Case Studies in Chemical and Environmental Engineering 6 (2022) 100227

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Case Report

Evaluation of bee wax propolis inhibitor for corrosion protection on stainless

steel in various pH solution
Femiana Gapsari a, *, Hastono Wijaya a, Renny Septiari b, Andoko c
a
Department of Mechanical Engineering, Faculty of Engineering, Brawijaya University, MT Haryono 167, Malang, 65145, Indonesia
b
Department of Industrial Engineering, Faculty of Engineering, National Institute of Technology (ITN), Malang, 65145, Indonesia
c
Department of Mechanical Engineering, Faculty of Engineering, State University of Malang, Malang, 65145, Indonesia

A R T I C L E I N F O A B S T R A C T

Keywords: The protective ability of an organic inhibitor varies and is affected by the pH of the solution. Related with this
304SS fact, this work investigated corrosion inhibition performance of Bee Wax Propolis (BWP) extract on 304 SS in
Electrochemical measurements various environment (0–14 pH). The BWP extract inhibitor had formed a passive layer on the surface, indicated
pH
by the increase of the passive region. The inhibition efficiency changed randomly at all pH. The optimum in­
BWP extract Inhibitor
hibition efficiency for the acid and alkaline condition happened at pH 2 (96.60%) and 12 (97.75%). BWP was
AFM
found to control corrosion better at pH 2 and 12.

1. Introduction
Organic inhibitor is well known for its corrosion protection ability in
a corrosive environment which includes acid, alkaline or salt [1–10]. In
order to reach outstanding corrosion protection, heteroatoms (N, S, and
O) in organic inhibitor play important role [11,12]. However, to meet
the commercial product standard, inhibition efficiency and the pro­
duction cost of an organic inhibitor need to be increased and decreased
respectively. An inhibitor suits a specific media. There are different
protection mechanisms for each environment. Therefore, studies on an
organic inhibitor in many kinds of environments need to be conducted to
find the most appropriate inhibitor for each environment.
Previously, Bee Wax Propolis (BWP), the residual material from
honey process production, was proposed to be an alternative organic
inhibitor for 304SS [13–15]. The flavonoid and antioxidant in BWP
extract have an excellent corrosion protection behaviour for 304SS.
They can inhibit corrosion of 304SS in 0.5 M sulfuric acid up to 97.29
[14], and constructed 304SS diagram Pourbaix with BWP extract [16].
The inhibitor addition changed the 304SS E-pH diagram. The active area
on the E-pH diagram where the inhibitor decreased up to 15.69% and
the passive area broadens up to 6.01%. However, as a critical factor that
determines the alteration of 304SS E-pH diagram, the chemical activity
in various pH conditions has not been studied.
This study was performed to know the influence of pH on corrosion
protection using BWP inhibitor. The finding is expected to recommend
the appropriate way of using BWP on 304SS. Corrosion inhibition per­
formance of BWP extract on 304SS specimen in sulfuric acid environ­
ment by adjusting pH from 0 to 14 at room temperature was
characterized by using electrochemical and surface analysis techniques.
2. Experimental
2.1. Synthesis and characterization of BWP inhibitor
The synthesis and characterization of BWP referred to the previous
works [13,14]. BWP was obtained from the waste of bee farm in
Northern Lombok, Indonesia. 1000 g of BWP was oven dried and
ground. Then, it was mixed with 50 ml of ethanol. Next, the mixture was
squeezed and heated at 60 ◦ C. The results showed that the main com­
pound in BWP extract is quercetin with chemical structure of 2-(3,
4-dihydroxyphenyl)-3,5,7-trihydroxy-4H-chrome-4-one.
2.2. Solution preparation
H2SO4 and double-distilled water were used to make solution. The
pH value was carefully controlled by adding the NaOH solution into the
mixture to get the expected pH, the pH was set up from 0 to 14.

* Corresponding author.
E-mail address: memi_kencrut@ub.ac.id (F. Gapsari).

https://doi.org/10.1016/j.cscee.2022.100227
Received 11 May 2022; Received in revised form 25 June 2022; Accepted 27 June 2022
Available online 5 July 2022
2666-0164/© 2022 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).
F. Gapsari et al. Case Studies in Chemical and Environmental Engineering 6 (2022) 100227

2.3. Materials Table 2

Inhibition efficiency measurement with the polarization method in acidic
The material used in this research was 304SS with dimension of 4 × environment.
1 × 0.2 cm (the chemical composition is detailed in Table 1). Each pH βa -βc Ecorr icorr Corrosion IE
sample was ground using SiC grinding papers from grade 200 to 2000 rate (%)
grit and coated with epoxy resin (exposed surface area of 1 cm2). Next, (V/ (V/ (V) (A/ (mm/year)
the specimens were coated with epoxy resin and leaving an open area of dec) dec) cm2)
1 cm2 on the surface. The BWP extract was coated onto the open area 0 0.25 3.43 0.17 8.77 x 0.09
and dipped into a mixture of H2SO4 and DI water solutions having 10-6
various pH values. 1 0.27 1.74 0.09 3.89 x 0.04
10-6
Absence 2 0.53 − 1.11 − 0.03 2.25 x 0.23
2.4. Electrochemical measurement 10-5
3 0.64 − 1.14 − 0.13 2.55 x 0.27
10-5
Corrosion behaviour was studied using an electrochemical mea­ 4 0.86 − 1.38 − 0.21 5.99 x 0.62
surement system (Autolab PGSTAT 128 N) at room temperature with the 10-5
platinum as the counter electrode (CE), Ag/AgCl (KCl 3 M) as the 0 0.3 1.18 0.09 3.85 x 0.04 56.08
reference electrode (RE), and 304SS specimen as the working electrode 10-6
1 0.21 0.23 − 0.16 1.77 x 0.02 54.44
(WE). Three electrodes were immersed in electrolyte with various pH
10-6
values (0–14). The electrochemical measurement was conducted in Presence 2 0.16 0.11 − 0.15 7.63 x 0.01 96.60
absence and presence (2000 ppm of BWP inhibitor) conditions [14]. 10-7
Quercetin is proven to be the main ingredient of BWP, which is 43.90% 3 0.63 − 1.13 − 0.09 2.02 x 0.21 21.04
10-7
[13].
4 0.67 − 1.37 − 0.17 3.45 x 0.3589 42.43
The Tafel curves were measured in the potential range of -1 V to +1 V 10-5
with a scan rate of 0.001 V/s. The inhibition efficiency can be calculated
using the Equation (1) [17,18]:

icorr0 − icorr Table 3

IE (%) = × 100% (1) Inhibition efficiency measurement with the polarization method in neutral
icorr0
environment.
The icorr 0 and icorr are corrosion current density from the potentio­
pH βa -βc Ecorr icorr Corrosion IE
dynamic polarization measurement absence and presence BWP. rate (%)
In order to observe the oxidation and reduction activity of 304SS,
(V/ (V/ (V) (A/ (mm/year)
cyclic voltammetry (CV) measurement was conducted at the scan rates dec) dec) cm2)
of 10, 50, 100, 250, 500, 750, and 1000 mV/s. The CV data was per­
5 0.40 − 1.46 − 0.20 5.49 x 0.57
formed to determine the peaks of oxidation and reduction currents.
10-5
Thus, the best scan rate variation can be known. CV test was performed 6 0.56 − 0.88 − 0.38 5.87 x 0.61
with varied scan rate to determine the effect of solution speed. 10-5
Absence 7 0.39 − 0.62 − 0.22 2.99 x 0.31
10-5
3. Result and discussion
8 0.36 5.71 − 0.15 1.83 x 0.19
10-5
3.1. Effect of pH on electrochemical corossion 9 0.52 − 1.06 − 0.17 1.06 x 1.10
10-4
5 0.24 3.25 − 0.22 6.73 x 0.07 87.75
The related parameters are listed in Tables 2–4. Fig. 1 of the typical
10-6
potentiodynamic polarization curves for 304SS in various pH shows 6 0.36 − 15.35 − 0.15 1.24 x 0.13 78.93
depicts the active and passive region of corrosion of 304SS. 10-5
Fig. 1a displays the typical potentiodynamic polarization curves for Presence 7 0.39 − 0.62 − 0.22 2.99 x 0.31 0.00
304SS in acid condition (pH 0–4) absence and presence of inhibitor. The 10-5
8 0.53 − 3.83 − 0.15 1.40 x 0.15 23.77
304SS Ecorr is almost in the negative shift with the increasing of pH
10-5
value. At pH 0, 3 and 4, the inhibitor changes Ecorr shift to the positive 9 0.39 − 1.77 − 0.24 2.51 x 0.26 76.32
value. Meanwhile, at pH 1 and 2, Ecorr shifts to the negative value. Yet, 10-5
the icorr decreases significantly (approximately by one degree lower)
compared to the 304SS absence inhibitor as described in Table 2. Based
on our previous study, BWP extract acted as mixed type inhibitor [14]. decrease of icorr (Table 4). The addition of OH- concentration controls
Therefore, this inhibitor might have protected 304SS either in anodic or the oxygen reduction reaction which causes the anodic dissolution of
cathodes site. 304SS [19]. Therefore, the icorr value decreases to smaller value.
Fig. 1c shows that in the absence of inhibitor the corrosion rate of The inhibition efficiency changes randomly at all pH. This is maybe
304 in alkaline solution (pH 10–14) changes the Ecorr shift randomly. caused by the physisorption mechanism of BWP extract inhibitor. Op­
Presence of inhibitor, Ecorr slightly shifts to positive value at pH 11, 13, timum inhibition efficiency (96.60%) for the acid condition was reached
and 14. At pH 10 and 12. Ecorr shifts to negative value followed by the at pH 2, while for the alkaline condition it was reached at pH 12
(97.75%). This evidence indicated that the BWP inhibitor had a good
performance either in acid or in alkaline condition. Furthermore, in a
Table 1
neutral condition, the inhibition efficiency of BWP on 304SS did not
Chemical composition of 304SS.
considerably change because pH of BWP is also the same with the
Elements (%) neutral environment [14].The inhibition efficiency went down at pH 13
Cr Si Ni Mn C P S Fe where the passive region was more at the pH. Under high positive po­
18.15 0.52 9.58 0.92 0.04 0.03 0.002 Bal. tential, there was an increase in corrosion rate that went to the

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F. Gapsari et al. Case Studies in Chemical and Environmental Engineering 6 (2022) 100227

Table 4 Fig. 2 shows the CV curves of 304SS presence and absence BWP in­
Inhibition efficiency measurement with the polarization method in alkaline hibitor. The test was carried out using pH 0 media. The CV curve illus­
environment. trate the reaction at anodic (oxidation) and cathodic (reduction)
pH βa -βc Ecorr icorr Corrosion IE regions. The oxidation region can be classified into three sub-regions
rate (%) namely (a) anodic, (b) passive, and (c) trans passive region. Mean­
(V/ (V/ (V) (A/ (mm/year) while, the reduction region consists of two peaks that signify (d)
dec) dec) cm2) hydrogen revolution and (e) oxygen reduction sub-regions. At peak (a)
10 0.44 − 0.85 − 0.16 3.77 x 0.39 decomposition rate of the reaction increases with the increasing acid
10-5 concentration and scan rate [21,24]. Fig. 2a shows that the formation of
11 0.14 − 1.56 − 0.29 3.24 x 0.03 iron hydroxide occurs through the precipitation-dissolution mechanism
10-6 formed on the solute and formed a deposit on the electrode surface when
Absence 12 0.56 − 1.02 − 0.14 8.46 x 0.88
10-5
the reaction product is exceeded by its solubility [21]. At peak (a) which
13 0.12 0.28 − 1.08 2.27 x 0.24 is a potential anodic region (e) with a value of about -0.23 V (Ag/AgCl),
10-5 the reaction occurring at pH 0 absence of inhibitor
14 0.13 − 0.20 − 0.70 2.40 x 0.25
10-5 Fe + H2 O→FeO + 2H + + 2e (2)
10 0.16 − 7.07 − 0.20 3.56 x 0.04 90.55
10-6 Ni + H2 O→NiO + 2H + + 2e (3)
11 0.19 0.47 − 0.21 3.24 x 0.03 0.19
10-6
Presence 12 0.19 0.81 − 0.16 1.90 x 0.02 97.75
Cr + H2 O→CrO + 2H + + 2e (4)
10-6
The peak value (a) with E = -0.23 is a CV with a scan rate of 10 mV/s.
13 0.15 0.18 − 1.04 1.71 x 0.18 24.85
10-5
The reaction at peak (b) E is about -0.1 V (Ag/AgCl) reaction that occurs:
14 0.17 0.76 − 0.50 7.40 x 0.01 96.92
2FeO + H2 O→Fe2 O3 + 2H + + 2e (5)
10-7

2CrO + H2 O→Cr2 O3 + 2H + + 2e (6)

passivation potential maximum value. Passive means disappearance of
Peak (b) is a passive and peak area (c) is a transpassive region formed
metal chemical reactivity under certain environment because of the
by Fe, Ni, and Cr hydroxide. At peak (b), there is higher oxide formation
protective layer formation [20]. Passive areas seem larger at pH above 6.
of iron and chromium as well as some nickel oxide thickening. However,
The larger passive areas at various pH are due to the adsorption mech­
no indication of the formation of nickel oxide at E of 0.1V. This is due to
anism performed by the BWP extract in inhibiting the rate of corrosion
the passivation nature and resistance to the acidic solution of chromium
[21].
oxide (Cr2O3). Cr2O3 is considered as the main component in the passive
The active region (pH potential region) indicates the corrosion on a
layer of pliers formed. Therefore, the anodic peak (b) is identified as the
metal appears with a positive potential rise. Corrosion rate ends in the
main passive stage in the anodic polarization of 304SS [21]. It appears
passive region. The anodic current density does not escalate with the rise
that after the peak (b) is passed the anodic current begins to decrease
of potential, signalling that passivation starts. A passive layer is the
until the peak (c) starts. The presence of a current flowing along the
product of corrosion that protects the metal and behaves as a barrier
passive region at an acid concentration increases with the increase in
between the metal and corrosive environment. The BWP extract formed
scan rate. This indicates that BWP inhibitor affects the mechanism re­
passive layer by physisorption mechanism [22,23]. The reaction that
action in the passive region [14,22].
happened in acidic pH could be predicted from CV test. This test was
Peak (d) illustrates the cathodic area of reaction at E +0.16 to +0.11
conducted to find out the oxidation and reduction reaction.
V (Ag/AgCl) during hydrogen evolution. Peak (e) is the cathodic area of
reaction at E +0.59 to +0.51 V (Ag/AgCl) where the oxygen reduction
reaction occurs.
3.2. The BWP extract inhibition mechanism in acid environment
Fig. 2b also shows the same parts,but the value of potential oxidation
and reduction potential are different. In CV variations presence of in­
The decrease in corrosion rate at various pH presence of BWP indi­
hibitors, the flow of the reaction occurs the same as absence inhibitors.
cated the inhibition. An adsorption mechanism occurs on the metal
The current difference is seen at peak (a) to (e) as shown in Table 3.
surface [16]. CV test with various scan rate was conducted to confirm
The current oxidation density presence inhibitors is smaller than that
the inhibition reaction due to presence of inhibitor.

Fig. 1. Potentiodynamic polarization curves of 304SS in various pH presence and absence BWP inhibitor, a) pH 0–4, b)5–9, c) 10-14.

3
F. Gapsari et al. Case Studies in Chemical and Environmental Engineering 6 (2022) 100227

Fig. 2. CV curves with the variation of scan rate at pH 0 (a) absence BWP inhibitor (b) presence BWP inhibitor.

of absence inhibitors. It proves the inhibitory effect of inhibition [21]. to (Equation (12)), the mechanism occurs in the presence of water
The process of inhibition appeared through the adsorption of the active molecules on the metal surface which is replaced by the inhibitor species
side of the inhibitor to the metal surface. The inhibitory process is shown to produce Feetimed Intermediate Fe-quercetinads (Eq. (14)). This will
in the cathodic reaction in Table 3. It is seen that reduction current reduce the number of FeOHads species and cause anodic Fe bubbles [27].
density also decreases with the presence of BWP extract. The mechanism of passivation of 304SS thin films in atmospheric
The solubility reaction of Fe in sulfuric acid solution with inhibitors inhibitors and sulfuric acid is as follows: carbohydrates (quercetin) with
is as follows [4]: sulfuric acid produce carbon, water and water and acid mixtures [28].
Furthermore, water produces oxygen and hydrogen, in the final stages of
Fe + H2 O ↔ FeOHads + H + + e (7)
carbon and oxygen will meet with 304 SS to form oxide and carbide
layers. The presence of oxidation and reduction reactions in metal pol­
(8)
rds
FeOHads ̅→FeOH + + e ishes in the presence of BWP inhibitors can be proved by changes in the
surface of finer specimens. This indicates a protective metal,and there is
FeOH + + H + ↔ Fe2+ + H2 O (9) no corrosion trigger. The large passive areas are due to the protection of
According to the Bockris mechanism (Eqs. (7)–(9)), the dissolution of BWP extract inhibitors. The difference in the smoothness of the metal
Fe in sulfuric acid solution is affected by the absorbed FeOHads in­ surfaces by the addition of BWP extract inhibitors were revealed by AFM
termediates. The presence of anions such as SO2-
4 is also important in the
testing.
formation of reaction intermediates on metal surfaces either inhibiting
or accelerating corrosion reactions [25]. 3.3. AFM characterization
The mechanism involves the absorption of 2 intermediate species to
determine Fe’s solubility process in the presence of an inhibitor [26]. Fig. 3 shows AFM topography of 304SS in different environment
Reactions that may occur are as follows: condition (acid, neutral, and alkaline). As expected, the surface of 304SS
tends to be rough with unregularly surface absence BWP extract inhib­
Fe + H2 O ↔ FeH2 Oads (10) itor. The rough surface indicates that the corrosion appears faster
absence of inhibitor. Conversely, the surface of 304 SS is smoother
−
FeH2 Oads + quercetin ↔ FeOHads + H + + quercetin (11) presence BWP extract inhibitor. This indicates that BWP is effective to
inhibit the corrosion on 304SS either in acid, neutral, or alkaline
FeH2 Oads + quercetin ↔ Fequercetinads + H2 O (12)
condition.

(13)
− rds
FeOHads ̅→FeOHads + e 4. Conclusion

Fequercetinads ↔ Fequercetin+
ads + e (14) This study analyses BWP as an organic inhibitor. The BWP extract
inhibitor is effective to protect 304SS against corrosion at various pH (0-
FeOHads + Fequercetin+ ↔ Fequercetinads + FeOH +
(15)
ads 14). The inhibition process transpired due to an adsorption on the sur­
face of 304SS. The adsorption mechanism led to the formation of a
FeOH + + H + ↔ Fe2+ H2 O (16)
passive layer on the surface, indicated by the increase in the passive
Based on the reactions, water molecules adsorbed on the metal sur­ region. The passive regions got larger with the decrease in potential
face are replaced by the inhibitor species to form Fe-quercetinads inter­ passive values at each pH. Meanwhile, the potential range of oxidation
mediate species (Eq. (12)) This species reduces FeOH-ads that causes with reduction potential was smaller presence of BWP extract inhibitor.
anodic solubility inhibition of Fe [26]. This work does not only propose a concept of the BWP extract inhibitor’s
The inhomogeneous nature of metal surfaces produces lattice defects chemical reaction but also to provide and in-depth study of BWP extract
and dislocations. A corroded metal will produce several active sides to as an excellent alternative inhibitor for corrosion protection of 304SS.
be able to absorb some of the activation energy. The molecular inhibitor
can be absorbed more easily on the active surface side having the
appropriate adsorption enthalpy. Based on the equations (Equation (6))

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F. Gapsari et al.
Fig. 3. AFM topography of 304SS absence and presence BWP extracts inhibitor at pH (a) 0 (b) 7 (c) 11.
Declaration of competing interest
The authors declare that they have no known competing financial
interests or personal relationships that could have appeared to influence
the work reported in this paper.
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