Corrosion Science 64 (2012) 37–43

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Corrosion Science
journal homepage: www.elsevier.com/locate/corsci

An electrochemical investigation on the effect of the chloride content on CO2

corrosion of API-X100 steel
Faysal Fayez Eliyan ⇑, Farzad Mohammadi, Akram Alfantazi
Corrosion Group Department of Materials Engineering, The University of British Columbia, Vancouver, BC, Canada V6T 1Z4

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

Article history: This research argues that the corrosion rate for high strength steel in CO2-saturated solutions reaches a
Received 13 February 2012 maximum at a threshold chloride content. At 20 °C, the corrosion rates increased from 60 lA/cm2 in 5 g/L
Accepted 23 June 2012 solutions to a maximum of 185 lA/cm2 in 15 g/L solutions, and then became less in the more concen-
Available online 10 July 2012
trated solutions. The anodic dissolution accelerated at 90 °C and the cathodic reactions decelerated with
adding 10 vol.% oil where the chloride content effect remained relatively the same. Some EIS experiments
Keywords: demonstrated an agreement with the polarization results without confirming that threshold effect of
A. API-X100
chloride on charge transfer.
A. CO2
A. Oil
Ó 2012 Elsevier Ltd. All rights reserved.
B. Polarization
B. EIS
A. Chloride

1. Introduction techniques in many important papers to come, seems not to corre-

Carbon dioxide corrosion is a main contributor to many opera-
tion problems difficult to predict or control for oil pipelines [1]. It is
almost inevitable, and of course dependent on many interrelated
physicochemical factors whose interactions with a steel type are
till today a subject of ongoing research [2]. In the first place; carbon
dioxide dissolves [3], to extents dependent on its partial pressure
and temperature, in the water phase to principally result in
H2CO3. Along with other carbon carrying species, pH decreases in
a situation where corrosion occurs at higher rates and becomes
governed by the cathodic reactions [4]. A potential severity with
the flow chemistry is the chloride whose content is typically high
[5], and its effect – at least in accelerating the reactions – is widely
recognized both in the field and across CO2 corrosion research
community [6–10].
In recent years, potentiodynamic polarization and EIS tech-
niques proved reliable in analyzing CO2 corrosion reactions, and
in providing comparable rates to the conventional immersion cor-
rosion rates of between 0.05 and 0.5 mm/yr. Moreover, it seems
that the complexities of the environmental conditions, added to
the stricter safety regulations and the growing demand for pipeline
oil supply; make the researchers concerned mainly in simulating
field flows without giving attention to specific – but basic – chem-
ical considerations that might carry a scientific weight. That rush,
despite its successful deployment of the electrochemical
⇑ Corresponding author. Tel.: +1 778 997 4878.
E-mail address: faysal09@interchange.ubc.ca (F.F. Eliyan).
late the corrosion behavior to the contents of chemical constitu-
ents in specific; chloride included. Although studying the content
effect solely of chloride, bicarbonate, sulfate, etc. in CO2-saturated
solutions for the purpose of understanding situations in a pipeline
flow would not be well relevant to a real situation, however; a
good simulation seems to discourage tenets – if not to hide paths
– that lead find good insights. From the literature survey prior to
submitting this work and others [11,12], we fundamentally re-
garded chloride as an aggressive agent capable of destabilizing
the corrosion layers, initiating and increasing localized corrosion
rates in CO2-saturated media.
Examining the effects of the chloride content in 1-bar-CO2-sat-
urated solutions at 20 °C lead us to argue that there must be an
optimum chloride content at which CO2 corrosion rate is maxi-
mum. Measuring the corrosion rates in solutions containing 5–
80 g/L chloride on a 5 g/L-increment revealed they increased from
almost 60 lA/cm2 in 5 g/L solutions to reach a maximum 185 lA/
cm2 in 15 g/L solutions, and then were less and decreasing with
the increased chloride content of up to 80 g/L.
We believe our results resolve a big deal of controversy and
confusion from corrosion rates calculated either from complex
CO2 solutions [13], or from solutions did not contain broad ranges
of proportionate chloride contents [14]. Actually, both Papavina-
sam et al. and Fang et al. performed electrochemical experiments
in highly saline CO2-saturated brines, but the results of the formers
imply an increase, while the results of the latters imply a decrease
of the corrosion rates if the chloride content is higher! For a pipe-
line to be protected against complex flows they both established a

0010-938X/$ - see front matter Ó 2012 Elsevier Ltd. All rights reserved.
http://dx.doi.org/10.1016/j.corsci.2012.06.032
38 F.F. Eliyan et al. / Corrosion Science 64 (2012) 37–43

knowledge reliable to control corrosion, but the effect of the great

amounts of chloride remained somewhat vague. The electrochem-
ical effect of chloride – discounting pitting susceptibility and
changes with surface layers – cannot be fully understood in solu-
tions prepared to study 11 factors or in solutions did not contain
proportionate increments of chloride introduced with 3–25 wt.%.
In addition to the deceleration of the cathodic reactions, re-
ported before by Fang et al., we now report a decrease in the cor-
rosion potentials with the chloride content. And to establish some
relevance to the field, we introduced 10 vol.% light diesel fuel in
experiments repeated at 90 °C as well, measuring the corrosion
rates and reporting how different the behavior was from the major
20-°C, oil-free cases. We performed EIS experiments to find some
consistency between polarization and the free corrosion behavior.
API-X100 steel is a new pipeline infrastructure material and receiv-
ing a growing interest, and due to its special alloying composition
its corrosion resistance would be better and so would be the re-
search interest.
Fig. 1. The optical micrograph of the microstructure of API-X100.
2. Experimental details

2.1. Corrosion test setup

A standard three-electrode 1-L glass jacketed cell was selected
for the experiments. A saturated calomel electrode (SCE), which
the potentials were measured against, was kept isolated in a capil-
lary bridge at room temperature. Prior to performing the experi-
ments, the solutions were fully deoxygenated through which
carbon dioxide during the experiments was purged. The cell was
tubed to a heating unit which circulates a constant-velocity water
flow to heat the solutions for the 90-°C experiments. A constant-
speed rotating magnetic bar was used to homogenize solutions
that contained oil. A PAR Versatstat 4 potentiostat, synchronized
to VersaStudio software was our reliable electrochemical setup.
2.2. Test material
The test coupons were machined out of API-X100 pipeline shell
made by EVRAZ Inc. They were soldered to copper wires by a con-
ductive silver paste and mounted in hard epoxy resins which were
reliable at high temperature, and therefore there was no possibility
for crevice attack to occur. 120-, 320-, 600-grit emery papers were
used to wet grind the samples. They were ultrasonically degreased
with ethyl alcohol and rinsed with distilled water and dried in an
air stream. The chemical composition, shown in Table 1, was car-
ried out by inductive coupled plasma (ICP) and LECO carbon anal-
ysis. The microstructure is shown in Fig. 1. It was revealed from a
sample wet ground to 1200-grit emery finish and polished with 6
and 1 lm diamond suspensions. The sample was then immersed in
a Nital etchant (2 ml of 70% nitric acid and 98 ml of anhydrous,
denatured ethyl alcohol), and treated with alcohol swapping and
dried in an air stream. The microstructure consisted of a mixture
of ferrite, pearlite and bainite with slight microvariations in color.
2.3. Test solutions
with a 1-bar CO2 flow. The pH of the solutions was acidic and
unbuffered of between 4.2 and 4.8. For the test emulsions, ShellÓ
diesel fuel of 10 vol.% was emulsified with a 0.2-wt.% anionic sur-
factant dioctyl sulfosuccinate sodium (C20H37NaO7S) to homoge-
nize the solutions. The selection of the surfactant with that
amount was considered to our emulsions assuming no significant
adsorption interfering with that of oil, and considering its success-
ful use by Quiroga Becerra et al., and Zhang et al. in similar emul-
sions [15,16]. We performed some experiments in N2-saturated
solutions and in chloride-free solutions for comparison with the
main case of our subject. A 0.5-wt.% sodium sulfate was added to
the chloride-free solutions to make them conductive for the elec-
trochemical tests. It should be noted the hydrocarbon was less mis-
cible as the chloride content was higher, and so was at 90 °C.
Selected properties of the hydrocarbon are presented in Table 2.
2.4. Electrochemical tests
Before commencing the experiments, a 2 V vs. SCE potentio-
static cathodic conditioning for 2000 s was performed for all sam-
ples immediately after immersion in the solutions. The
experiments were repeated for many times to ensure reproducibil-
ity. We performed OCP tests for about 7000 s before analyzing the
polarization and EIS results. The potentiodynamic polarization
scan was 0.5 mV/s in an upward direction from 1.2 to 0.4 V
vs. SCE. The EIS tests were performed at the open circuit potentials,
0.8 V and 1.2 V vs. SCE, from 10,000 to 0.01 Hz with a sampling
rate of 10 points per decade.
Table 2
Properties of the ShellÓ diesel fuel emulsified with 10 vol.% in the test solutions.

Property Details
The test solutions were made with double-distilled deionized
water with different amounts of chloride, continuously purged Appearance Green
Carbon number C4–C12
Initial boiling point (°C) 25
Table 1 Boiling range (°C) 25–170
Chemical composition of the test material. Flash point (°C) >10
Lower/upper flammability (%V) 1–6
Composition (wt.%) C.E. Auto-ignition temperature (°C) >250
Vapor pressure (kPa) <38 at 20 °C
C Mn Mo Ni Al Cu Ti Nb Cr V
Density (g/cm3) 0.63 at 15 °C
0.1 1.67 0.21 0.13 0.02 0.25 0.01 0.043 0.016 0.003 0.47 Kinematic viscosity (mm2/s) 0.5–0.75 at 40 °C
 F.F. Eliyan et al. / Corrosion Science 64 (2012) 37–43 39

3. Results and discussion Fe þ 2H2 O ! FeðOHÞ2 þ 2Hþ þ 2e ð1Þ

and
3.1. OCP and potentiodynamic polarization tests
Fe þ 2H2 CO3 ! FeðHCO3 Þ2 þ H2 ; ð2aÞ
The OCPs were almost between 640 and 720 mV vs. SCE,
tending to be less with higher chloride content and at 90 °C. Oil,
FeðHCO3 Þ2 ! Fe2þ þ 2HCO3 ; ð2bÞ
more effective in the dilute solutions, made the OCPs in many of
the repeated experiments less than these in oil-free conditions.
Our high-temperature OCPs were closely within the range of the HCO3 ! Hþ þ CO2
3 ; ð2cÞ
longer-time OCP tests performed by Moiseeva et al. in similar con-
ditions [17]. We found, on all samples, intact gray–black layers Fe2þ þ CO2
3 ! FeCO3 ð2dÞ
whose formation could be well consistent with the valuable mech-
The potentiodynamic experiments were performed on fresh
anistic information Moiseeva et al. introduced in the beginning of
samples after being conditioned at 2 V vs. SCE for a period of
their paper. They believed that during the free conditions the pro-
time. Within a proper potential range and scan, some key charac-
portions between the oxide, hydroxide, and carbonate components
teristics of the anodic and cathodic kinetics appeared useful to
of the black layer undergo critical changes, probably responsible
handle our case. In Fig. 2, selected polarization profiles from
for the OCP changes over a long period of time. Since the pH in
20 °C conditions are shown together with the full corrosion poten-
our cases was well below 6, we cannot regard bicarbonate a key
tial and current data. The polarization behavior in the chloride-
oxidizer during the free conditions. But rather, as mentioned in
containing solutions was similar except that the corrosion rates
many CO2 corrosion studies [18–20], we generally regard the ano-
were chloride-dependent. Yet we do not know, in comparison to
dic dissolution and film formation being governed by the two
the chloride-free conditions whose rates were the lowest, how
simultaneous processes:
chloride exposed the cathodic regimes as being driven by at least
two reduced species, H2CO3 and H2O.

Fig. 2. Potentiodynamic polarization, and corrosion rates and potentials at 20 °C. Fig. 3. Potentiodynamic polarization, and corrosion rates and potentials at 90 °C.
40 F.F. Eliyan et al. / Corrosion Science 64 (2012) 37–43
Between 1.2 and 1 V vs. SCE, water is reduced in a charge-
transfer-limited fashion below H2CO3 and H+ were reduced at al-
most between 140 and 300 lA/cm2 limiting current densities.
The anodic dissolution currents accelerated with the overpotential
before showing, in the chloride-containing solutions, a decelera-
tion at about 0.5 V vs. SCE. A black intact film was found at the
end of the polarization on all samples. The corrosion current den-
sities (icorr) were iteratively calculated by Butler–Erdey–Grúz–Vol-
mer equation [21] (Eq. (3)), fitted with the ± 20 mV polarization
from the corrosion potentials.
   
2:3gs 2:3gs
i ¼ icorr exp  exp½  ð3Þ
ba bc
The corrosion rates, higher by about 40 lA/cm2 in the chloride-
free conditions, increased from about 60 lA/cm2 in 5 g/L, to
150 lA/cm2 in 10 g/L, and to 185 lA/cm2 in 15 g/L solutions in
which the corrosion rates were the maximum. The corrosion rates
were always less with the higher chloride content up to about 40 g/
L, and becoming finally almost insensitive of about 120 lA/cm2 in
the more concentrated solutions. The corrosion potentials being
less – from about 650 to 750 mV vs. SCE – with the increased
chloride content was of a good kinetic value in analyzing the
Fig. 4. Potentiodynamic polarization, and corrosion rates and potentials at 20 °C in
N2-saturated solutions.
chloride effect on the anodic and cathodic reactions. In other
words, that trend, which was actually reproducible, supports two
assumptions that the chloride, if introduced with few amounts, in-
creases the anodic sensitivity to result in an increase in the corro-
sion rates. Moreover, increasing the chloride content above a
threshold value makes the corrosion rates less in a manner the cor-
rosion polarization becomes governed by the cathodic reactions.
The notion that CO2 corrosion is originally governed by the catho-
dic reactions is uncontroversial and becoming more valid in many
mechanistic studies. We therefore believe the decrease of the cor-
rosion rates in our case is attributed to the deceleration of the
cathodic reactions for reasons difficult to determine. However that
encourages us, in future studies, to link the electrochemical results
to the main physical and compositional characteristics of corroding
interfaces. Deploying a good method to investigate some interfa-
cial aspects, with precise electrochemical measures, could help
understand the dependence of the cathodic reactions on the chlo-
ride content. That could be pursued together with benefiting from
the information on the cathodic dependence on the microstructure
and composition in similar conditions [22–24]. We also stress on
the need for special studies on the chloride effect on the polariza-
tion right above 1 V vs. SCE to CO2 corrosion potentials. Such
studies could lead to better understanding on the effects of the
solution conductivities and the interactions between chloride ions,
H+ and H2CO3 on CO2 corrosion.
The polarization behavior at 90 °C was similar to that at 20 °C,
but the anodic reactions accelerated. As a result, the corrosion rates
were higher – by almost three times – and the corrosion potentials
were lower – by almost 30–40 mV. We did not handle the high-
temperature cases with the same incremental chloride contents,
but despite of some discrepancy, the corrosion rates reached max-
ima in the dilute solutions of 5–20 g/L. The cathodic polarization,
as shown in Fig. 3, seemed to be more governed by mixed
charge-and-mass-transfer-limited reduction in the region above
1 V vs. SCE. Regardless of temperature, there was an interesting
short upright anodic overpotential exclusively in the highly con-
centrated solutions. That behavior, which is dependent on the high
chloride content, requires to be explained by a special physical
investigation.
Fig. 5. Potentiodynamic polarization at 90 °C in oil-containing solutions.
 F.F. Eliyan et al. / Corrosion Science 64 (2012) 37–43
We performed some experiments in N2-saturated solutions at
20 °C and, as shown in Fig. 4, the corrosion rates and potentials
were notably lower than these in CO2 solutions. As being princi-
pally governed by the water reduction in higher-pH solutions,
the cathodic current densities were less than in the CO2-solutions
and the corrosion rates appeared proportional with the chloride
content. That was contrary to what was found in the CO2 solutions
suggesting that the deceleration of the cathodic reactions, and con-
sequently the corrosion rates, with the chloride content is a special
case with CO2 corrosion. In the anodic branch, the current densities
showed a considerable upright deceleration for a wide potential
range corresponding possibly to the formation of hydroxide-based
films. The currents showed, regardless of the chloride content, an
acceleration at almost the same 0.72 V vs. SCE.
The current densities decelerated at the presence of 10 vol.% oil.
Being more effective at 20 °C and in the dilute solutions, oil re-
duced the corrosion rates by as much as 30–60% at 20 °C and by
not more than 10% at 90 °C. It should be noted that both corrosion
potentials and current densities changed with the chloride content
Fig. 6. EIS spectra at 20 °C at open circuit potentials.
41
in a manner relatively similar to that in oil-free solutions. Regard-
less of the chloride content and temperature, the corrosion poten-
tials were lower than these in the oil-free solutions suggesting oil
is a cathodic inhibitor. The difference was however much less at
90 °C and in the concentrated solutions. As shown in Fig. 5 for
90 °C conditions, oil caused some fluctuations in the cathodic
currents and, as was appreciably the case at 20 °C, the cathodic
shoulders extended to be more under a mixed-reduction control.
We like to mention that we saw, at low potentials, the intense
high-temperature hydrogen evolution passing through metastable
oil films by which we can relate that to cathodic fluctuations. We
found at the end of the polarization some oil well adsorbent on
the black layers, encouraging future investigations on the effect
of oil on the filming process probably could be best understood
by slower potentiodynamic polarization.
Fig. 7. EIS spectra at 20 and 90 °C, at (a) 0.8 V and (b) 1.2 V vs. SCE.
42 F.F. Eliyan et al. / Corrosion Science 64 (2012) 37–43
3.2. EIS tests
Some EIS tests were performed to study the chloride effect on
the double layer and charge transfer, and to find any consistency
with the polarization results. The tests were performed after a
short time of immersion after the cathodic conditioning in the
open circuit potentials and in 0.8 and 1.2 V vs. SCE. The capac-
itive, relatively overlapped Nyquist spectra, shown in Fig. 6 for
20 °C, suggest the interactions were mainly governed by adsorp-
tion. Supported by similar EIS measurements reported by Chen
et al. [25], we believe adsorption was sustained by iron intermedi-
ates originated from multi-step dissolution. Our understanding,
based actually on the chloride content effect, would be better to al-
low articulate on the hydrogen evolution –normally driven by
charge transfer and affected by the physical transitions [26]–
should we have performed successive experiments over a specified
long period of time. Rather, we now regard the chloride content – a
research keyword– as being not the strong factor with which the
mechanism of dissolution or reduction would change. The Nyquist
amplitudes – which actually reflect the charge transfer resistance
[27] – were not as reproducible with respect to a given chloride
Fig. 8. EIS spectra at 20 °C in oil-containing solutions.
content as were the interesting potentiodynamic trends. Abiding
to the assumption that adsorption in our case drove the interac-
tions; it appears difficult to propose how chloride affects the pro-
cess or what the mechanistic aspects are ready to change with
respect to the chloride content. However, the EIS results were use-
ful in knowing charge transfer resistance decreased generally with
the chloride content and as clearly did the solution resistance. The
EIS was fitted with a nested {R(Q(R(QR)))} equivalent circuit. It was
applicable to fit the experimental data and it showed both the dou-
ble layer and adsorption were highly capacitive. At 90 °C, the spec-
tra were similar, but smaller than these in 20 °C solutions. The
charge transfer resistance was also three times less and the phase
peak location and intensity were more related to the chloride con-
tent. Recognizing the importance of the cathodic reduction, some
EIS tests were performed at 0.8 and 1.2 V vs. SCE during which
the mass-transfer-limited reduction of H2CO3 and H+, and charge-
transfer-limited reduction of H2O occur, respectively. The spectra,
shown in Fig. 7, depicted clear evidence the course of the cathodic
reactions, at least from the electrochemical perspective at these
low potentials, is independent from the chloride content. It would
be interesting that EIS of 0.8 V vs. SCE was under diffusion control
while that of 1.2 V vs. SCE was clearly under adsorption control as
water was reduced at high rates. The spectra of both potentials at
90 °C were apparently smaller. Oil, as shown in Fig. 8, made EIS
inductive at the low-frequency regions, and increased markedly
the charge transfer resistance. The charge transfer resistance de-
creased with the chloride content and was lower at 90 °C. The
phase peaks appeared at about 10 Hz and some little valleys ap-
peared at the low-frequency regions.
4. Conclusion
This research is a special electrochemical corrosion study on the
behavior of API-X100 steel in saline CO2-saturated solutions. Inves-
tigating 5-to-80-g/L chloride effect, the corrosion rates were higher
to reach a maximum in 15 g/L solutions, and were less in the rest of
the more concentrated solutions at 20 °C. The corrosion potentials
were less with the chloride content. The corrosion rates increased
at 90 °C and the potentials were lower. Oil decelerated the corro-
sion rates and acted as a cathodic inhibitor. The EIS experiments
showed that the interactions were governed by adsorption, and
the charge transfer resistance decreased with the chloride content
and at 90 °C.
Acknowledgment
The authors sincerely thank Qatar National Research Fund
(QNRF) for the financial support to carrying out this pipeline corro-
sion research.
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