174

Table 6: Results from the experimental runs with θ and IE response.

Run	T (ºC)	IT (days)	C of ESE (g/L) (g/L)	θ	IE (%)
1	27.5	9	0.6	0.333	33.3
2	24.4	15	0.6	0.200	20
3	30.6	15	0.6	0.573	57.333
4	24.4	6	0.4	0.953	95.333
5	27.5	15	0.8	0.667	66.66677
6	27.5	9	0.6	0.333	33.3
7	24.4	9	0.8	0.560	56
8	30.6	9	0.8	0.633	63.333
9	24.4	3	0.6	0.573	57.333
10	27.5	15	0.4	0.666	66.667
11	27.5	3	0.4	0.713	71.333
12	27.5	9	0.6	0.333	33.3
13	27.5	9	0.6	0.333	33.3
14	30.6	3	0.6	0.573	57.333
15	27.5	3	0.8	0.132	13.2
16	27.5	9	0.6	0.333	33.3
17	30.6	9	0.4	0.466	46.6777

The graph for IE(%) of ESE vs. WL of MS is shown in Fig. 1.

Figure 1: Graph for IE(%) of ESE vs. WL of MS.

Fig. 2 shows graph of ESE IE(%) vs. CR of MS.

Figure 2: Graph for IE(%) of ESE vs. CR of MS.

Statistical analysis on CI of MS in 30 wt% NaCl by ESE

As shown in Table 7, the observed model F-value was 118.45.

Table 7: ANOVA.

Source	Sum of squares	DF	Square	Value	Prob > F
Model	6946.19	9	771.80	118.45 < 0.0001	significant
A	447.46	1	447.46	68.67 < 0.0001
B	433.57		1433.57	66.54 < 0.0001
C	683.87	1	683.87	104.96 < 0.0001
A²	2754.28	1	2754.28	422.71 < 0.0001
B²	1119.02	1	1119.02	171.74 < 0.0001
C²	1110.05	1	1110.05	170.37 < 0.0001
AB	1685.98	1	1685.98	258.76 < 0.0001
AC	66.10	1	66.10	10.14 < 0.0154
BC	2760.49	1	2760.49	423.67 < 0.0001
Residual	45.61	7	6.52
Lack of fit	45.60	1	45.60	34201.50 < 0.0001	significant
Pure error	8.000	6	1.333
Cor. total	6991.80		16
Squared R	0.9935
Pred. squared R	0.9851
Adj. squared R	0.9844

Model terms are significant if the "Prob > F" value is less than 0.0500. The significant model terms are: A, B, C, A², B², C², AB, AC and BC. R² value of 0.9935 showed that the existing model predicted more than 99% response variability. Predicted (0.9851) and adjusted R² (0.9844) were found to be in good agreement. The regression eq, observed in terms of coded and actual factors, is below:

()

where A is T, B is IT and C is ESE content.

Discussion on the 3D surface plots

Figs. 3-8 shows 3D plots for the variables interactions. They confirm the results from ²⁷

Figure 3: Plot of IT vs.T on C of ESE.

Figure 4: Plot of IT vs. C of ESE.

Figure 5: Plot of T vs. C of ESE.

Figure 6: Plot of predicted vs. actual values.

Figure 7: Normal plots residual values vs. Q residuals.

Results of FTIR analysis

Fig. 8 (a-c) shows FTIR spectra of MS immersed in NaCl without inhibitor, with ESE, at its highest IE (%), from result of experimental design, and validated optimal process level, respectively. The bands corresponding to O-H, C-H, O-H, C=N, C-H, O-H and C=C, for MS immersed in NaCl without and with ESE of highest IE (%), are 3598.13, 3210.55, 2527.03, 2350.74, 2000.08, 1426.28 and 1096.32 cm^-1, respectively. MS immersed in NaCl without inhibitor (8a) had transmittance percentage from 62.71 to 39.26, while of highest IE, seen in 8b was from 48.71 to 26.00. The bands at 3500.26, 3200.41, 3098.15, 2043.15, 2000.08, 1325.80, 1100.73 and 750.26 cm^-1 were of optimal process level (8c).

The peak at 3500.26 cm^-1 represents the stretching vibrations of O-H group. 3200.41 cm^-1 is C-H stretching vibration. 3098.15 cm^-1 is C-H symmetric stretching vibration of the CH₂ group connection. 2043.15 cm^-1 is C-N stretching vibration of conjugated ketone or alkene. 2000.80 cm^-1 is C-N symmetric stretching vibration of the CH₂ group connection. 2043.15 cm^-1 is C-N stretching vibration amide. ESE functioned as a mixed I of validated optimal process level, which agreed with findings of ²²^,²⁸.

Figure 8: FTIR spectra of MS: a) without ESE; b) with ESE of highest IE(%); and c) at optimal process level.

Results of SEM analysis

Figs. 9-11 show micrographs of MS immersed in 30 wt% NaCl with and without ESE and the optimal process level (validated experiment), respectively.

Figure 9: SEM micrographs of MS in 30 wt% NaCl (blank).

The blank coupon was highly corroded with cracks, as shown in Fig. 9. Fig.10, which was derived from experimental design, shows that ESE formed layers of protective film, whereas Fig. 11 (validated optimal level) depicted more protective film that was due to ESE adsorption ²⁵.

Figure 10: SEM micrograph of MS in 30 wt% NaCl with ESE of highest IE(%).

Figure 11: SEM micrograph of MS in 30 wt% NaCl with ESE of optimal process level

PDP results

Fig. 12 shows the polarization map of MS in 30 wt% NaCl without and with 0.4, 0.6 and 0.8 g/L ESE. ESE worked as a mixed-type I, as evidenced by E_corr displacement (Table 8), which was less than 85 mV ²⁶^-²⁹.

Figure 12: PDP plot.

Table 8: PDP parameters for MS corrosion in 30 wt% NaCl with ESE.

C (g/L)	E_Corr (V)	I_Corr (A/cm²)	CR (mm/yr)	R_p (Ω)	(_a (v/dec)	(_c (v/dec)
Blank	-0.59747	0.0000011895	0.013822	442.41	0.0020693	0.0029237
0.4	-0.6394	0.000001086	0.012619	435.49	0.0026357	0.0018557
0.6	-0.62701	0.0000010752	0.012494	426.16	0.0020757	0.0021455
0.8	-0.64813	0.000001007	0.011701	412.08	0.0019249	0.0021929

At 0.4 g/L ESE, CR of MS was the lowest and R_p was the highest, indicating that this C was the most effective. Furthermore, it was also seen that ESE addition blocked MS active sites, which slowed down CR. WL and PDP results were in good agreement.

Results of EDXS analysis

The elemental compositions of MS without and with ESE, at its highest IE(%) and via best process variables, were investigated using EDXS, as shown in Fig. 13 (a-c). Fig. 13c shows O heteroatom larger amount, which could be due to Fe oxidation (Fig 13b). It is manifest that corrosion damage was minimised, as depicted in Fig. 13c, which confirmed the result of ³⁰.

Figure 13: EDXS of MS in 30 wt% NaCl: (a) blank; (b) with ESE at its highest IE(%); and (c) with ESE at its optimal IE(%).

Conclusion

The presence of proteins (a type of amino acid), N, fat and moisture content in the Pc analysis confirmed that ESE is an effective I. The results of the experimental design showed ESE highest IE(%) of 95.33%, with IT of 6 days, C of 0.4 g/L and T of 24.4 ºC. PDP results showed that the lowest CR was obtained at experiment 4. Results from PDP and WL techniques were in good agreement. SEM outcomes showed that a more passive film was formed on the MS surface, via the optimal process level, than on that with ESE best IE (%). This confirmed that ESE is an effective and environmentally friendly I.

Acknowledgments

The authors appreciate Landmark University, Omu-Aran, Nigeria, for their support to this research, and provision of facilities.

Authors’ contributions

Olamide Oyewole: wrote the manuscript; interpreted the data; conceived the idea; analyzed the results. John Busayo Adeoye: wrote the manuscript; interpreted the data; analyzed the results. Mark Lucas: performed the experiment and interpreted data; analyzed the results; did the experimental design. Wuraola Olugbemi: analyzed the results.

Abbreviations

BB: Box-Behnken

C: concentration

CNE: chicken nail extract

CR: corrosion rate

DF: degree of freedom

E_corr: corrosion potential

EDXS: energy disperse x-ray spectroscopy

ES: eggshell

ESE: eggshell extract

FTIR: Fourier transform infrared spectroscopy

I: inhibitor

I_corr: corrosion current

IE(%): inhibition efficiency

IT: immersion time

LE: leaves extract

MS: mild steel

NaCl: sodium chloride

OCP: open circuit potential

OPL: optimal process level

Pc: physochemical

PDP: potentiodynamic polarization

Q: studentized range of means divided by the mean estimated standard error for a set of compared samples

R²: determination coefficient

R_p: polarization resistance

SEM: scanning electron microscopy

SR: scan rate

T: temperature

WL: weight loss

Symbols definition

(_a: Tafel anodic slope

(_a: Tafel cathodic slope

θ: degree of surface coverage

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Received: September 21, 2022; Accepted: December 27, 2022

Corresponding author: adeoye.john@lmu.edu.ng

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