Paper No.

11232

Mechanism of CO2 Corrosion of Mild Steel: a New Narrative

Aria Kahyarian, Bruce Brown, and Srdjan Nesic

Ohio University
342 W. State St.
Athens, OH 45701
USA

ABSTRACT

The polarization behavior of API 5L X65 mild steel at various pH values and CO2 partial pressures was
investigated at a high flow velocity. In contrast to the commonly accepted mechanistic view of CO 2
corrosion, it is shown that the direct reduction of carbonic acid is insignificant at CO2 partial pressures up
to 5 bar. That suggests that carbonic acid is merely a “reservoir” of hydrogen ions and its presence only
increases the observed limiting current densities by buffering the H+ concentration at the metal surface.
Furthermore, the rate of anodic iron dissolution reaction was shown to be significantly increasing in the
presence of CO2, suggesting that dissolved CO2 or its associated carbonate species are directly involved
in the iron dissolution reaction. The findings of the present mechanistic study showed that the increased
corrosion rates of mild steel in acidic solutions in the presence of CO2, which were previously associated
with carbonic acid direct reduction, are in fact due to the increased rate of iron dissolution in the presence
of CO2, in combination with the increased cathodic limiting currents resulting from buffering ability of
dissolved CO2 and H2CO3.

Key words: Metallic corrosion, acidic corrosion, mild steel, carbon dioxide, mechanism, iron dissolution

INTRODUCTION

The profound effect of dissolved CO2 on increasing the corrosion rate of pipeline steel, as compared to
solutions of strong acids with the same acidity, has been known for many decades. However, findings in
the last two decades have challenged the commonly accepted ideas about the underlying mechanisms
of this process. This study is focused on the fundamentals of the electrochemical reactions involved in
the CO2 corrosion of mild steel in an attempt to further elucidate the mechanisms of the CO 2 corrosion
process.

Carbon dioxide (CO2) in gaseous or dissolved state is non-corrosive. However, upon dissolution in water
(reaction ( 1 )) and a subsequent hydration reaction (reaction ( 2 )), a more reactive chemical species,
carbonic acid (H2CO3), is formed. This hydration reaction is followed by dissociation reactions (reactions
( 3 ) and ( 4 )) to form bicarbonate (HCO3-), carbonate (CO32-), and hydrogen (H+) ions; resulting in an
acidic, corrosive solution.

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1
 CO2(g) ⇋ CO2(aq) (1)
CO2(aq) + H2 O(l) ⇋ H2 CO3 (2)
(aq)
H2 CO3(aq) ⇋ HCO−
3 (aq) + H + (aq) (3)
HCO− 2− +
3 (aq) ⇋ CO3 (aq) + H (aq) (4)
H2 O(l) ⇋ OH − (aq) + H + (aq) (5)

The chemical equilibria and water chemistry associated with dissolved CO2 and its carbonate derivatives
has been extensively studied. A more comprehensive discussion on this matter can be found
elsewhere.1,2

Cathodic reactions in CO2 Corrosion

The electrochemical reactions associated with CO2 corrosion, based on the commonly accepted
mechanisms, are shown below.3–6 Anodic reaction ( 6 ) is the cause of metal deterioration, and reactions
( 7 ) through ( 10 ) are the commonly accepted cathodic reactions, providing the electron sink required
for the anodic reaction to progress spontaneously. This mechanism is mainly based on the original
studies of de Waard and Milliams in 1975, 7 Schmitt and Rothmann in 1977, 8 and Gray et al. in 1989 and
1990, 9,10 as reviewed in more details elsewhere. 1,2,6

Fe2+ (aq) + 2e− ⇋ Fe(s) (6)

1 (7)
H + (aq) + e− ⇋ H2 (g)
2
1 (8)
H2 O (l) + e− ⇋ OH − (aq) + H
2 2 (g)
1 (9)
H2 CO3(aq) + e− ⇋ HCO−3 (aq) + H
2 2 (g)
1 ( 10 )
HCO− − 2−
3 (aq) + e ⇋ CO3 (aq) + H
2 2 (g)

The effect of homogeneous chemical reactions of the water/CO 2 system on the rate of electrochemical
reactions is probably the most important aspect of CO 2 corrosion that differentiates the uniform CO2
corrosion from the corrosion induced by strong acids (e.g. HCl or H2SO4) or other weak acids such as
H2S and organic acids. There are two known effects associated with homogeneous chemical reactions
in CO2 corrosion:
a) The more significant effect is related to dissolved CO2 gas. Only ~0.2 % of dissolved CO2
molecules are hydrated to form H2CO3 according to the hydration equilibrium (reaction ( 2 )). This
means there is a large reservoir of dissolved CO2 present in the solution to replenish the H2CO3
concentration as it is consumed by dissociation and/or reduction at the steel surface. Therefore,
in addition to mass transfer of H2CO3 from the bulk solution, the limiting currents are increased as
a result of this hydration reaction.
b) The second effect is associated with H2CO3 and its generic buffering ability as a weak acid.
Considering the H2CO3 dissociation reaction (reaction ( 3 )), the concentration of H+ at the metal
surface is buffered when the equilibrium shifts towards the right-hand side (i.e. consumption of H+
by the reduction reaction). While this does not influence the magnitude of limiting current directly,
it is of significance when discussing the mechanisms of charge transfer controlled corrosion at
high CO2 partial pressures.

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2
 The abovementioned mechanistic view of the cathodic reactions in CO2 corrosion is now widely accepted,
however, the new findings in more recent studies have challenged its foundations 11–13. In those studies,
it was shown quantitatively, that the limiting currents could be adequately explained even if H 2CO3 was
not considered an electroactive species. This can be understood when considering the local
concentration of chemical species in the vicinity of the metal surface, where the homogeneous H2CO3
dissociation reaction (reaction ( 3 )), followed by electrochemical reduction of the produced H+ ions
(reaction ( 7 )), provides a parallel reaction pathway to the direct H2CO3 reduction reaction (reaction ( 9
)). This observation carries a significant mechanistic implication, since it undermines the previous
commonly accepted mechanistic arguments, which were developed based on the analysis of cathodic
polarization behavior at or close to limiting currents 8–10. Therefore, to date, the evidence for direct H2CO3
reduction is mostly circumstantial. This was perhaps best noted by Nordsveen et al. 11 who suggested
that while the cathodic limiting currents can be quantitatively explained without considering H2CO3 as an
electroactive species, the predicted corrosion rates are in better agreement with the experimental data
when this additional reaction was included in the model.

The reaction mechanism that suggests H2CO3 dissociation is followed by H+ reduction, is now known in
the literature as the “buffering effect” mechanism, which was proposed as an alternative to the
conventional mechanism including the carbonic acid reduction, the so called “direct reduction”
mechanism. These proposed mechanisms are not particular to CO2 corrosion. Similar arguments have
been put forward for various weak acids such as acetic acid and hydrogen sulfide 14–17. Considering a
generic weak acid, HA, (representing: H2CO3, HCO3-, H2S, HAc, etc.), its direct reduction can be
expressed as reaction ( 11 ). As a weak acid that is only partially dissociated in the solution, HA is also
involved in the homogeneous chemical equilibrium described via reaction ( 12 ). Additionally, in acidic
solutions, the H+ reduction reaction occurs as shown by reaction ( 13 ).

1
HA + e− ⟶ H + A− ( 11 )
2 2
HA ⇌ H + + A− ( 12 )
1
H + + e− ⟶ H2 ( 13 )
2

The “direct reduction” mechanism suggests that HA reduction (reaction ( 11 )) is significant, therefore,
the cathodic currents in acidic solutions are the result of two parallel electrochemical reactions, HA
reduction, and H+ reduction. On the other hand, the “buffering effect” mechanism suggests that, reaction
( 11 ), the reduction of HA, is insignificant as compared to reaction ( 13 ), the reduction of H+. Therefore,
the dominant cathodic reaction in acidic solutions, is H+ reduction, while HA buffers the concentration of
H+ ions at the surface through the homogeneous reaction ( 12 ). These two mechanisms may be
qualitatively distinguished by studying the behavior of charge transfer controlled cathodic currents 14,15. If
the concentration of the common reactant between the two possible mechanisms (H+) is kept constant,
each mechanism shows a distinct behavior as the concentration of the weak acid is increased (Figure 1).
For the case of the “buffering effect” mechanism, no significant change in charge transfer controlled
currents is expected, since the weak acid is not electrochemically active (Figure 1.B). On the other hand,
for the “direct reduction” mechanism the charge transfer controlled cathodic currents are increased as
the concentration of the reactant (the weak acid) is increased (Figure 1.A). It is important to note that the
magnitude of the limiting current in both mechanisms are identical and the shape of the limiting current
does not provide conclusive evidence for the electrochemical activity of a chemical species.

Considering these two hypothetical behaviors, Tran et al. studied the effect of H2CO3 in CO2 corrosion18.
The authors noted that, even at higher CO2 partial pressures the pure charge transfer control cathodic
currents are not clearly observed on an X65 mild steel surface and this hypothetical behavior cannot be

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3
 verified. Therefore, stainless steel electrodes, being a more noble substrate, were used to eliminate the
interference by the anodic iron dissolution reaction. By comparing the steady state voltammograms for
pH 4 and pH 5 at 1 and 10 bar CO2 partial pressures, the authors reported a behavior resembling that
shown in Figure 1.B, and hence concluded that the cathodic currents in CO2 saturated solutions follow
the “buffering effect” mechanism18. However, considering the effect of alloying compounds of stainless
steel (~ 20 wt. % Cr, and 10 wt. % Ni) and their corresponding passive films on the electro-activity of the
metal surface, the observed mechanism for cathodic currents could not be applied to mild steel without
further verification.

(A) (B)
Charge transfer Charge transfer
-0.3 controlled region -0.3 controlled region

Potential vs. SHE / V

-0.5 -0.5
Potential vs. SHE / V

-0.7 -0.7

H+ reduction w/o weak acid

H+ reduction w/o weak acid

-0.9 -0.9

-1.1 -1.1

-1.3 -1.3
0.01 0.1 1 0.01 0.1 1 density / (A.m
Current 10 -2) 100 1000
Current density 10
/ (A.m -2) 100 1000

Figure 1: Hypothetical cathodic steady state voltammograms for (A) Direct reduction
mechanism and (B) Buffering effect mechanism.

Anodic reactions in CO2 corrosion

Iron oxidation as the dominant anodic reaction is a key element in acidic corrosion of mild steel. The
mechanism of the iron oxidation reaction in acidic media has been extensively studied over the last few
decades.19–30 In this section, the mechanism of acidic iron dissolution is briefly discussed to provide the
necessary context relevant to CO2 corrosion, while a thorough review of the existing literature can be
found elsewhere. 29,31

El Miligy et al. 22 showed that the iron dissolution in mildly acidic environments occurs in four different
states, depending on the potential and solution pH. The authors categorized these as active dissolution,
transition, pre-passivation, and passivation, as demonstrated in Figure 2. Each range was shown to have
a different electrochemical behavior, characterized by different apparent Tafel slopes and reaction orders.
The peak potentials of the two local current maxima, observed in transition and pre-passivation ranges,
were shown to be pH dependent. This suggests that the governing mechanism of iron dissolution at the
corrosion potential could vary depending on the solution pH and other environmental conditions.

There are two classic mechanisms proposed for iron dissolution in acidic solutions in the literature, which
are commonly referred to as: the “catalytic mechanism” and the “consecutive mechanism”. These two
mechanisms are associated with two distinct electrochemical behaviors observed in the active dissolution
range. The catalytic mechanism, first proposed by Heusler et al. 32, is based on the experimental Tafel
slope of 30 mV and second order dependence on hydroxide (OH-) ion concentration. On the other hand,
the consecutive mechanism proposed by Bockris et al. 27, was formulated to explain the observed Tafel
slope of 40 mV and a first order dependence on OH- ion concentration. These two significantly different

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4
 reaction kinetics are believed to be caused by the surface activity and microstructure of the metal
substrate. 20,28,30,31 In more recent years there seems to be a consensus that these two mechanisms are
in fact occurring in parallel. That can be seen in the so called “branching mechanism” proposed by Drazic,
28
which includes two parallel dissolution pathways: one resulting in a 40 mV Tafel slope and a first order
pH dependence, and the other with a 30 mV Tafel slope and a second order pH dependence. The author
suggested that the change of the mechanism between these two scenarios occurs with variation in the
adsorption energy of the intermediate species that are affected by the steel microstructure or the
environmental conditions. It was also suggested that the observed pH dependences ranging between 1
and 2 occurs when both mechanisms are at play simultaneously. A mechanism including parallel
pathways was also proposed in the more comprehensive work of Keddam et al. 24,25 The authors
proposed a mechanism including 7 elementary steps, resulting into 3 parallel dissolution pathways that
incorporated the elementary steps for both the consecutive and the catalytic mechanisms.

400
Passive
300

200
Potential vs. SHE / (mV)

100

-100
Pre-Passivation
-200

-300
Transition
-400
Actrive dissolution
-500
0.0001 0.001 0.01 0.1 1
Current density / (A.m-2)

Figure 2: Anodic polarization curve of iron in 0.5 M Na2SO4 solution at pH 5 and 298 ̊ K.
With the scan rate of 6.6 mV.s-1 and rotating disk electrode at 69 rps. Data taken from
El Miligy et al. 22

The anodic polarization curves obtained for mild steel dissolution in acidic CO2-saturated aqueous
environments have frequently been reported to have a 40 mV Tafel slope and a first order dependence
on hydroxide ion concentration. 9,10,33–35 The literature, as it relates to CO2 corrosion, appears to be settled
on the consecutive mechanism proposed by Bockris et al. 27 which has been frequently used to describe
the anodic currents without considering any effect of dissolved CO2 or the related carbonate species
present in the solution. 9,33,36–39

An in-depth analysis on the possible effect of dissolved CO2 and/or other carbonate species on the iron
oxidation reaction in acidic solutions is not available in the literature. Nevertheless, a significant effect of
carbonate species on the rate of iron dissolution has been mentioned in a few different studies over the
years 23,34,40–43. The rate of anodic dissolution of iron in mildly alkaline solutions was shown to be
increased in the presence of bicarbonate ions in several studies 41–43. It that pH range, the anodic
polarization curves showed that the iron dissolution reaction was at the passivation and trans-passivation
range. There is a general agreement in the literature that the increasing rate of anodic dissolution is a
result of chemical reaction of bicarbonate ion with the passive layer (e.g. Fe(OH)2 and Fe2O3) to form
various more soluble iron-complex species. 41–43

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5
 The effect of CO2 on the iron dissolution reaction was also studied by Linter and Burstein 40 at the pH
range more relevant to the present study (pH 4). It was reported that the rate of iron dissolution from 0.5
Cr alloyed steel increased significantly in the transition and pre-passivation range, while the active
dissolution range remained unaffected. Similar to what was proposed in previous works, 41–43 the authors
associated this effect to destabilization of the passive layer through a chemical attack and complex
formation by CO2 or its related carbonate species 40. In a study by Nesic et al. 23 the anodic polarization
curves were used to discuss the effect of CO2 in a relatively narrow potential range (~100 mV) above the
corrosion potential. Experiments were performed in acidic perchlorate solutions (pH 2 to pH 6), and partial
pressure of CO2 limited to the 0 to 1 bar range. The proposed mechanism by Nesic et al. suggests that
CO2 is actively engaged in the electrochemistry of iron dissolution by directly adsorbing onto the metal
surface and forming a chemical ligand that replaced the ferrous hydroxide intermediate species. The
authors suggest that the presence of CO2 did not affect the observed Tafel slopes, whereas the exchange
current densities increased with a linear proportionality to pCO2 up to 1 bar. Furthermore, it was noted
that as pCO2→1 bar, the effect of CO2 reaches its maximum and the rate of anodic reaction was not
further increased with increasing pCO2. In a more recent study, Almedia et al. 44 revisited this subject by
investigating the corrosion of X65 mild steel at pCO2=0, 1, and 30 bar. Based on electrochemical
impedance measurements at corrosion potential, the authors concluded that CO2 does not directly act
on the metal surface and it has no significant effect on the iron dissolution reaction, in contrast to what
was proposed by Nesic et al. 23 Nevertheless, considering that this mechanistic argument is developed
merely based on measurements at the corrosion potential and only at pH 4, the reported mechanistic
behavior may not be reasonably generalized to the wide range of conditions typically encountered in CO2
corrosion.

Despite the reported influence of CO2 on the iron dissolution reaction, the current narrative of the CO2
corrosion mechanism in the literature does not account for this mechanistic aspect. The present study is
an attempt to further elucidate the possible influence of CO2 or its related carbonate species on the rate
of steel dissolution in mildly acidic environments relevant to CO2 corrosion. The investigation of the anodic
behavior in the presence of CO2 complements the findings in the first part of this study on the cathodic
reactions, in order to provide a more inclusive description of the effect of CO2 on acidic corrosion of mild
steel.

EXPERIMENTAL PROCEDURE

The experiments were conducted in a thin channel flow cell (TCFC) described in detail elsewhere 45–49.
The test section was modified for electrochemical measurements by introducing a saturated Ag/AgCl
reference electrode facing the working electrode (3.175 mm apart), as shown in Figure 3. The TCFC
stainless steel structure was used as the counter electrode.

A 0.1 M NaCl supporting electrolyte solution (110 L), used throughout this study, was initially purged for
~ 3 hr, with N2 or CO2 gas depending on the experimental conditions, while the outlet gas was monitored
with an oxygen sensor (Orbisphere 410). Maximum dissolved oxygen content before initiating the
experiment was 3 ppb (typically ~1 ppb). For experiments at elevated pCO2, this deoxygenation step was
followed by pressurizing the system to 5 bar for at least 3 hr, or until a steady pH was obtained. As the
last step, the pH was adjusted to the target value by gradual addition of deoxygenated HCl or NaOH
solutions into the system. The temperature was controlled (±0.5oC) by means of electric heaters placed
in the tank and in the test section (used for experiments at 30oC) as well as a heat exchanger (used for
experiments at 10oC) connected to a chiller (Air-3000 FLUID CHILLERS Inc.). The pump output was fixed
throughout the experiments such that the flow velocity of 11 m.s-1 was obtained inside the thin channel
test section (3.3E-4 m2 cross sectional area).

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6
 The disk shaped working electrodes were made of API 5L X65 mild steel with the same chemical
composition as reported in our earlier study.14 Prior to each experiment, the electrodes were abraded
with a 600 grit silicon carbide paper and rinsed and sonicated in isopropanol for 5 minutes. After inserting
the working electrodes into the test section, the test section was purged using dry N2 or CO2 gas. After
introducing the solution into the test section, the measurements were carried out following a 15 min rest
at open circuit potential (OCP) in order to assure a stable readout. The polarization curves reported in
the present study were obtained using staircase voltammetry at 0.5 mV.s-1 scan rate and 1 s-1 sampling
period. The anodic and cathodic polarizations were obtained in separate experiments by sweeping the
potential from OCP towards more positive and more negative potentials, respectively. The reported
polarization curves were corrected for ohmic drop with the solution resistance obtained by
electrochemical impedance spectroscopy (EIS) measurements (DC potential 0 mV vs. OCP, AC potential
5 mV, frequency range 100KHz to 0.2 Hz at 10 points/dec), after polarization measurements and a 15
min rest so that a stable OCP was reached. The LPR measurements were also carried out in separate
experiments, following the above mentioned preparation sequence, using a ±5 mV potential range and
the scan rate of 0.125 mV.s-1.

Reservoir

Thin channel cell pump

test section Flow direction
Heat exchanger

Ag/AgCl reference
electrode

Thin channel cell

lid/counter
electrode
X65 mild steel
surface
Rubber seal

Thin channel cell

base/counter Working electrode
electrode assembly

Figure 3. The experimental setup and electrode arrangement inside the thin channel flow test
section.

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7
 RESULTS AND DISCUSSION

The experimental conditions were designed to improve the likelihood of observing the charge transfer
controlled cathodic currents, needed to verify one of the hypothetical behaviors shown in Figure 1. The
polarization curves obtained on API 5L X65 mild steel surface at pH 4 and pH 5 are shown in Figure 4.A
and Figure 4.B, respectively. These experimental results revealed a notable influence of CO2 on both
cathodic and anodic polarization curves.

(A) (B)
pCO₂ = 0 bar pCO₂ = 1 bar pCO₂ = 5 bar pCO₂ = 0 bar pCO₂ = 1 bar pCO₂ = 5 bar
-0.1 -0.1
120 120 mV
-0.2 pH 4 -0.2 pH 5
-0.3 -0.3
Potetnial vs. SHE / (V)

Potential vs. SHE / (V)

-0.4 -0.4

-0.5 -0.5

-0.6 -0.6

-0.7 -0.7

-0.8 -0.8

-0.9 -0.9

-1 -1
0.1 1 10 100 1000 0.1 1 10 100 1000
Current density / (A.m-2) Current density / (A.m-2)

Figure 4. Polarization curves at 30oC, 11 m.s-1, 0.1 M NaCl, 0.5 mV.s-1 scan rate on an X65
mild steel surface. A) pH 4, B) pH 5.

The effect of pCO2 on the cathodic limiting current density is now well understood. A detailed evaluation
of this parameter requires comprehensive calculations that accounts for the mass transfer of numerous
species and their interaction through homogenous chemical reactions inside the boundary layer.1,2
However, an estimate can be obtained considering that the magnitude of the limiting current density in
CO2 saturated solutions is the same whether carbonic acid was assumed to be electroactive or not.11,13
That suggests the kinetics of the carbonic acid dissociation reaction are fast enough so that the
concentrations of involved species reaches a quasi-equilibrium state. The reported experimental data in
the present study show that carbonic acid is not electrochemically active, as discussed further in the
following paragraphs. However, at mass transfer limiting conditions the surface concentration of carbonic
acid can be assumed to be close to zero since the local concentration of H+ is close to zero and that is
directly reflected on the concentration of carbonic acid through the homogenous dissociation reaction.
Therefore, while H2CO3 is not reduced directly, its flux can be calculated in the same fashion to that of
an electrochemically active species. Knowing that all the H2CO3 transferred to the surface is eventually
consumed through the H+ reduction reaction, the limiting current density can be expressed as the
superposition of the limiting current arising from the mass transfer of H+ and that of H2CO3.
The limiting current density can be obtained if the mass transfer coefficient is known. The mass transfer
coefficient (km) for a thin channel flow can be obtained via the same correlations proposed for pipe flow,
using the equivalent hydraulic length:50

𝑘𝑚 𝑙𝑒𝑞 (14)
= 𝑆ℎ = 0.0165 𝑅𝑒 0.86 𝑆𝑐 0.33
𝐷

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8
 where D is the diffusion coefficient (m2.s-1), Sh is the Sherwood number, Re is the Reynolds number, Sc
is the Schmitt number, and 𝑙𝑒𝑞 is the equivalent hydraulic length (m). The equivalent hydraulic length for
a thin channel flow was calculated using 4A/P=7.1 mm, where A (m2) is the flow cross section area and
P (m) is the wetted wall perimeter. The limiting current density of H+ was calculated using Equation ( 15
), where F (Col.eq-1) is the Faraday’s constant, and CH+ (mol.m-3) is the concentration of hydrogen ion:

𝑖𝑙𝑖𝑚,𝐻+ = 𝐹𝑘𝑚 𝐶H+ ( 15 )

The limiting current arising from H2CO3 was calculated via Equations ( 16 ) and ( 17 ) as discussed by
Nesic et al. 51, in order to account for the effect of CO2 hydration reaction.

𝑖𝑙𝑖𝑚,𝐻2 𝐶𝑂3 = 𝐹 𝐶H2 CO3 √𝑘ℎ𝑦𝑑,𝑏 𝐷 coth 𝜉 ( 16 )

𝐷⁄
𝑘𝑚
𝜉= ( 17 )
√𝐷⁄𝑘ℎ𝑦𝑑,𝑏

where km is the mass transfer coefficient from Equation (14), khyd,b is the rate constant of CO2 dehydration
reaction 52, 𝜉 is the ratio of the “mass transfer layer thickness” over the “chemical reaction layer thickness”,
and 𝐶H2 CO3 (mol.m-3) is the equilibrium concentration of carbonic acid that can be obtained as discussed
elsewhere 2,11. The total limiting current densities (𝑖𝑙𝑖𝑚,𝐻 + + 𝑖𝑙𝑖𝑚,𝐻2 𝐶𝑂3 ), calculated as described above,
were compared with those obtained experimentally as shown in Figure 5.

Calculated at 30°C Calculated at 10°C

Measurement at 30°C Measurement at 10°C
4.50E+01 45

4.00E+01 40
Limiting current density / (A.m-2)

3.50E+01 35

3.00E+01 30

2.50E+01 25

2.00E+01 20

1.50E+01 15

1.00E+01 10

5.00E+00 5

0.00E+00 0
pH 4, 0 bar pH 4, 1 bar pH 4, 5 bar pH 5, 0 bar pH 5, 1 bar pH 5, 5 bar
CO₂ CO₂ CO₂ CO₂ CO₂ CO₂

Figure 5 . The comparison of the experimental limiting current densities shown in Figure 4
(solid bars) with the calculated values (dashed bars). The error bars represent the standard
deviation of three measurements.

In Figure 4, the charge transfer controlled cathodic currents were to some extent observed at pH 4, which
were not significantly increased as the pCO2 was increased. Considering the aforementioned
hypothetical behavior (Figure 1.B), these results suggest that carbonic acid was not significantly reduced
during the cathodic polarization measurements. However, at pH 5 the cathodic currents were under mass
transfer/chemical reaction control at all pCO2 values, hence, the hypothesis could not be properly verified.

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9
 Over the anodic current range, the polarization curves showed a significant effect of pCO 2 on the
electrochemical behavior of the iron dissolution reaction. Considering the categorization of El Miligy et
al., 22 the results reported in Figure 4 only show the transition and the pre-passivation ranges, while the
active dissolution range was covered by the cathodic currents. As shown by the guidelines in Figure 4,
the pre-passivation range was found to be reasonably quantified with a 120 mV Tafel slope. The
guidelines were used to obtain the reaction order versus pH and pCO2. Comparing the anodic curves
where no CO2 was present showed a negligible dependence on the solution pH, which was found to
agree with that previously reported in the literature. 22,53,54 In the presence of CO2, while the Tafel slope
in the pre-passivation range was not affected, reaction orders of 0.34 and 0.61 vs. pCO2 were observed
at pH 4 and pH 5, respectively.

In order to improve the likelihood of observing the effect of CO2 on the charge transfer cathodic currents
and the anodic currents at the active dissolution range, a set of experiments at a lower temperature
(10oC) were conducted in the present study. Decreasing the temperature was expected to influence the
observed polarization curves though number of different processes:

a) The mass transfer coefficient and the rate of hydration reaction would decrease by decreasing
the temperature (decreasing the limiting current), while the solubility of CO 2 in water increases
(increasing the limiting current).
b) The charge transfer controlled currents would decrease exponentially, following the Arrhenius
law.

Overall, one could expect that the charge transfer controlled currents to decrease with decreasing
temperature more effectively than the limiting currents would, which broadens the potential range where
one can observe the charge transfer controlled currents. Additionally, decreasing the rate of both anodic
and cathodic reactions at a low current density range would reveal more details of the kinetics of iron
dissolution in the active dissolution range.

T = 10° C T = 30° C
-0.1

-0.2
28 mV
-0.3
Potential vs. SHE (V)

-0.4

-0.5

-0.6

-0.7

-0.8

-0.9

-1
0.1 1 10 100 1000
Current density / (A.m-2)

Figure 6. Temperature dependence of polarization curves at pH 4, pCO2=0 bar, 11 m.s-

1
, 0.1 M NaCl, 0.5 mV.s-1 scan rate on X65 mild steel surface.
The effect of temperature on polarization curves obtained on X65 mild steel at 10oC and 30oC is shown
in Figure 6. The results at 10oC showed a clear Tafel behavior for the cathodic currents, indicating a
charge transfer controlled range. Additionally, a linear range in anodic currents with the Tafel slope of
~28 mV was observed, which is associated with the active dissolution range for the anodic reaction. The
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10
 clear separation between the cathodic and anodic currents observed at lower temperature provides a
great opportunity for better understanding the effect of CO2 on the electrochemical behavior of iron in
acidic solutions.

The polarization curves obtained at 10oC, various pCO2, and at pH 4 and 5 are shown in Figure 7.A and
B, respectively. Over the cathodic current range, at pH 4, the charge transfer controlled current (Tafel)
range were clearly observed at all pCO2 values up to 5 bar, and were not significantly affected by the
presence of CO2. This behavior was similar to that observed at 30oC (Figure 4.A) and the hypothetical
behavior shown in Figure 1.B that further supports the argument that carbonic acid was not reduced on
the X65 mild steel surface during cathodic polarization. At pH 5 and pCO2=0 bar, the cathodic currents
were still under mass transfer control at 10oC, however, the charge transfer controlled currents were
observed at pCO2=1 bar and pCO2=5 bar. Here also the results suggest that increasing CO2 partial
pressure does not significantly increase the charge transfer controlled cathodic currents and that the so
called “buffering effect” is the governing mechanism for carbonic acid contribution to the cathodic
currents.

(A) (B)
pCO₂ = 0 bar pCO₂ = 1 bar pCO₂ = 5 bar pCO₂ = 1 abr pCO₂ = 1 bar pCO₂ = 5 bar

120 mV 120 mV
-0.20 pH 4 -0.20 pH 5
22 mV
22 mV
-0.40 -0.40
Potential vs. SHE / (V)
Potetnial vs. SHE / (V)

60 mV

-0.60 -0.60

-0.80 -0.80

-1.00 -1.00

-1.20 -1.20
0.1 1 10 100 1000 0.1 1 10 100 1000
Current density / (A.m-2) Current density / (A.m-2)

Figure 7. Polarization curves at 10oC, 11 m.s-1, 0.1 M NaCl, 0.5 mV.s-1 scan rate on an X65
mild steel surface. A) pH 4, B) pH 5.

Over the anodic current range, the polarization curves obtained at 10oC also showed the significant
influence of CO2 or, what is more likely, its associated carbonate species, on the kinetics and the
mechanism of iron dissolution reaction. Figure 8 demonstrates the effect of pH on the observed anodic
polarization curves obtained at 10oC and 30oC. At 30oC, only the transition and the pre-passivation ranges
were observed, while the anodic polarization curves obtained at 10oC clearly demonstrate a range of
anodic currents associated with the active dissolution range, in addition to the transition and pre-
passivation range. The electrochemical behavior at the pre-passivation range is similar to that observed
at 30oC. At the active dissolution range, a ~28 mV Tafel slope and a ~ -1.5 reaction order vs. H+
concentration was observed.

The effect of pCO2 on the iron dissolution reaction at pH 4 and pH 5 are shown in the polarization curves
reported in Figure 7.A and Figure 7.B, respectively. In these graphs the active dissolution, transition and
the pre-passivation ranges were observed clearly, while pCO2 was shown to have a profound effect over
the whole range. In the presence of CO2, the Tafel slope in the active dissolution range slightly decreased
from ~28 mV (in Figure 8) to ~22 mV (in Figure 7). The decrease in the Tafel slope in this range remained
the same at higher CO2 partial pressures. Furthermore, in the transition range, an additional linear

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11
 behavior with Tafel slope of ~60 mV was observed (most clearly at pH 4 and 5 bar CO2). The pre-
passivation range was also significantly affected by the pCO2. In that range, the Tafel slope was ~120
mV for all pCO2 values, similar to what observed at 30oC. The reaction orders vs. pCO2 of 0.39 and 0.30
were observed for pH 4 and pH 5, respectively, which were somewhat lower than that observed at 30oC.

pH 4 - 30 C pH 5- 30 C pH 4 - 10 C pH 5 - 10 C
-0.10
120 mV
-0.15

-0.20
Potential vs. SHE (V)

-0.25

-0.30
28 mV
-0.35

-0.40

-0.45

-0.50
0.01 0.1 1 10 100 1000
Current density / (A.m-2)

Figure 8. Anodic polarization curves at 11 m.s-1 flow rate, 0.1 M NaCl, 0.5 mV.s-1 scan
rate on an X65 mild steel surface. Error bars represent the minimum and maximum
values obtained in at least three repeats.

The observed influence of CO2 on anodic reaction in active dissolution range was found to partially agree
with the results reported by Nesic et al. 23 in the sense that the presence of CO2 resulted in an increased
rate of reaction which was not further intensified at pCO2>1. However, in the present study the effect was
in the form of a slight change of Tafel slope. Despite the fact that this effect was quantitatively small (only
~6 mV), it could still imply a change of mechanism. The 28 mV Tafel slope which correlates well with
1/2×2.303RT/F, is a characteristic of an electrochemical reaction preceded by one or more elementary
steps, whereas the 22 mV Tafel slope (2/5× 2.303RT/F) may suggest an electrochemical reaction
preceded by two or more elementary steps.

The significant increase of the anodic reaction rate in the transition and pre-passivation ranges appears
to be in agreement with the results reported previously by Linter and Burstein.40 In that study, the authors
suggested that the increased rate of iron dissolution was a result of the destabilization of the passive
layer, Fe(OH)2 or Fe2O3 species, through a chemical attack by bicarbonate ion, similar to that proposed
for the alkaline pH range.41–43 Such an explanation may not be assumed to be valid for the conditions of
the present study, considering that the formation of a passive layer on a mild steel surface is not
thermodynamically favored at the pH and potential range of interest. 55 However, a rather similar chemical
interaction of CO2 or other associated carbonate species could be feasible for the conditions in the
present study. The previously proposed mechanism of iron dissolution in acidic solutions without CO2
suggests that the first current maximum observed in the polarization curves is associated with
accumulation of the reaction intermediate Fe(I), i.e. FeOH, on the metal surface. 24,25,31 Keddam et al.
suggest that the increased current after the first arrest is a result of a parallel reaction pathway involving
Fe(II) intermediate species. 24,25,31 The second current maximum at more positive potentials leading to
the surface passivation (not observed in the polarization curves presented here), was associated with a
chemical transformation of Fe(II) intermediates into insoluble passivating species, e.g. Fe(OH)2. 31
Therefore, the increase of current at the first peak could possibly be explained by an interaction of
dissolved carbonate species with Fe(I) reaction intermediate, providing an additional chemical desorption

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12
 pathway for this species that could increase the observed current densities at the first peak. However,
the observation of an additional 60 mV Tafel slope range below the first peak and the continuous increase
of the exchange current density at the 120 mV range could also be a strong indication of electrochemical
reactions where carbonate intermediate species are involved.

Developing a detailed mechanism for the iron dissolution reaction at these conditions requires a
comprehensive investigation on the subject, considering the complexity of the reaction. However, the
results presented here demonstrate a significant effect of CO2 on the rate and the mechanism of iron
dissolution in acidic environments. The more strongly influenced transition and pre-passivation ranges
are of particular interest in the typical CO2 corrosion scenarios. As shown in Figure 4, at pH values of 5
and higher, even at 30°C, the corrosion current is in the transition/pre-passivation range. The polarization
curves clearly indicate that the effect of CO2 on the anodic reaction rate is as significant as its effect on
the cathodic limiting current density.

Effect of pCO2 on corrosion rate

The effect of pCO2 on corrosion rate of X65 mild steel was further discussed based on the experimental
data obtained by LPR measurements. The change in corrosion rates with respect to CO 2 partial pressure
at pH 4 and pH 5 are shown in Figure 9.A and B, respectively. The observed behavior was found to agree
well with the abovementioned mechanistic discussion. At pH 4, increasing pCO2 from 0 to 5 bar only
resulted in a minor increase in the corrosion rates. In these conditions, the cathodic currents were under
charge transfer control. Considering that carbonic acid was not directly reduced, increasing pCO2 was
not expected to result in any higher cathodic current. The minor increase of corrosion rates are associated
with the slight increase of the anodic reaction rate in the active dissolution range by introducing CO2.

The corrosion rates obtained at pH 5 demonstrate a rather different trend. At 10oC, as shown in Figure
9.B the cathodic currents were under charge transfer control, and anodic currents were in the active
dissolution range. Hence, increasing pCO2 did not result in significantly higher corrosion rates, similar to
that observed at pH 4. On the other hand, at 30oC, the cathodic currents were under mass transfer control
and the anodic currents were in the transition range, therefore, increasing pCO2 significantly increased
the observed corrosion rates from 2.8 mm.y-1 at pCO2=0 bar to 13.2 mm.yr-1 at pCO2=5 bar, by increasing
both the mass transfer limiting current and the rate of anodic reaction in transition state.

A) B)
10°C 30°C 10°C 30°C
Corrosion rate / (mm.yr-1)

Corrosion rate / (mm.yr-1)

10 10

1 1

0.1 0.1
0 1 5 0 1 5
CO2 partial pressure / bar CO2 partial pressure / bar

Figure 9: Corrosion rates obtained at 11 m.s-1 flow rate and 0.1 M NaCl on X65 mild steel
surface at 10oC and 30oC: A) pH 4, B) pH 5.

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13
 CONCLUSIONS

The polarization behavior of API 5L X65 mild steel at various pH and pCO2 values was investigated at a
high flow velocity and temperatures 30oC and 10oC. The electrochemical behavior of the cathodic and
anodic reactions suggested that:
1- The direct reduction of carbonic acid was negligible. Therefore, the effect of CO2 on the cathodic
currents is primarily reflected on the limiting current, which increases due to: CO2 hydration
reaction that replenishes the surface concentration of carbonic acid and carbonic acid dissociation
that buffers the H+ concentration at the metal surface.
2- The rate of iron dissolution reaction was significantly increased in the presence of CO2, suggesting
that the mechanistic description previously developed in acidic aqueous solutions is not valid
when CO2 is present. The profound effect of CO2 on anodic currents suggests that CO2 or its
related carbonate species are directly involved in the iron dissolution reaction.
3- Considering the abovementioned findings, the increased corrosion rates of mild steel in acidic
solutions in the presence of CO2 are due to the increased rate of iron dissolution in presence of
CO2, in addition to the increased cathodic limiting currents resulting from the buffering ability of
dissolved CO2 and H2CO3.

ACKNOWLEDGEMENTS

The author would like to thank the following companies for their financial support:
Anadarko, Baker Hughes, BP, Chevron, CNOOC, ConocoPhillips, DNV GL, ExxonMobil, M-I SWACO
(Schlumberger), Multi-Chem (Halliburton), Occidental Oil Company, Petrobras, PTT, Saudi Aramco,
Shell Global Solutions, SINOPEC (China Petroleum), TransCanada, TOTAL, and Wood Group Kenny.

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