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. 2023 Jan 9;8(3):3303–3309. doi: 10.1021/acsomega.2c06639

Inhibitory Capabilities of Sweet Yellow Capsicum Extract toward the Rusting of Steel Rebars in Cement Pore Solution

Mohamed A Deyab †,*, Q Mohsen ‡
PMCID: PMC9878660  PMID: 36713737

Abstract

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The inhibitory capabilities of the sweet yellow capsicum extract (SYCE) toward the rusting of steel rebars in cement pore solution (CPS) were tested employing the electrochemical and mass loss methods. Gallic acid, caffeic acid, p-coumaric acid, ferulic acid, luteolin, and cinnamic acid are the most important constituents in the SYCE extract. By adsorbing them on steel bars, the organic compounds in the CSA extract enable them with an effective mixed-type inhibition, suppressing both anodic and cathodic procedures. At 300 ppm, the highest performances were 95.3 and 97.5% utilizing mass loss and electrochemical approaches, respectively. The activation energy for the corrosion process is greatly increased by the addition of the SYCE extract, going from 13.2 kJ mol–1 (blank solution) to 30.0 kJ mol–1 (300 ppm SYCE extract). The physical adsorption actions of the SYCE extract are described by the Freundlich equilibrium constant’s smallest value, which is 0.074 ppm–1. Many future investigators will be attracted by these discoveries to work relentlessly to uncover the anti-corrosion characteristics of novel plant extracts in the area of concrete additives.

1. Introduction

Concrete with chloride salts contains corrosion inhibitors, which are used in large buildings, coastal buildings, and bridges.1−3 Chlorides have the ability to degrade concrete reinforcing steel.4,5 Inside the alkalinity condition of concrete, ferrous oxide is persistent, but it combines with chloride ions to produce complexes that migrate away from the steel and promote rusting.6 The chloride ions continue to destroy the steel till the passivating oxide film is eliminated.7,8 Corrosion inhibitor compounds chemically impede the corrosion operation.9,10 Inorganic corrosion inhibitors that are commercially accessible include calcium nitrite, sodium nitrite, and phosphates.11 Such inorganic chemicals are hazardous to the environment and are forbidden in many industries.12 Another alternative for steel corrosion inhibitors in concrete is to employ organic inhibitors such as alkanolamines and amines, which are commonly used.13,14 Nevertheless, there are certain concerns concerning the miscibility of organic inhibitors and also their harmful and toxic influences on living beings and concrete. Because of the negative effects of inorganic and organic corrosion inhibitors, the usage of plant extracts as corrosion inhibitors has grown significantly during the last two decades.15−18

Harb et al.19 evaluated the use of the olive leaf extract as an eco corrosion inhibitor for reinforced concrete polluted with saltwater. They discovered that the methanol extract provides the highest inhibition (91.9%). Loto et al.20 studied the influence of the Vernonia amygdalina extract on the corrosion response of implanted mild steel rebar in concrete. At 25% concentration, the smallest inhibitor levels were utilized and the maximum inhibition effectiveness of 90.08% was observed. Asipita et al.21 employed a Bambusa arundinacea extract as a corrosion inhibitor. It already has a pore-blocking ability and inhibits variable oxygenation of concrete, which promotes steel corrosion.

Due to worldwide environmental problems, environmental legislation, and public health issues, numerous scientists in the area of anti-corrosion began to work on environmentally acceptable inhibitors in concrete building processes.22,23

We use sweet yellow capsicum extract (SYCE) as an ecologically friendly inhibitor in CPS solutions to increase the corrosion resistance of steel rebars in this article. The primary novelty of this work is to present a new green inhibitor (i.e., SYCE) for steel rebars corrosion in cement pore solution (CPS) and explain its inhibitory effect and processes in order to extend its applicability in the building structural applications. Utilizing electrochemical, mass loss, and surface exploratory tools, the SYCE extract was prepared, characterized, and applied as a corrosion inhibitor for steel rebars in the research work.

2. Experimental Section

2.1. Materials and Solutions

Steel rebar and CPS compositions are presented in Table 1.

Table 1. Steel Rebar and CPS Compositions.

steel rebar composition wt % 0.18C, 0.29Mg, 0.020P, 0.003Si, 0.026Al, 0.029Ni, 0.02Cr and the remaining Fe sources: Egypt. Steel company
CPS composition 4 g/L NaOH, 11.2 g/L KOH, 3.5 g/L Ca(OH)2, 0.5 g/L NaCl, 0.43 g/L Na2SO4, pH = 13.5sources: EPRI Lab. Preparation
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An Egyptian plant company supplied a sweet yellow capsicum powder. At 348 K, 20 g of sweet yellow capsicum powder was refluxed using 100 mL of stocking solutions (60 percent ethanol + 20 percent ethyl acetate + 20 percent distilled H2O) for 3 h. The refluxed solution was then cleaned using a Buchner funnel. The solution then was condensed in a rotating suction evaporator and left to dry in a pressurized drying furnace at 333 K. The largest and most significant constituents of the SYCE extract were identified by liquid chromatography (shimadzu Instruments) and FTIR (PerkinElmer Instruments).

2.3. Corrosion Rate Measurements

The corrosive rate of reinforcing steel in the CPS liquid was estimated using the mass loss and electrochemical methodology in absence/presence of the SYCE extract. For mass loss studies, ASTM G 31–72 standard practice was applied.24 The steel samples (dimension = 1.5 cm × 1.0 cm × 0.3 cm) were submerged for 10 days inside a 100 mL CPS solution in the absence/presence of the SYCE extract.

The rate of corrosion (Wcorr) and the degree protection performance (Pw %) were computed using eqs 1 and 2(25,26)

2.3. 1
2.3. 2

where W1, W0corr and W2,Wcorr are the mass loss and corrosion rate before and after soaking in CPS solution, respectively. Also, S is the steel surface area and t is experiment time.

A three-electrode crystal unit was utilized for electrochemical testing. This experiment employed a Pt strip (counter element), a saturated calomel electrode (SCE, reference element), and a potentiostat/galvanostat (kinds: Gamry 3000). Potential–current graphs were created in specific circumstances (temperature 298 K, scan rate 0.125 mV s–1, potential field ±250 mV vs OCP).

The percent protecting performance (Pj %) was computed using the below equation27

2.3. 3

The corrosion current density in the absence/presence of the SYCE extract is represented by jcorr(0) and jcorr, respectively.

After 24 h of soaking in the solutions, electrochemical impedance spectroscopy (EIS) assays were produced with a 10 mV AC-signal magnitude and a frequency variety of 100 kHz to 10.0 mHz.

The percent protecting performance (ER %) was computed using the below equation

2.3. 4

The charge transfer resistance in the absence/presence of the SYCE extract is represented by RCT0 and RCT0, respectively.

2.4. Surface Morphology Analyses

Surface morphologies of the steel rebar after submerged for 10 days inside a 100 mL CPS solution in the absence/presence of the 300 ppm SYCE extract were investigated using scanning electron microscopy (SEM) and FTIR (PerkinElmer Instruments).

3. Results and Discussion

3.1. SYCE Extract Characterization

The essential chemical components of the SYCE extract were investigated using high performance liquid chromatography (HPLC) analysis (see Figure 1a). The active ingredients for the number of bands in the HPLC graph are shown in Figure 1a. The most essential parts of the SYCE extract are gallic acid, caffeic acid, p-coumaric acid, ferulic acid, luteolin, and cinnamic acid (see Figure 1b).

Figure 1.

Figure 1

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(a) HPLC graph of the SYCE extract and (b) chemical structures of essential parts of the SYCE extract.

Figure 2 shows the FT-IR spectrum of the pure SYCE extract. It contains OH stretching at 3277 cm–1, sym and asym stretching of CH3 groups at 2978, 2937, and 2885 cm–1, C=O stretching groups at 1644 cm–1, CH2 bending at 1460 cm–1, CH3 bending at 1381 cm–1, C–O stretching at 1291, 1080, and 1041 cm–1, C–O–C stretching at 1236 cm–1, C–H out-of-bending at 991 cm–1, and C–H out-of-plane bending and 922 and 836 cm–1.

Figure 2.

Figure 2

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FTIR spectra of the pure SYCE extract.

3.2. Anti-Corrosion Characteristics of SYCE Extract

The mass loss assay is done to determine the Wcorr and Pw % of steel rebar pieces dipped in CPS solution including the SYCE extract. Table 2 contains a list of these parameters. Based on mass loss data, the SYCE extract lowers the corrosion activity of rebar sample dipped in CPS solution. The amount of the SYCE extract has a strong influence on its anti-corrosion efficacy. At the optimal quantity of the SYCE extract (i.e. 300 ppm), the efficiency of the SYCE extract Pw % achieved 95.3%.

Table 2. Corrosion Rate Wcorr and Inhibition Efficiency Pw % Values for the Steel Rebar in CPS Solution in the Presence/Absence of the SYCE Extract at 298 K.

SYCE extract concn ppm Wcorr(μg cm–2 h–1) × 10–3 Pw %
blank 16.4 ± 0.42  
50 9.21 ± 0.36 43.8
100 5.57 ± 0.30 66.0
150 1.98 ± 0.17 87.9
200 1.08 ± 0.15 93.4
300 0.77 ± 0.05 95.3
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The kinetic performance of steel rebar oxidization in CPS medium including the SYCE extract was evaluated using electrochemical experiments. Figure 3 depicts the polarization plot (Tafel form). Table 3 provides polarization factors such as corrosion potential (Ecorr) as well as corrosion current density (jcorr). We observed that using the SYCE extract minimizes jcorr values to extremely small levels (i.e. 0.23 μA cm–2). For all concentrations, the movements in Ecorr values as compared to the blank condition generally lower than 85 mV. This demonstrates that the SYCE extract is a mixed category inhibitor.28,29 The Pj % is shown to grow with increasing SYCE dosage and attain an optimum value (97.3%) at 300 ppm.

Figure 3.

Figure 3

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Polarization plot (Tafel form) for the steel rebar in CPS solution in the presence/absence of the SYCE extract at 298 K.

Table 3. Polarization Parameters and the Corresponding Corrosion Inhibition Efficiency for the Steel Rebar in CPS Solution in the Presence/Absence of the SYCE Extract at 298 K.

SYCE extract concn ppm jcorr(μA cm–2) –Ecorr mV vs SCE Pj %
blank 8.56 360  
50 4.46 345 47.8
100 2.52 332 70.5
150 0.83 313 90.3
200 0.44 305 94.8
300 0.23 281 97.3
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Figure 4 shows the EIS plot (Nyquist form) for the steel rebar in CPS solution in the presence/absence of the SYCE extract at 298 K. The size of the semicircle yielded in the CPS solution was the smallest in Figure 4, and the size expanded as the dosage of SYCE extract increased. Table 4 displays the quantified values of EIS parameters upon fitting.30 The Rct is revealed to be maximum for 300 ppm SYCE extract actually contains CPS solution, followed by 200, 150, 100, and 50 ppm, and without SYCE. Solutions containing the SYCE extract have lower CPEdl (constant phase element) values while having higher Rct values. This is because the nearby dielectric constant has decreased while the electrical double layer width has increased. For 300 ppm of the SYCE extract, the received ER % is 92.7%. The efficiency results from electrochemical analysis and mass loss are consistent between each other.

Figure 4.

Figure 4

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EIS plot (Nyquist form) for the steel rebar in CPS solution in the presence/absence of the SYCE extract at 298 K.

Table 4. EIS Parameters and the Corresponding Corrosion Inhibition Efficiency for the Steel Rebar in CPS Solution in the Presence/Absence of the SYCE Extract at 298 K.

SYCE extract concn ppm RctΩ cm2 CPEdl(F cm–2) ER %
blank 678 2.3 × 10–5  
50 1967 1.4 × 10–5 65.5
100 2235 7.1 × 10–6 69.6
150 4898 3.2 × 10–6 86.1
200 6454 2.6 × 10–6 89.4
300 9340 1.7 × 10–6 92.7
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The SYCE extract’s inhibitory mechanism is based on the fundamental ingredients of the extract as well as the physical connection of various functional groups (see Figure 1b). The additional electron donor groups provided, primarily heteroatoms with conjugated double bonds, better inhibitor derivatives’ anticorrosion performance.31 The anti-corrosion abilities of the SYCE extract operate by producing an adsorbed layer on the steel surface.32 Their effect on the steel surface is based on physical adsorption, which involves the creation of a barrier layer that eliminates water or corrosive ions out from surface.33 The inhibitory activity of the tested SYCE extract was driven by the connection of aromatic ring electrons and p-electrons of OH groups with unoccupied d-orbitals of steel, via which they created an adherent, solid, and homogeneous thin layer on the steel surface.

3.4. Impacts of Temperature and Thermodynamic Calculation

Temperature is a significant component in the study of corrosion inhibition phenomena.34Table 5 depicts the Wcorr and Pw % of steel rebar in CPS solution with and without the SYCE extract (300 ppm) at several temperatures (298–328 K).

Table 5. Mass Loss Data at Different Temperatures for Steel Rebar in CPS Solution in the Presence/Absence of the SYCE Extract (300 ppm).

temperature (K) SYCE extract Wcorr(μg cm–2 h–1) × 10–3 Pw %
298 0 16.4 ± 0.42  
  + 0.77 ± 0.05 95.3
308 0 18.4 ± 0.53  
  + 0.98 ± 0.03 94.6
318 0 22.1 ± 0.43  
  + 1.7 ± 0.22 92.3
328 0 26.6 ± 0.63  
  + 2.2 ± 0.13 91.7
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The findings clearly show that the Wcorr of steel rebar in CPS solution (both control or inhibited) tends to change with temperature. This tendency may be explained by the roughness of the steel rebar surface produced by the higher temperature and also a transform in the adsorption/desorption equilibrium forward into desorption of the SYCE extract from the steel rebar interface.35

As the temperature goes up, the Pw % percent decreases consistently (Table 5), reflecting a physisorption activity.36 Increasing temperatures seemed to have no impact on Pw %, revealing that the SYCE extract/surface interaction is highly stable. The SYCE extract can indeed be considered an acceptable inhibitor, especially at elevated temperatures. The investigation of the Arrhenius (eq 5) and transition state (eq 6) relationships enabled the determination of various variables like activation energy (Ea), enthalpy change (ΔHa), and entropy change (ΔSa) to clarify the oxidation activity and the probable method of SYCE extract adsorption.37,38

3.4. 5
3.4. 6

(R = molar gas constant, N = 6.2022 1023 mol–1, T = temperature, h = 6.6261 10–34 m2 kg s–1, A = pre-exponential constant).

The Arrhenius profile (Figure 5a) was utilized to assess Ea in the presence and without the SYCE extract (300 ppm). The addition of the SYCE extract greatly enhances the Ea from 13.2 kJ mol–1 (blank solution) to 30.0 kJ mol–1 (300 ppm SYCE extract). Steel rebar corrosion in CPS solution is retarded by the addition of the SYCE extract, which has high activation energy. The adsorption of the SYCE extract on the surface of steel rebar increases the size of the double layer, raising the energy gap required to activate the corrosion process.39 This has been attributed to steel rebar molecules’ superior physical sorption.40

Figure 5.

Figure 5

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Arrhenius (a) and transition state (b) plots for steel rebar in CPS solution in the presence/absence of the SYCE extract (300 ppm).

The values of ΔHa and ΔSa were calculated using the transition state profile (Figure 5b). The SYCE extract increases the ΔHa from 10.6 kJ mol–1 (blank solution) to 27.4 kJ mol–1 (300 ppm SYCE extract). The positive value of ΔHa41 signifies that steel rebar oxidation in CPS solution is endothermic. The ΔSa ranged from −151.4 J mol–1 K–1 (blank solution) to −182.2 J mol–1 K–1 (300 ppm SYCE extract). Furthermore, the transition from a negative quantity of ΔSa in the absence of the SYCE extract toward a more negative quantity of ΔSa in the addition of SYCE extract might be compared to diminished disorder during the creation of the activated complex in the presence of the SYCE extract.42

The Freundlich isotherm concept is an adsorption pattern that assumes a multi-layer adsorption operation with adsorbent desorption occurring on a heterogeneous sorbent. This is an approach that is commonly used to yield an interpretation for the adsorption properties of heterogeneous surfaces.43 In this study, we used the Freundlich isotherm (eq 7) to explain the adsorption of the SYCE extract on the steel rebar interface.44

3.4. 7

(θ = Pw %/100, Cinh = SYCE extract, 1/n = Freundlich slope, KF = Freundlich equilibrium constant).

The Freundlich isotherm for the SYCE extract is depicted in Figure 6. The linear correlation (R2) for Figure 6 is significantly nearer to one, confirming that this mode is appropriate for evaluating adsorption tendency.45 Furthermore, the smallest KF value (i.e. 0.074 L/mmol) describes the physical adsorption actions of the SYCE extract.44 The presence of a value of 1/n (1/n = 0.468) between 0 and 1 verifies the remarkable adsorption scenarios.46

Figure 6.

Figure 6

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Freundlich isotherm for adsorption of the SYCE extract on steel rebar in CPS solution at 298 K.

3.3. Examination of the Steel Rebar Surface

Experimental research SEM examinations were supplemented with quantified FT-IR analysis to validate the findings from the electrochemical and mass loss experiments.

In Figure 7a, a SEM surface view of the steel rebar in CPS solution without the SYCE extract reveals that the irregular rusting over a steel surface is highly thick and visible. As shown in the SEM image (Figure 7b), adding 300 ppm of the SYCE extract to CPS solution lowers the level of corrosion on the steel surface.

Figure 7.

Figure 7

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SEM images for steel rebar surface: (a) exposed to blank CPS solution and (b) exposed to CPS solution containing the 300 ppm SYCE extract.

The FT-IR spectra of the SYCE extract and the layer produced on steel rebar in CPS solution containing the SYCE extract are shown in Figures 2 and 8, respectively. The characteristic absorption bands of the SYCE extract can indeed be seen in FTIR spectra of Figure 8. It contains OH stretching (3212 cm–1), sym and asym stretching of CH3 groups (2972 and 2923 cm–1), C=O stretching groups (1637 cm–1), CH2 bending (1454 cm–1), CH3 bending (1376 cm–1), C–O stretching (1286, 1076 and 1040 cm–1), C–O–C stretching (1232 cm–1), C–H out-of-bending (987 cm–1), and C–H out-of-plane bending (829 cm–1). This spectrum displays that O and π-electrons (aromatic ring) may form covalent connections with the surface of steel rebar. When comparing FTIR spectra in Figure 8 to spectra in Figure 2, the position of the O–H and C–H peaks has shifted together low intensity, indicating that these groups interact in the adsorption process.46

Figure 8.

Figure 8

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FT-IR spectra of layer produced on steel rebar in CPS solution containing the SYCE extract.

4. Conclusions

In order to broaden its applicability in the building structural applications, this research introduces a new green inhibitor (i.e. SYCE) for steel rebar corrosion in CPS and explains its inhibitory effect and processes.The most important constituents of the SYCE extract are gallic acid, caffeic acid, p-coumaric acid, ferulic acid, luteolin, and cinnamic acid. At concentrations of 300 ppm, SYCE demonstrated the highest inhibition efficacies, with values of 95.3 and 97.5%, respectively, for mass loss and electrochemical methods. The SYCE extract functions as a combined corrosion inhibitor, slowing both anodic and cathodic reactions, according to Tafel curves. The presence of the SYCE extract significantly increases the activation energy for the electrochemical reactions, increasing it from 13.2 kJ mol–1 (blank solution) to 30.0 kJ mol–1 (300 ppm SYCE extract). The smallest value of the Freundlich equilibrium constant, 0.074 ppm–1, describes the physical adsorption actions of the SYCE extract. SEM and FT-IR surface inspection results support the adsorption of SYCE extract ingredients on steel surfaces. The current findings cleared the path for future efforts to increase corrosion protection efficiency through the use of non-toxic compounds.

Acknowledgments

This work was supported by Taif University Researchers Supporting Project number (TURSP-2020/19), Taif University, Saudi Arabia. The authors gratefully acknowledge the support of the “Egyptian Academy of Scientific Research and Technology”. Also, we are grateful for the help of the Egyptian Petroleum Research Institute.

Data Availability Statement

The data sets used and/or analyzed during the current study are available from the corresponding author on reasonable request.

The authors declare no competing financial interest.

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Associated Data

This section collects any data citations, data availability statements, or supplementary materials included in this article.

Data Availability Statement

The data sets used and/or analyzed during the current study are available from the corresponding author on reasonable request.

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