Materials Today: Proceedings xxx (xxxx) xxx

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Corrosion inhibitory action of leaves of Mussaenda Frondosa Extract on

controlling corrosion of carbon steel in well water
X. Joy Pradeep, J. Sathiyabama ⇑
Department of Chemistry, G.T.N. Arts College, Dindigul 624005, Tamilnadu, India

a r t i c l e i n f o a b s t r a c t

Article history: Environmental friendly inhibitor system MF-Zn2+ was investigated by Gravimetric process. The inhibitor
Received 17 April 2021 system of Mussaenda Frondosa Extract (300 ppm) and Zn2+ ions (50 ppm) offers a better inhibition pro-
Accepted 28 April 2021 ficiency of 96% in well water. Potentiodynamic Polarization analysis expose that this inhibitor system
Available online xxxx
affords a mixed nature of inhibition. AC impedance spectra studies confirmed that the binary system
was effectively coated over carbon steel. The surface morphology of inhibited and uninhibited carbon
Keywords: steel was studied using Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray (EDX)
Mussaenda Frondosa Extract
Spectroscopy was performed to analyze the elemental composition. Fourier-transform infrared
Carbon steel
Corrosion inhibitor
spectroscopy technique was used to analyze any formation of surface layer.
Well water Ó 2021 Elsevier Ltd. All rights reserved.
MF-Zn2+ system Selection and peer-review under responsibility of the scientific committee of the 12th National Confer-
ence on Recent Advancements in Biomedical Engineering.

1. Introduction investigated [10].Ginger extract’s corrosion inhibitive ability on

steel in salt water polluted with sulphide has been reported [11].
The study of an inhibitor to prevent carbon steel corrosion The Polysaccharide extracted from Plantago ovata was applied
becomes more critical owing to its wider application of steam pres- for enhanced anti-corrosion over carbon steel in 1 M Hydrochlori-
sure system in power plants, heat exchangers and boiler tubing [1]. cacid solution [12]. Our study was intended to explore the corro-
In general, the inhibitors study was risky and brutal to the healthy sion inhibition property of Mussaenda Frondosa plant leaves
and larger environment. As a result, researcher put a hard work to extract on the carbon steel in well water. (See Fig. 1.).
extend the research on environmental safe inhibitors, in particular
plant extracts are economical, eco-friendly, renewable sources and
2. Experimental
readily accessible for effective corrosion inhibitors [2,3]. The ability
of rosemary oil to inhibit the corrosion in carbon steel by
2.1. Coupons preparation
hydrochloric acid solution was already explored [4]. Henna has
been used for as an anti-corrosive agent for iron in the hydrochloric
Carbon steel coupons [0.02–0.03% S, 0.06–0.08% P, 0.4–0.5% Mn,
acid [5]. The corrosion-inhibition property of lemongrass (Cymbo-
0.1–0.2% C and the rest iron] exhibiting dimensions of 1.0 cm
4.
pogon citratus) extract in oilfield water on carbon steel was evalu-
0 cm
0.2 cm were rubbed with emery polishing papers of 1/0,
ated by Deyab et al. [6]. The inhibitive performance of Euphorbia
2/0, 3/0, 4/0, 5/0 6/0 respectively, for mirror finishing, It was
falcata extract (EFE) on carbon steel in 1 M HCl was evaluated by
degreased with trichloroethylene, dried and then kept in desiccator
El Bribri et al.[7]. Mangifera indica leaves extracted by ethanol
for preventing them from oxidation by atmospheric moisture. .
are used as corrosion inhibitor for mild steel in 1 M HCl environ-
ment [8]. Cuminum cyminum has been tested and verified as an
2.2. Preparation of Mussaenda Frondosa Extract
environmental-friendly anti-corrosive agent for mild steel in sea
water [9]. The influence of Jatroph stem extract on corrosion
A fine powder of leaves of Mussaenda Frondosa were refluxed
inhibition of the mild steel in sea water environment has been
with ethanol at temperature of 70 °C for a period of 12 h. The crude
extract was acquired with help of rotatory evaporator. In this pre-
⇑ Corresponding author. sent study, the obtained Mussaenda Frondosa (MF) Extract used as
E-mail address: j.sathiyabama@gmail.com (J. Sathiyabama). corrosion inhibitor.

https://doi.org/10.1016/j.matpr.2021.04.498
2214-7853/Ó 2021 Elsevier Ltd. All rights reserved.
Selection and peer-review under responsibility of the scientific committee of the 12th National Conference on Recent Advancements in Biomedical Engineering.

Please cite this article as: X. Joy Pradeep and J. Sathiyabama, Corrosion inhibitory action of leaves of Mussaenda Frondosa Extract on controlling corrosion
of carbon steel in well water, Materials Today: Proceedings, https://doi.org/10.1016/j.matpr.2021.04.498
X. Joy Pradeep and J. Sathiyabama Materials Today: Proceedings xxx (xxxx) xxx

Fig. 1. Structure of Main constituents of Mussaenda Frondosa (MF) Extract.

Table 1 was used as reference electrode, counter electrode and working

Physiochemical parameters of well water. electrode respectively. The scan rate (V/s) was maintained at
Parameters Results 0.01. Hold time at Ef (sec) was 0 and quiet time (sec) was 2. The
Appearance Colorless
following equation was used to calculate the inhibition
Total dissolved solids 1804 ppm efficiency [13],
pH 7.95 !
0
Total hardness 950 ppm icorr  icorr
Calcium 151 ppm IEð%Þ ¼ 0

100
icorr
Magnesium 87 ppm
Iron 0.76 ppm 0
Conductivity 3459 Micro mho / cm For both the uninhibited and inhibited solutions icorr and icorr
Chloride 515 ppm corresponds to the corrosion current densities. By extrapolation
Sulphates 25 ppm of anodic and cathodic regions of tafel plots, corrosion current
(icorr), corrosion potential (Ecorr), anodic Tafel slope (ba), and catho-
dic Tafel slope (bc) were obtained.
2.3. Corrosion medium
2.6. Electrochemical impedance spectroscopy (EIS)
In our present study, well water chosen as corrosive media were
collected from due well at Seelapadi village, Dindigul (See Table 1). The carbon steel specimen was analysed for the electrochemical
impedance measurements (EIS) in the frequency range of 100 kHz
2.4. Gravimetric studies to 0.00001 kHz under potentio-static circumstances with an AC at
open circuit potential with amplitude 10 mV peak to peak. The
In this technique, already weighed carbon steel coupons were charge transfer resistance (Rct) and the double layer capacitance
dipped in 100 mL of well water in the presence and as well as (Cdl) values were obtained using the following equation [14].
the absence of varied concentrations of Zn2+ and MF at 25 °C. After
Rct = (Rs + Rct ) - Rs
a day of immersing the coupons made of carbon steel, they were
subjected to washing well with the water which as subjected to Where, Rs is the solution resistance and Cdl value are obtained
double distillation. Then they were weighed using SHIMADZU bal- from the following equation,
ance, model ATY224. The following formula was adopted for the
1
inhibition efficiency (IE) calculation. f max ¼
2p
C dl
Rct
W2  W1
IEð%Þ ¼
100 where, fmax is maximum frequency, Cdl is the double layer capaci-
W2
tance, Rct corresponds to the charge transfer resistance [15].
where W2 and W1 is the weight loss value in the absence of inhibi-
tor and the weight loss value in the presence of inhibitor, 2.7. Scanning electron microscopy
respectively.
The SEM micrograph of the carbon steel surface was performed
2.5. Potentiodynamic Polarization study using VEGA3-TESCAN apparatus of accelerating voltage of 20.0 kV
and 1.12 kx magnification. The morphology of the carbon steel sur-
CHI-electrochemical workstation was used to analyse the face that was immersed in well water, without and with inhibitor
potentiodynamic Polarizatio. A three-electrode system consisting was obtained. Later carbon steel was properly washed with dis-
of saturated calomel electrode (SCE), platinum foil and carbon steel tilled water and then dried.
2
X. Joy Pradeep and J. Sathiyabama Materials Today: Proceedings xxx (xxxx) xxx

Table 2
Results of CR and IE (%) of the carbon steel within inhibitor and without inhibitor system for 24 h of immersion in well water obtained by gravimetric method.

MF (ppm) Zn2+
0 25 50
IE (%) CR (mdd) IE (%) CR (mdd) IE (%) CR (mdd)
Blank – 50.63 15 43.03 22 39.44
100 45 27.82 53 23.77 62 19.69
200 55 22.75 62 19.20 79 10.60
300 63 18.73 75 12.64 96 2.01
400 56 22.73 64 18.18 85 7.57
500 51 24.76 57 21.76 72 14.13

2.8. Energy dispersive X-ray spectroscopy
The EDX images were measured in JEOL-JSM-6390 LV SEM
model found with an energy dispersive X-ray device, it has acceler-
ating voltage of 10 kV before and after immersion of binary system.
2.9. FT-IR spectroscopy
The functional group of the binary system was measured in a
Perkin-Elmer 1600 spectrophotometer. The Potassium bromide
pellet was used to study the scratched.
3. Results and discussion
3.1. Gravimetric studies
The Table 2 illustrates that the 300 ppm of MF (Mussaenda
Frondosa) has exhibited a poor corrosion inhibition. After addition
of Zn2+ ions, the inhibition efficiency (IE) was found to be increased
with highest efficiency of 96% for MF (300 ppm) and Zn2+ ions
(50 ppm). The existence of synergistic effect between Zn2+ and
MF was noted [16]. Individually Zn2+ and MF exhibits a poor corro-
sion inhibition of 22% and 63% respectively. Therefore it is clear
that over than individual inhibitors, the mixture of inhibitors is
observed to show better IE. However in case of Zn2+, the concentra-
tion is increased from 25 to 50 ppm the IE is also increased in pres-
ence of MF. It may be noted that the formation of MG-Zn2+ complex
involves the MF molecules and Zn2+ ions in the solution [17]. The
inhibition efficiency was significantly decreased by MF-Zn2+ sys-
tem and increase in concentration of MF was observed. This can
be due to the fact that in the bulk of solutions, of MF-Zn2+ complex
precipitates [18,19]. All these results indicates that the concentra-
tion of 300 ppm of MF and 50 ppm of Zn2+ is constituted the good
protection for carbon steel against corrosion [20].
protective film is not stable for longer immersion period as a result
of corrosivity of well water [21]. This identical finding is also con-
tained in the Phyllanthus amarus extract [22] and Banana Peel
Extract [23].
3.3. Potentiodynamic polarization studies
Potentiodynamic polarization analysis was used to study the
role of surface layer on the bare metal surface throughout corro-
sion inhibition process [24,25]. The tafel plots for the carbon steel
dipped in solution that is blank and binary inhibitor system are
given in Fig. 2 (a) and (b) respectively. The Potentiodynamic Polar-
ization analysis on corrosion parameters is discussed in Table 4.
When bare carbon steel is dipped inside the well water, it dis-
played a corrosion potential of 690 mV Vs SCE. While Ecorr value
has shifted to 688 mV Vs SCE by the addition of inhibitor formu-
lation of 300 ppm of MF and 50 ppm of Zn2+. The binary system has
controlled the anodic and cathodic reaction mutually as observed
from anodic slope and cathodic slope (167.78 mV/dec and
163.03 mV/dec) correspondingly [25]. It can be concluded that
the MF-Zn2+ system performed as an assorted form of inhibitor
[26]. The value of icorr and LPR for well water is 3.9912
105 A/
cm2 and 2894.2 X cm2. The existence of surface layer over carbon

3.2. Effect of immersion period on the inhibition efficiency of

Mussaenda Frondosa (MF) Extract in well water:

The effect of immersion period was present in Table 3, it has

depicted the Inhibition Efficiency (IE) of binary system of MF
(300 ppm) and Zn2+ ions (50 ppm). The obtained result shows that
the immersion period has increased, while the IE of MF-Zn2+
Fig. 2. Tafel plots of the carbon steel in well water a) Blank b) MF-Zn2+ system.
system is gradually decreased. It could be understood that the

Table 3
Effect of immersion period on the inhibition efficiency of MF-Zn2+ system.

Parameters System Immersion Period in days

1 3 5 7
Corrosion Rate (mdd) Well water 50.63 61.31 72.42 96.46
MF-Zn2+ system 2.01 4.89 8.32 13.14
Inhibition Efficiency (IE%) MF-Zn2+ system 96 83 67 43

3
X. Joy Pradeep and J. Sathiyabama Materials Today: Proceedings xxx (xxxx) xxx

Table 4
Potentiodynamic Polarization parameters derived from tafel plots of the carbon steel in well water alone and in the presence of inhibitor system (MF-Zn2+).

Concentration (ppm) LPR (X cm2) ba (mV/dec) bc (mV/dec) icorr (A/cm2) Ecorr (mV vs SCE)
2+
MF Zn
0 0 2894.2 122.42 107.08 3.9912
105 690
300 50 8301.9 167.78 163.03 1.0133
105 688

formed by the adsorption of binary system over the surface of car-

bon steels [35].

3.5. Scanning electron microscopy (SEM) analysis

The SEM analysis was examined to know additional information

Fig. 3. Nyquist plots of carbon steel in well water a) Blank b) MF-Zn2+system.
about the surface film morphology of formation [36]. The Fig. 4a
shows SEM images of bare carbon steel of 1.12 kx magnification.
The Fig. 4b exhibits the SEM images of carbon steel with 1.12 kx
magnifications without the inhibitor, it is found that the surface
of carbon steel are corroded and its surface appears to be uneven
and rough [37]. The Fig. 4c depicts the existence of binary system
of MF with Zn2+ ions over the metal surface and this defensive sur-
face layer protect form corrosion to exhibits a smooth surfaces
[38,39]. The surface film is randomly observed over the metal sur-
face. The defensive surface layer which acts as an adsorption inhi-
bitor has blocked the active sites available over the carbon steel
surface to protect from corrosion [40,41].

3.6. Energy dispersive X-ray (EDX) spectroscopy studies

steel has decreased the corrosion current values to 1.0133
105
A/cm2 and increased the LPR values to 8301.9 X cm2[27]. The bin-
ary system MF (300 ppm) and Zn2+ ions (50 ppm) was used for the
carbon steel in well water as an corrosion inhibitor [28].
3.4. Electrochemical impedance spectroscopy (EIS) studies
Nyquist plot represents the effective coating of MF-Zn2+ system
over carbon steel was investigated [29] as shown in Fig. 3. The
observed AC impedance spectra depicts, over the carbon steel in
well water a defensive surface layer formation has formed [30].
The formed defensive surface layer, has increased the charge trans-
fer resistance (Rct) and also decreases the double layer capacitance
(Cdl) value [31]. The impedance response obtained from the plots
has been significantly influenced by inhibitors [32]. The impedance
plot appears to be semicircular, indicating that the corrosion of car-
bon steel was restricted by a process called charge transfer [33].
The frequency dispersion of interfacial impedance causes a shift
from accurate semicircle shape. This strange performance is owing
due to the non–homogeneity of carbon steel surface occurred by
surface roughness [34,36]. The electrochemical kinetic parameters
impedance parameters, are in Table 5.
As shown in the Fig. 3, the presence of MF-Zn2+ system, the
value of Rct (from 192.32 X cm2 to 640.40 X cm2) is found to be
increased and Cdl value (from 8.1309
106 lF/cm2 to
1.1847
106 lF/cm2) is decreased as compared to the well water
alone. This means that, inhibiting action of MF-Zn2+ system is per-
Table 5
Electrochemical kinetic parameters obtained by EIS technique for the corrosion of
carbon steel in well water alone and with inhibitor system (MF-Zn2+).
Concentration (ppm) Charge transfer Double Layer
Resistance, Capacitance,
MF Zn2+
Rct (X cm2) CdI (lF/cm2)
0 0 192.32 8.1309
106
300 50 640.40 1.1847
106
4
The elemental composition over the carbon steel surface was
calculated using EDX spectra [24]. The bare carbon steel surface
is primarily composed of iron with small percentages of Carbon
and Oxygen as revealed in Fig. 5a [42]. In Fig. 5b carbon steel in
well water alone shows that the surface includes mainly Fe due
to Fe2O3/Fe(OH)2 formation. Fig. 5c indicates that elements of inhi-
bitor formulation namely O and Zn are found on the carbon steel
surface with remarkable reduction in Fe peak [43]. From the find-
ings of the EDX study, it can be understood that the binary inhibi-
tor Zn2+ has been closely coordinated with the Fe2+/Fe3+ ion on the
metal surfaces to form a defensive surface layer [44].
3.7. FT-IR studies
FTIR spectra is an analytical tool used for the identification of
the protecting film that is formed over the surface of the metal
[45]. Few drops of an ethanolic MF extract is let to dry on a plate
of glass. A strong, thick residue was collected [46]. It displays in
Fig. 6a. The resulting stretching frequency of carboxyl group is
found to occur around 1630 cm1. The –OH band is present at
3422 cm1. As presented in Fig. 6b, the frequency of C = O and –
OH stretching is changed from 1630 cm1 to 1612 cm1 and also
from 3422 cm1 to 3416 cm1 respectively. Such changes suggest
that the distribution of the electron cloud of C = O and –OH func-
tional groups in MF has modifies Fe2+/Fe3+ ions of the metal surface
at anodic region, which leads to the development of Fe2+-MF com-
plexes [47]. A band around 663 cm1 is attributable to Zn-O
stretching in cathodic regions by Zn(OH)2 [48,49].
Four Components are found to be prominent out of thirty two
components that is contained by the MF extract as revealed by
the GC–MS analysis. A development in the topology of the surface
in the corrosion inhibited MS was observed by SEM micrograph. It
is found that the concentration of the MF extract exerts corrosion
mitigation as explained by ANOVA studies. A significant interaction
between the exposure time and the concentration of inhibitors was
observed. With the formation of an even film on the surface of MS
X. Joy Pradeep and J. Sathiyabama Materials Today: Proceedings xxx (xxxx) xxx

Fig. 4. SEM micrographs of carbon steel in well water a) bare b) Blank c) MF-Zn2+ system.

Fig. 5. EDX images of the carbon steel in well water a) bare b) Blank c) MF-Zn2+ system.

electrode, it is evident that the Isopropyl 2-phenyl-4,5-dihydro-1,

3-oxazole-4-carboxylate (CP3) controls the acid corrosion.

4. Conclusions

The current study reveals the subsequent summary. The binary

system consisting of Mussaenda Frondosa (MF) Extract (300 ppm)
and Zn2+ ions (50 ppm) has exhibited a highest inhibition efficiency
of 96% for carbon steels dipped in well water. When immersion
period and corrosion rate increases, markedly inhibition efficiency
of MF-Zn2+ system decreases. Potentiodynamic polarization mea-
surement showed that the Mussaenda Frondosa (MF) extract-
Zn2+ ions are an inhibitor of mixed type. The EIS measurements
indicates that the presence of MF-Zn2+ system has noticeably
reduced the double layer capacitance (Cdl) of surface film. While
the charge transfers resistance (Rct) was appreciably higher. The
Fig. 6. FT-IR spectra of carbon steel in a) pure MF extract c) MF-Zn2+ system. formation of surface film that is protective over carbon steel was
5
X. Joy Pradeep and J. Sathiyabama
confirmed by SEM and EDX analysis. The FTIR analysis reveals that
the surface layer comprises of MF-Zn2+ ions binary system.
Declaration of Competing Interest
The authors declare that they have no known competing finan-
cial interests or personal relationships that could have appeared
to influence the work reported in this paper.
Acknowledgements
The author thanks the GOD Almighty for the grace that accom-
plished this research work.
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