Materials Chemistry and Physics 140 (2013) 508e515

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Materials Chemistry and Physics

journal homepage: www.elsevier.com/locate/matchemphys

Influence of temperature on the corrosion behavior of API-X100

pipeline steel in 1-bar CO2-HCO

3 solutions: An electrochemical
study
Faysal Fayez Eliyan*, Akram Alfantazi
Corrosion Group, Department of Materials Engineering, The University of British Columbia, Vancouver, BC V6T 1Z4, Canada

h i g h l i g h t s

 An increase in the corrosion rates with bicarbonate concentration and temperature.

 High temperature anodic peaks are compared with standard potentials of formation of iron oxides.
 Adsorption-controlled and diffusion-controlled EIS interactions at the OCPs and 0.6 V vs. SCE, respectively.

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

Article history: This paper addresses on the influence of temperature, elucidated with a number of electrochemical
Received 12 October 2012 methods and immersion tests, on the corrosion behavior of API-X100 steel in CO2-saturated bicarbonate
Received in revised form solutions. Investigated by cyclic potentiodynamic polarization, the corrosion rates, which showed a
23 February 2013
sensible increase with 10 g L
1 (0.16 mol L
1), 30 g L
1 (0.5 mol L
1) and 50 g L
1 (0.82 mol L
1) bi-
Accepted 23 March 2013
carbonate concentrations, increased from about 500, to 1500 and 1800 mA cm
2 at 20, 50 and 90  C,
respectively. Passivation at 50 and 90  C showed resistance to deteriorate against 100 ppm chloride ions,
Keywords:
of which anodic 0.5 V vs. SCE peaks exclusively appeared. Moreover, transpassivation occurred at 0.9 and
Metals
Electrochemical techniques
0.7 V vs. SCE, respectively, unlike with the 20  C cases whose chloride-induced-pitting-vulnerable,
Energy dispersive analysis of X-rays gradually-forming passive films transpassivated at 1 V vs. SCE. At different potentials, the potentiostatic
Corrosion currents increased with temperature, but their profiles suggested more effective passivation, accordingly.
The charge transfer resistance, calculated by electrochemical impedance spectroscopy, decreased with
temperature at the open circuit potentials and 0.6 V vs. SCE, where the interfacial interactions were
governed by adsorption, and diffusion-limited processes, respectively.
Crown Copyright Ó 2013 Published by Elsevier B.V. All rights reserved.

1. Introduction contributes to the reliable design of the pipelines to transport oil

Corrosion in oil and gas pipelines is one of the most challenging
operation problems to predict and control. Its dependence on the
environmental factors and flow rates, which are numerous and
intertwined for pipeline steel, and its nature as sustained chains of
multiple reactions, in a flow condition on the long run, are the
broad topics that still spur the ongoing research interests [1e4].
They have become over the years more interdisciplinary to achieve
for better understanding and reliable prediction of the corrosion
behavior, susceptibility and rates [5]. And albeit of the complexities
of the problem, it can be tackled from certain aspects in association
to specificly simulated laboratory conditions, and appropriately
selected and implemented experimental methods. Ultimately, that
* Corresponding author. Tel.: þ1 778 997 4878.
E-mail addresses: faysal09@interchange.ubc.ca, faysalfayez@yahoo.ie (F.F. Eliyan).
and gas at variable demands and to be operated more efficiently
and safely [6].
In this research, the influence of temperature on the corrosion
behavior of API-X100 pipeline steel is evaluated in CO2-saturated
bicarbonate solutions. In many previous studies, it was not mostly
addressed by more than one method, especially with the passiv-
ation growth and the consequent interference with the interfacial
interactions. In addition, the investigations were carried out in
aerated or deoxygenated bicarbonate, and CO2-saturated solutions,
with no consideration for a possible synergism imposed by bicar-
bonate and the dissolved CO2 e a situation that can frequently be
encountered during internal pipeline corrosion. API-X100, a new-
generation pipeline steel, received our interest in a number of
previous studies. In saline CO2-saturated solutions, the corrosion
rates, and apparently the cathodic current densities, increased with
temperature [7,8]. The passive currents and transpassivation, in

0254-0584/$ e see front matter Crown Copyright Ó 2013 Published by Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.matchemphys.2013.03.061
 F.F. Eliyan, A. Alfantazi / Materials Chemistry and Physics 140 (2013) 508e515 509

correlation to bicarbonate concentration and temperature in

aerated and deoxygenated solutions, showed discrepancy and the
nature of the interfacial interactions showed dependence on tem-
perature [9,10]. Jelinek et al. reported a decrease in the pitting
potentials with temperature for a mild steel, measured by
30 mV min
1 potentiodynamic polarization sweeps, in deoxygen-
ated 0.1 M bicarbonate solutions of few chloride traces [11]. In
0.5 g L
1 NaHCO3, CO2-saturated solutions, Louafi et al. reported an
increase of the corrosion rates of N80 steel from about 100 to
270 mA cm
2, at 20 and 50  C, respectively [12]. Parkins et al.
correlated a number of parameters of kinetics and passivation of a
mild steel to bicarbonate concentration at 23  C in CO2-saturated,
but carbonate-containing solutions [13].
In this study, the influence of temperature, with a range of bi-
carbonate concentrations, is evaluated by a number of electro-
chemical methods and immersion. More comprehensively,
therefore, the corrosion rates, and the properties of the passive
films evaluated can serve for better predicting the corrosion
Fig. 1. Microstructure of as-received API-X100.
behavior of the new High Strength Low Alloy (HSLA) steels, and for
effective control of the corrosive pipeline flows of different
types [14]. 2.3. Test solutions

2. Experimental details
2.1. Test setup
The electrochemical tests were carried out in a 1-L, three-
electrode, multi-port jacketed cell. The working electrode was the
test material API-X100 machined into flat, thin, rectangular speci-
mens which were sealed and immersed by a special holder. The
potentials were measured against the saturated calomel electrode
(SCE) of þ0.241 V vs. SHE, which was kept isolated at room tem-
perature, and the counter electrode was made of graphite. To heat
the solutions to 50 and 90  C, the jacketed chamber of the cell was
part of a hydraulic loop in which a constant-velocity water flow was
maintained circulated by a Cole-Parmer heater. A regulated flow of
high-purity carbon dioxide was purged into the solutions
throughout a time period of an electrochemical test. A computer-
synchronized Versastat 4 potentiostat was used to perform and
control the experiments and analyze the results.
2.2. Test material
The specimens were sequentially wet-ground by silicon carbide
papers of 120, 320, and 600 grit, and then degreased ultrasonically
with ethyl alcohol for 10 min, rinsed with distilled water, and dried
with hot air. The chemical composition, shown in Table 1 on wt%
basis, was made by inductive coupled plasma (ICP) and LECO car-
bon analysis. A Nikon EPIPHOT 300 optical microscope was used to
reveal the microstructure of as-received sample. It was wet-ground
with silicon carbide papers of up to 1200 grit, polished with 6 and
1 mm diamond suspensions, then immersed in 2% nital (2 ml
acid þ 98 ml ethyl alcohol) etchant, swapped with alcohol, and
dried in a hot air stream. The microstructure is shown in Fig. 1. It
mainly consists of a mixture of small amounts of ferrite and
dispersed pearlite and bainite. There are slight microvariations in
colour with the microstructure attributed possibly to some micro-
heterogeneity in the alloying composition.
Table 1
Chemical composition of the test material.
Composition (wt. %)
The solutions were synthesized to simulate one of the most
typical types of water cuts that are saturated with CO2 which dis-
solves to contribute, in mildly alkaline conditions, to increased
concentrations of the coexisting bicarbonate and H2CO3 [1]. In our
study, the solutions were first purged for 60 min with CO2, for
deoxygenation, and the purging was maintained continuous during
the tests. To evaluate certain extents of aggressiveness of bicar-
bonate in 1 bar CO2-saturated solutions, three concentrations of
NaHCO3, which is of analytical grade Fisher procured type, of 10, 30
and 50 g L
1 were introduced to the solutions. The effect of
100 ppm chloride was also studied in solutions of the same bicar-
bonate concentrations. The pH, which was unbuffered, was be-
tween 7.8 and 8.8. The tests were carried out at 20, 50 and 90  C,
maintained within 1  C.
2.4. Tests
After immersing the specimens, a potentiostatic
2 V vs. SCE
cathodic conditioning for 800 s was applied to dissolve any air-
formed oxides before running the experiments, which were
repeated at least for three times to ensure the reproducibility of the
results. The cyclic potentiodynamic experiments were performed
with a scan rate of 0.5 mV s
1 from
1 to a vertex 1.2 V vs. SCE and
then reversed to potentials below 1 V vs. SCE. The vertex 1.2 V vs.
SCE potential was selected as a criterion of which the phase of
passive film formation was assumed complete when the passive
currents show an abrupt increase at transpassivation. The poten-
tiostatic polarization tests were performed at
0.6, 0, 0.6 and 1.2 V
vs. SCE for 2000 s. The EIS tests were carried out at the open circuit
potentials and 0.6 V vs. SCE with a range of frequency of 0.01e
10,000 Hz with a sampling rate of 10 points per decade.
The immersion tests were carried out for 6-day periods. The
weight loss was measured across after 2-day intervals. The bicar-
bonate concentrations were 10 and 50 g L
1 at 20 and 50  C.
3. Results and discussion
3.1. Cyclic potentiodynamic polarization and immersion
C.E.

C Mn Mo Ni Al Cu Ti Nb Cr V The potetiodynamic polarization experiments were carried out

0.1 1.67 0.21 0.13 0.02 0.25 0.01 0.043 0.016 0.003 0.47
to measure the corrosion rates, and investigate the influence of the
environmental factors on the anodic and cathodic reactions in the
510 F.F. Eliyan, A. Alfantazi / Materials Chemistry and Physics 140 (2013) 508e515

a b

c d

e f

Fig. 2. Cyclic potentiodynamic polarization in: a) 20  C, chloride-free, b) 20  C, chloride-containing, c) 50  C, chloride-free, d) 50  C, chloride-containing, e) 90  C, chloride-free, f)
90  C, chloride-containing solutions.
 F.F. Eliyan, A. Alfantazi / Materials Chemistry and Physics 140 (2013) 508e515 511

Fig. 3. Corrosion current densities, corrosion potentials, passivation potentials, and transpassivation potentials as parameters depending on bicarbonate, temperature, and chloride.

kinetic region, and on the passivation. As shown in Fig. 2, temper-
ature appeared to be the controlling factor, and where the behavior,
relatively regardless of bicarbonate concentration and/or chloride
at a given temperature, was similar. The behavior at 20  C, both in
chloride-free and chloride-containing solutions, was unique from
50 and 90  C solutions’ during passivation. After the active disso-
lution of high current densities, broad anodic peaks appeared
which were the largest in 10 g L
1 solutions. The smaller size in
more concentrated solutions suggests an earlier passivation in
situations where the pH was higher [15]. The potentials of these
peaks were lower. The shape of the peaks was different from those
of the aerated and N2-saturated bicarbonate solutions [10,16],
which at the passivation onset, the currents decelerated abruptly to
almost two orders of magnitude. For about 350 mV above the

Fig. 4. The potentiodynamic profiles at 20, 50, and 90  C in chloride-free, 30 g L
1 Fig. 5. The peak potentials and the equilibrium potentials of some possible passivation
solutions. reactions at 90  C.
512 F.F. Eliyan, A. Alfantazi / Materials Chemistry and Physics 140 (2013) 508e515

anodic peaks at 20  C, the passivation currents showed a gradual

decrease, until about 0.5 V vs. SCE the currents up to trans-
passivation were relatively stable. Independent from the bicar-
bonate concentration, transpassivation occurred at around 1 V vs.
SCE and negative hysteresis loops resulted upon scan reversal.
Chloride seemed to cause destabilization onto passivation and
initiated many repassivated pits, as evident from the positive hys-
teresis loops. Nevertheless, although it is difficult to articulate on
how thicker a passive film would be with higher bicarbonate con-
tent e so that it would be more immune to deterioration e bicar-
bonate, which is also an active anion, seemed to reduce the critical
concentration of chloride ions adsorbed onto a passive film to
deteriorate. Small positive loops appeared, but the passivation
range was notably broad in 50 g L
1 solutions, suggesting that the
bicarbonate contributed to thicken the passivation or it adsorbed
on the majority of the surface likely sustaining for further oxidation
reactions. The cathodic branch at low temperature showed small
inner cathodic peaks, which were more apparent in chloride-
containing solutions, possibly associated to bicarbonate reduction,
obliterating that of charge transfer limited reduction of water
at
0.9 V vs. SCE.
At 50 and 90  C, the current densities were higher, the anodic
peaks were smaller and blunt, and the passivation commenced at
lower potentials. The physical effect of temperature on the
passivation structure was not to be resolved in this study, but
although of the given controversy in many previous studies [17e
20], the higher temperature generally hinders the chloride ions
from deteriorating the passive films, with no clear mechanism to be
suggested. The small second and third anodic peaks, which
appeared at 50  C, were notably larger at 90  C. Some parameters,
shown in Fig. 3, were extracted from the polarization profiles to
Fig. 6. The morphologies of the corrosion products formed during the potentiody-
better correlate the environmental factors of bicarbonate, temper-
namic polarization to 0.6 V vs. SCE in 30 g L
1 solutions, at a) 50, and b) 90  C.
ature and chloride with the corrosion behavior. At 20  C, the
corrosion rates increased with bicarbonate concentration from
about 400 to 600 mA cm
2, which were significantly higher than the

Fig. 7. Elemental EDS mapping for the corrosion surface in a 30 g L
1 solution at 50  C.
 F.F. Eliyan, A. Alfantazi / Materials Chemistry and Physics 140 (2013) 508e515 513

aerated or N2-saturated bicarbonate systems’ [21,22], suggesting anodic peaks were a result of transformation from Fe3O4 and/or
that H2CO3 might have a strong effect in accelerating the reactions FeCO3 to g-Fe2O3. Fig. 6 shows the morphologies of the corrosion
in CO2-saturated bicarbonate solutions, relatively regardless of the products formed during the potentiodynamic polarization up to
pH. This is well backed by a model published by Han et al. to predict 0.6 V vs. SCE at 50 and 90  C in 30 g L
1 solutions. Regardless of
the corrosion rates in similar solutions reporting that H2CO3 exists the presence or absence of chloride, the corrosion products at
with comparable concentrations of about 1.8 x 10
5 mol kg
1 in 50  C seemed more compact and of larger grains, while those of
solutions containing 4.9 x 10
6 to 0.95 mol kg
1 bicarbonate [23]. 90  C appeared dispersed. This could be well relevant to the high
The corrosion potentials decreased from about
730 to
760 mV passive current densities and the low transpassivation potentials
vs. SCE indicating the anodic sensitivity towards the increased bi- at 90  C. An elemental EDS mapping for iron, oxygen, carbon,
carbonate concentration. The corrosion rates increased by as much and manganese of the corrosion surface formed at 50  C is
as two to three times at 50 and 90  C, with which the corrosion shown in Fig. 7. Fe was semi-qualitatively analyzed to constitute
potentials respectively decreased, indicating the acceleration, pre- almost 50 wt% of the surface rich with O and C of about 40 and
dominantly, of the anodic reactions. The effect of chloride was more 10 wt%, respectively. Some other elements like manganese and
apparent in accelerating the corrosion rates at higher temperatures silicon were found to exist with about 0.81 and 0.6 wt%,
than 20  C, while the corrosion potentials in both cases were mostly respectively.
less than the chloride-free cases. Passivation onset potentials (Epass) The corrosion rates from the immersion tests are shown in Fig. 8.
were the highest in 10 g L
1 solutions but their dependence on In 10 g L
1 solutions, as shown in Fig. 8a, the corrosion rates were
higher bicarbonate concentrations was not clear, similar to the notably higher than that of the 50 g L
1 solutions’. They decreased
discrepancy of the locations and shapes of the anodic peaks re- over time from about 12 g m
2 day
1 to 5 g m
2 day
1 and
ported by Gonzalez-Rodrigues et al. [24]. The higher temperature, 0.5 g m
2 day
1 at 20 and 50  C, respectively. The sample surfaces
however, made the passivation to onset at lower potentials, were shiny clean in 50 g L
1 solutions and were, however,
regardless of the bicarbonate concentrations and chloride, completely covered with corrosion scales in 10 g L
1 solutions
decreasing from about
300 mV to
600 mV vs. SCE. The chloride growing to decelerate the corrosion rates. It seems that the bicar-
effect was not as clear but it seemed to make the anodic peaks bonate can act as an effective inhibitor to protect the pipeline
bigger, or to appear overlapped of multiple peaks. The currents in surfaces if it exists with sufficiently high concentrations.
the passivation regimes at 50 and 90  C were almost one order of
magnitude higher than the 20  C cases’, being almost within 110e
280 mA cm
2. The critical current densities of the first anodic peaks
a
were almost independent from the environmental factors, and they
were between 4.5 and 7 mA cm
2. The transpassivation potentials
(Etranspass), which reflect on the quality of the passive films, were
the highest at 20  C of about 1000, decreasing to 900 and 700 mV
vs. SCE, at 50 and 90  C, respectively. The reasons behind that highly
reproducible trend encourage special physico-electrochemical in-
vestigations to be carried out in the future.
The peaks which appeared above the first anodic peaks at
around
0.2, and more notably at 0.5 V vs. SCE at 90  C drew our
attention. Although we cannot articulate on the quality of the
passive films at that high temperature, these peaks could less
represent repassivated ruptures [11] than the formation of other
oxides having greater tendency at high temperatures to constitute
multi-layered passivation. As shown in Fig. 4, the three peaks were
annotated EP1, EP2, and EP3 indicating them with comparisons to 50
and 20  C cases in 30 g L
1 solutions. From the passivation reactions
utilized to analyze the polarization behavior and the chemistry of
the corrosion products in CO2-saturated bicarbonate solutions, by b
Parkins et al., Castro et al., and Lu et al. [13,25e27], we calculated
the equilibrium potentials of the reactions (1) to (5), plotted along
with the peak potentials in Fig. 5.

Fe þ HCO
þ
3 /FeCO3 þ H þ 2e


(1)

3FeCO3 þ 4H2 O/Fe3 O4 þ 3HCO
þ

3 þ 5H þ 2e


(2)

2Fe3 O4 þ H2 O/3Fe2 O3 þ 2Hþ þ 2e
(3)

2FeCO3 þ 3H2 O/g
Fe2 O3 þ 2HCO
þ

3 þ 4H þ 2e


(4)

2Fe3 O4 þ H2 O/3g
Fe2 O3 þ 2Hþ þ 2e
(5)

The figure implies that the first anodic peaks are likely Fig. 8. Corrosion rates calculated from immersion tests in a) 10 and b) 50 g L
1
associated with FeCO3 oxidation, while the second and third solutions.
514 F.F. Eliyan, A. Alfantazi / Materials Chemistry and Physics 140 (2013) 508e515
Fig. 9. Potentiostatic polarization in chloride-free, 10 g L
1 solutions at 20  C.
3.2. Potentiostatic polarization
The potentiostatic experiments were performed at four poten-
tials of
0.6, 0, 0.6, and 1.2 V vs. SCE to observe for the variations of
the current densities in relation to the dissolution and passivation
across almost 2000 s. The potentiostatic profiles of 10 g L
1 solu-
tions at 20  C are shown in Fig. 9. In
0.6 V vs. SCE, the currents
increased quickly in the first 120 s to reach 2.45 mA cm
2 (it was
almost 1.2 mA cm
2 during the potentiodynamic polarization) and
the substrate underwent extensive dissolution. During 0 V vs. SCE,
the currents were less by almost three orders of magnitude, of
about 1.5 mA cm
2, corresponding to a passive state across which
the potentiodynamic currents were gradually decreasing. The
profile showed extensive current fluctuations (or spikes) repre-
senting, as reported by Tang et al. [28], ruptures and consequent
repairs of metastable passive films. The spikes dampened with time
until the currents became stable in the last 400 s. Interestingly, the
currents at 0.6 V vs. SCE were significantly more stable and less
than that of the 0 V vs. SCE case, indicating a better passivation. The
currents at 1.2 V vs. SCE increased steadily with time, but remained
less than 300 mA cm
2, corresponding possibly to parallel processes
of transpassivation and O2 evolution. The currents in other bicar-
bonate solutions were generally within comparable ranges, but in
the presence of chloride, the currents showed discrepancy, espe-
cially at the high potentials. At 90  C, whose profiles are shown in
Fig. 10 representing for 10 g L
1 solutions, the currents were higher
Fig. 10. Potentiostatic polarization in chloride-free, 10 g L
1 solutions at 90  C.
but the profile of
0.6 V vs. SCE, although of the highly intense
fluctuations within the other potentials in the passivation range,
was different notably from that of the 20  C case.
3.3. Electrochemical impedance spectroscopy
The electrochemical and other diffusion-limited interactions
[29] during the open circuit potentials and 0.6 V vs. SCE were
investigated by EIS. As shown in Fig. 11, it was evident that the
interfacial reactions were mainly governed by adsorption during
the OCP conditions. Raising the temperature to 90  C did not
change the nature of the interactions but the overlapped,
depressed, capacitive arcs were smaller, reflecting less charge
transfer resistance and confirming with the polarization results.
Zhang et al. and Farelas et al. discussed the role(s) of certain in-
termediate species in similar corrosion environments [30,31].
Complex species such as FeOHþ get adsorbed to drive the disso-
lution with rates changing over time, and as the reductions of
H2CO3, HCO
þ
3 and H simultaneously take place with slower rates.
The impedance modules were noticeably less at higher tempera-
tures across the full frequency range, and the sole phase peaks
appeared to shift to higher frequencies at higher temperature. The
EIS response in the other solutions, regardless of the bicarbonate
concentration, and to a high extent of the chloride, was not quite
different. The experimental data were simulated with the equiva-
lent circuit {R(Q(R(QR)))} which accounts for charge transfer at the
 F.F. Eliyan, A. Alfantazi / Materials Chemistry and Physics 140 (2013) 508e515 515

typical pipeline flow. The influence of temperature on the

a
corrosion rates and passivation was investigated by electro-
chemical methods and immersion in CO2-saturated bicarbonate
solutions. The corrosion rates showed sensible dependence on bi-
carbonate concentration, but they increased from about 500 to
1500 and 1800 mA cm
2 at 20, 50 and 90  C, respectively. At 20  C,
the passivation onset was at high potentials, showed evidence of
gradual formation and deteriorated by 100 ppm chloride ions in
dilute bicarbonate solutions. At 50 and 90  C, the passivation was
resistant against the chloride pitting, and the transpassivation
occurred at lower potentials of 0.9 and 0.7 V vs. SCE, respectively.
The potentiostatic currents, although of being higher with tem-
perature at different potentials, suggested effective passivation
accordingly. The charge transfer resistance decreased with the
higher temperature, as revealed by the EIS measurements, and the
interactions were governed by adsorption and diffusion-limited
processes at the OCPs and 0.6 V vs. SCE, respectively.

Acknowledgment

This publication was made possible by NPRP grant # 09-211-2-

b
089 from the Qatar National Research Fund (a member of Qatar
Foundation). The statements made herein are solely the re-
sponsibility of the authors.

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