Research Article

Received: 17 December 2008 Revised: 14 February 2009 Accepted: 16 February 2009 Published online in Wiley Interscience: 18 March 2009

(www.interscience.wiley.com) DOI 10.1002/sia.3057

Effect of temperature on CO2 corrosion of

carbon steel
Z. F. Yin,a,b∗ Y. R. Feng,b W. Z. Zhao,a Z. Q. Baib and G. F. Linb
This work investigates the effect of temperature on the corrosion product layer of carbon steel exposed to a CO2 -containing
solution. The measurement techniques, such as scanning electron microscopy with energy dispersive spectrometry, X-ray
diffraction, and X-ray photoelectron spectroscopy, were used to systematically characterize the morphology and composition
of the corrosion product layer. The corrosion rates were calculated by weight loss method. The corrosion mechanisms as a
function of temperature are studied and discussed. The results showed that temperature is an important factor in the corrosion
rate of carbon steel. Copyright

c 2009 John Wiley & Sons, Ltd.

Keywords: CO2 corrosion; carbon steel; corrosion product layer; XPS; solution chemistry

Introduction product layers can offer some protection against corrosion by

Dissolved CO2 in aqueous solutions can lead to serious corrosion on
the steel pipelines or equipments used in the oil/gas production or
transport, which can even result in major safety accident.[1,2] The
understanding of CO2 corrosion mechanisms under the effects
of many mechanical and environmental factors, such as flow,
temperature, pressure, oil–water ratio, pH, solution chemistry,
and corrosion product layer, has been of great concern in
corrosion field.[1,3 – 6] Carbon steels are often used as materials
in oil-producing and -gathering facilities; however, they are very
susceptible to corrosion in CO2 environments, leading to severe
damage.
It is known that CO2 hydration is a slow chemical reaction and
can be the rate-determining step for the overall corrosion rate.
Only a small fraction of carbonic acid is dissociated in two steps
to form hydrogen, bicarbonate, and carbonate ions. The anodic
reaction is iron dissolution and the cathodic reactions include
one or more of the following: hydrogen ion reduction, carbonate
acid reduction (perhaps bicarbonate ion reduction), and water
reduction (generally occurring at a pH value above 6).[3,7]
Temperature is one of the most important influencing factors
in CO2 corrosion environments. In general, temperature plays an
important effect on the formation rate of corrosion product layer.
At low temperatures (below 60 ◦ C), no protective layer is formed
on the steel surface because of the high solubility of the iron
carbonate layer. The corrosion product layers are generally porous
and loose, leading to increased corrosion rates. As temperature
increases, the corrosion product layers become more compact,
dense, and adherent to the steel surface, resulting in the formation
of more protective precipitates on the steel surface. Therefore, the
corrosion rate generally decreases when the temperature is around
or above 80 ◦ C.[8 – 12]
The effect of protective corrosion layers related with different
kinds of variables in CO2 environments has been discussed. The
main corrosion product of carbon steel is iron carbonate (FeCO3 ),
which precipitates on the steel surface when the FeCO3 level is
high enough close to the steel surfaces.[8,13] Depending on the
type of the corrosion product layers present and the experimental
reducing mass transfer of the reactants and products between
bulk solution and steel surface.[14] If the products are adherent
and dense, they can cover the steel surfaces, leading to a good
protection. However, localized corrosion can also occur when the
product layers break down locally and cannot be repaired by
nucleation and growth. The kinetics of FeCO3 precipitation seems
to be a controlling factor for the protection of corrosion product
layers. At higher temperatures, the FeCO3 solubility is decreased
and the precipitation is much faster.[12,15] In addition, protective
product layers can be formed more easily and fast at higher pH
values in CO2 environments.[11,15,16] Many protective mechanisms
of corrosion product layers are published in the past decades; for
instance, Nesic et al.[11] thought that the product layers act as a
physical barrier that can restrict the diffusion transfer of aggressive
species and prevent further steel dissolution.
The difficulty in defining and describing corrosion mechanisms
involving many variables in CO2 environments leads to complexity
in understanding the morphologies of corrosion product layers,
solution chemistry, and corrosion prediction models. The purpose
of the present work is to investigate the effect of temperature
on corrosion product layers of carbon steel exposed to CO2 -
containing solution by using SEM, energy dispersive spectrometry
(EDS), X-ray diffraction (XRD), and XPS measurement techniques.
The corrosion mechanisms are also studied as a function of
temperature and discussed.
∗ Correspondence to: Z. F. Yin, School of Materials Science and Engineering, Xi’an
Jiaotong University, Xi’an 710049, People’s Republic of China.
E-mail: yinzhifu919@sohu.com
a School of Materials Science and Engineering, Xi’an Jiaotong University, Xi’an
710049, People’s Republic of China
b The Key Laboratory for Mechanical and Environmental Behavior of Tubular
Goods, Tubular Goods Research Center, CNPC, Xi’an 710065, People’s Republic
517

conditions under which these layers can be formed, the corrosion of China

Surf. Interface Anal. 2009, 41, 517–523 Copyright

c 2009 John Wiley & Sons, Ltd.

(a)
(c)
(e)
Figure 1. Morphologies of corrosion product layers formed at various temperatures: (a) 50 ◦ C, (b) 70 ◦ C, (c) 100 ◦ C, (d) 130 ◦ C, (e) 150 ◦ C, and (f) 180 ◦ C.
Magnification 1000×.
Experimental
Materials and weight loss measurements
The test material was P110 carbon steel slice with a size of
35 × 25 × 3 mm, whose chemical composition was 0.31 wt.% C,
0.22 wt.% Si, 1.40 wt.% Mn, 0.011 wt.% P, 0.0037 wt.% S, 0.044 wt.%
Cr, 0.032 wt.% Mo, 0.019 wt.% Ni, 0.08 wt.% Cu, 0.0061 wt.% Ti, and
0.052 wt.% V, the remaining being Fe. The samples were initially
polished by emery sandpaper progressively up to 800 grit, then
degreased with acetone, rinsed with absolute alcohol, weighted
using an electronic balance with a precision of 0.1 mg, and finally
placed in the high-temperature and high-pressure autoclave made
in China. Before the tests, the solution was deoxygenated by
bubbling pure N2 for 12 h before the introduction of CO2 gas,
and then the solution in the autoclave was pressured with CO2
gas to the invariable value of 4 MPa. Experiments were performed
518
at the temperature range of 50–180 ◦ C. Corrosion tests were
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c 2009 John Wiley & Sons, Ltd.
Z. F. Yin et al.
(b)
(d)
(f)
carried out for 120 h under static condition. The test solution
was composed of deionized water and pure chemical agents
with a concentration of NaCl 164.8 g L−1 , CaCl2 1.3 g L−1 , and
MgCl2 · 6H2 O 12.6 g L−1 . At least three samples were tested for
each experimental condition. After each test, the samples were
rinsed with distilled water and ethanol, and then divided into
two groups. The samples in group one were descaled with Clark
solution (20 g Sb2 O3 +50 g SnCl2 +1 L HCl); then visual observation
was done and weight loss was measured. The samples in group
two were not descaled and were dried and stored in desiccator
until analysis using SEM, EDS, XRD, and XPS.
SEM, EDS, XRD, and XPS analyses
Corrosion product layer on the corroded sample was analyzed
using Model PHI-5400 XPS system made by Perkin ELMer Corpo-
ration (USA) with the following set of experimental parameters: a
Surf. Interface Anal. 2009, 41, 517–523
Effect of temperature on CO2 corrosion
(a)
(c)
(e)
Figure 2. Cross-section images of corrosion product layers formed at various temperatures: (a) 50 ◦ C, (b) 70 ◦ C, (c) 100 ◦ C, (d) 130 ◦ C, (e) 150 ◦ C, and
(f) 180 ◦ C. Magnification 500×. This figure is available in colour online at www.interscience.wiley.com/journal/sia.
magnesium Ka X-ray source with a power of 400 W, a pass energy
of 89.450 eV for narrow scan, an analysis area approximately
1.0 mm2 , and a vacuum of 2 × 10−8 Pa in the test chamber.
The binding energies (BEs) were calibrated by taking C 1s peak,
284.6 eV, as the standard. The XRD experiment was performed
using Japanese D/Max-2400 automatic XRD apparatus with Cu
Ka X-ray source, an accelerating voltage of 40 kV, and a current
density of 40 mA cm−2 . SEM and EDS were utilized to investigate
surface morphologies and element contents of the corrosion
product layer. Before SEM, EDS, XRD, and XPS analyses, the samples
were cleaned in acetone to remove surface contamination.
Results and Discussion
Morphologies observation
The samples retrieved from each test were examined by SEM
to investigate the morphologies of corrosion product layers
Surf. Interface Anal. 2009, 41, 517–523
(b)
(d)
(f)
developed in autoclave. Figure 1 shows the surface morphologies
of corrosion product layers at various temperatures. The crystalline
particles are uniformly distributed on the sample surfaces, which
can offer some protection to metal surfaces. From the surface
morphologies in Fig. 1, we cannot judge whether these product
layers formed at various temperatures have good protection.
However, there is an obvious difference between the product
layers formed at 180 ◦ C and those formed at other temperatures,
i.e. the corrosion products appear adherent to each other without
any gap. In addition, the crystalline sizes corresponding to the
temperature of 100 ◦ C are small in comparison with those under
other temperatures conditions. Figure 2 shows the cross-section
morphologies of corrosion product layers, which clearly represent
the surface microstructures’ characterization. The thicknesses of
corrosion product layers are approximately 69.49, 48.71, 46.21,
34.03, 12.89, and 9.67 µm corresponding to 50, 70, 100, 130,
150, and 180 ◦ C, respectively. The present work indicates that the
519
thickness of corrosion product layer decreases with increasing
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10
8
Corrosion rate (mm a-1)
6 can accelerate the precipitation of product layers and can result in
4
2 follows[9,20,21] :
0 PRFeCO3 =
40 60 80 100 120 140 160
Temperature (°C)
Figure 3. Corrosion rates by weight loss method at various temperatures.
temperature. This conclusion confirms the common overview that
the corrosion product layers have more effective protection to steel
surfaces by restricting the transfer rate of reactants and products to
and from the steel surfaces.[11,12] Examination of the samples under
SEM shows two main types of development of corrosion product
layer. The first product type is a thick, porous, and loose layer that
can give partial protection to the steel beneath it. Another type
is a thin, dense, and adherent layer formed on the steel surface,
which is usually associated with a lower corrosion rate. The layer
thicknesses formed at 150 and 180 ◦ C are obviously different from
those at temperatures at and below 130 ◦ C. Of course, the thickness
of product layer is not completely proportional to the corrosion
rate, which will be proved by the relation between corrosion rate
and temperature subsequently.
It is clear that the thick and porous corrosion product layers in
Fig. 2(a)–(d) belong to the first product layer type. The micropits
offer ‘transfer tunnel’ for aggressive species in bulk solution,
and thus the solution species can readily penetrate the product
layers to corrode the metal below them continuously, leading to
increased corrosion rate. It is worth mentioning that an important
characterization of this type is a small gap between the metal
surface and corrosion product layer, where the corrosion product
layer cannot effectively prevent corrosion chemical reactions from
taking place beneath the scale layer. Compared with this type,
the thin and compact product layers are well bonded to the
metal as shown in Fig. 2(e) and (f). However, the corrosion rates
calculated by weight loss methods are not in accordance with the
results under the morphology observation. The average corrosion
rate at 50 ◦ C is much higher than those at higher temperatures,
as shown in Fig. 3. In the current tests, the average corrosion
rate is the lowest at 100 ◦ C, which then increases slightly with
increasing temperature. However, there is no literature related
to the high temperatures above 150 ◦ C for carbon steels used
in the present work. In addition, when compared with the
calculation results using the well-known de Waard–Milliams
model[17] , we can find that the calculated corrosion rates are
much higher than the actual corrosion rate, which is because this
model omits many other factors such as pH value, temperature
range, and the most significant factor – product layer protective
factor.
The formation of corrosion product layer is a very complicated
520
process that depends on many influencing factors. In principle,
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Z. F. Yin et al.
it has two precipitation processes, initiation and growth. The
initiation rate is reported to increase exponentially with relative
supersaturation, whereas the growth rate has an approximately
linear relationship with this parameter. Growth should therefore
predominate at low relative supersaturation. A high initiation rate
the more protective corrosion product layers.[18,19] The definition
of precipitation rate of the iron carbonate layers (PRFeCO3 ) can
be described using supersaturation index (SS), solubility product
(Ksp ), temperature (T), and surface area-to-volume ratio (A/V) as
A
× f(T) × Ksp × f(SS) (1)
V
180 200 CFe2+ CCO2−
SS = 3
(2)
Ksp
Despite the corrosion product layer growth being significantly
dependent on the precipitation rate of FeCO3 , the steel surface
beneath the product layer probably creates some micropits or gaps
between the product layers and the steel surfaces, which is the so-
called scale undermining. If the precipitation rate equals or exceeds
the undermining rate, the compact, adherent, and protective
product layers are formed on the steel surfaces. Conversely, the first
product layer type (porous and unprotective product layer) sticks
on the steel surface.[11,21] Nesic et al.[11] proposed an equation
describing the product layer growth kinetics of mass conservation
for FeCO3 , which can be written as
∂CFeCO3
= PRFeCO − CR
∂CFeCO3
(3)
∂t 


 3
∂x 
local precipitation undermining
change rate rate
EDS, XRD, and XPS analyses
Energy dispersive spectrometry was utilized to detect the element
contents (at.%) in the corrosion product layers on the samples
obtained at the temperatures of 70, 100, 130 and 150 ◦ C. Some
differences exist in the element contents, as shown in Fig. 4. On
the basis of the experimental data of EDS, the Fe/O ratios (at.%)
are 29.64/45.51, 30.15/46.78, 27.15/45.77, and 27.10/46.25 (i.e.,
0.652, 0.645, 0.593, and 0.586) respectively, with respect to the
temperatures 70, 100, 130, and 150 ◦ C. It is clear that Fe/O ratio
slightly decreases with increasing temperature, indicating that the
compositions possibly change. In addition, it is worth mentioning
that the Mg at.% (i.e., 0.92, 1.91, 4.76, and 5.71) increases with
the increase in temperature, while the Ca at.% (i.e., 3.29, 3.87,
3.52, and 3.07) remains the same. The analyses also indicates
that (Mg,Fe)CO3 is possibly a corrosion product with increasing
temperatures.
The constituents of the product layers developed in CO2
environment are identified by XRD. Figure 5 shows the XRD
spectrum detected from corrosion product layers on steel
surface at 70 ◦ C. The result indicates that the constituent of
the product layers is composed of iron carbonate under this
condition. Although no other product constituent is detected at
this temperature, many other corrosion products are generated
under different conditions. For instance, at higher temperature,
magnetite (Fe3 O4 ) may occur on the steel surfaces, while at
lower temperature iron carbide (Fe3 C) is one of the significant
c 2009 John Wiley & Sons, Ltd. Surf. Interface Anal. 2009, 41, 517–523
Effect of temperature on CO2 corrosion

(a) (b)

(c) (d)

Figure 4. The EDS diagrams obtained on samples at various temperatures: (a) 70 ◦ C, (b) 100 ◦ C, (c) 130 ◦ C, and (d) 150 ◦ C. This figure is available in colour
online at www.interscience.wiley.com/journal/sia.

spectra of the corrosion product layer, in which the peaks at BEs

1200 1 1 --- FeCO3 529.75 and 531.45 eV, respectively, correspond to Fe(HCO3 )2 and
FeCO3 . An examination of Fe 2p spectra in Fig. 6(d) reveals a peak
1000
at 709.82 eV, which demonstrates the presence of FeCO3 deposit.
In addition, the peak around 713.53 eV may be characteristic of the
Intensity (cps)

800
Fe3+ compound, which may be attributed to the decomposition
of FeCO3 , despite the formation of corrosion product layer under
600
deoxidized solution. On the other hand, it can be explained that
1 the Fe3+ compound forms during the exposure of the corroded
400
1 sample to dried atmosphere before the XPS analysis.
1 1 1
200 1 1
1 1 1 1 Solution chemistry and electrochemistry
0
The chemical and electrochemical reactions in CO2 corrosion
20 40 60 80 system can have a significant impact on the corrosion rate and
2θ (degree) surface morphologies by changing the local concentrations of
reactants and products, resulting in a concentration gradient
Figure 5. XRD spectrum obtained from corrosion product layer at 70 ◦ C. from bulk solution to the sites close to the metal surface. As
is well known, dry carbon dioxide gas has no corrosivity unless
constituents, which is a former part of the original steel in the non- it dissolves into aqueous solution, and this dissolution can be
oxidized state that accumulates on the steel surface as corrosion represented by[25]
KH
proceeds.[22,23] CO2(g) ←−→CO2(aq) (4)
Figure 6 shows the peak fitting spectra of corrosion product layer
The equilibrium constant (Henry’s law constant) for the above
formed at 70 ◦ C using XPS, in which the elements of special interest
reaction as a function of temperature was reported by Roberts
are iron, oxygen, and carbon. Figure 6(a) shows survey spectrum
et al.[25] :
of the corrosion layer on steel surface. The C 1s high-resolution
XPS scans in Fig. 6(b) reveal three peaks at the BEs 284.64, 286.90,
and 289.42 eV. The first peak at 284.64 eV close to 284.6 eV lgKH = 3482.89/T + 8.3068 ln T − 2.790
corresponds to hydrocarbonate absorbed in corrosion layer, while × 10−4 T − 60.3994 (5)
the third peak at 288.89 eV around 289.6 eV is attributed to pure
iron carbonate.[24] However, the third C 1s peak is the undefined Then, only a small fraction of the dissolved CO2 reacts with
substance, because of the presence of the complex carbides or water, forming carbonic acid, which is corrosive to carbon
521

imprecise fitting. Figure 6(c) shows the O 1s high-resolution XPS steel as expressed in Eqn (6). Palmer et al.[26] thought that the

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 Z. F. Yin et al.

(a) 10 (b) 10

- Fe 2p1
Survey spectrum C 1s peak spectra Fe(HCO3)2

- Fe 2s
(284.62eV)
8 8

Na 1s -

- O 1s
- Fe LMM
Fe2p3- O KVV -
6 6

N(E) (E)
N(E) (E)

- Fe LMM
FeCO3

- Fe LMM
(289.42 eV)

- Na KLL- C 1s
4 4

- Fe 3p
- Ca 2p
- Na KLL
- Ca2s
286.90 eV

- Fe3s
2 2

- O 2s
0 0
1000 800 600 400 200 0 290 288 286 284 282
Binding Energy (eV) Binding Energy (eV)

(c) 10 (d) 10
Fe(HCO3)2
O 1s peak spectra (529.75 eV) Fe2p3/2 peak spectra
8 8 Fe2+
(709.82 eV)

6 FeCO3 6
N(E) (E)

N(E) (E)
(531.45 eV)

4 4

2 2 Fe3+
(713.53eV)

0 0
534 533 532 531 530 529 528 716 714 712 710 708 706
Binding Energy (eV) Binding Energy (eV)

Figure 6. XPS fitting spectra obtained from corrosion product layer at 70 ◦ C: (a) survey spectrum of corrosion product layer, (b) C 1s characteristic peak,
(c) O 1s characteristic peak, and (d) Fe 2p3/2 characteristic peak.

equilibrium constant of this reaction is around 2.58 × 10−3 when A higher temperature directly causes a higher corrosion rate
the temperature is in the range of 10–150 ◦ C. In addition, it can because of the acceleration of the electrochemical and chemical
be concluded that only a small amount of the resultant of H2 CO3 reactions. However, precipitation rate also increases at a higher
form in the solution based on the equilibrium constant provided. temperature, so the protective product layers form more easily
and can lead to a reduction in the corrosion rate.[9,28]
CO2(aq) + H2 O ↔ H2 CO3 (6) In the past several years, many corrosion models involving lots
of influencing factors, such as temperature, CO2 partial pressure,
Nestic et al.[4] proposed a model for carbon dioxide corrosion, oil–water ratio, pH value and flow rate, and so on, were proposed.
based on the models of individual electrochemical reactions de Waard and Milliams revised the constants of the well-known
occurring in water–carbon dioxide systems. At the metal surface, de Waard–Milliams model[17] proposed in 1975 on the basis of
the cathodic process generally involves the following three the experiment data obtained by Dugstad et al.[29] The revised de
reactions: Waard–Milliams equation is given as

2H2 CO3 + 2e− −−−→ H2 + 2HCO− (7) 1710

3 lg(Vcorr ) = 5.8 − + 0.67lg(PCO2 ) (14)
2HCO− −
+ 2e −−−→ H2 + 2CO2− (8) 273 + t
3 3
2H + 2e− −−−→ H2
+
(9) where Vcorr is the corrosion rate in mm/yr, t is the temperature in ◦ C,
and PCO2 is the CO2 partial pressure in bar (105 Pa). In the present
The anodic reaction is given by work, based on Eqn (4), the corrosion rates are 3.206, 60.513,
16.444, 36.058, 57.149, and 105.925 mm a−1 , respectively. The
Fe −−−→ Fe2+ + 2e− (10) corrosion rate evidently increases with increasing temperature,
especially at temperatures above 100 ◦ C. This is not in accordance
Brockris et al.[27] showed that the rate-determining step de-
with the experimental results shown in Fig. 3. One important
pends upon the pH. The main corrosion product is the precipitate
reason is that the corrosion product layer is little protective at
iron carbonate (FeCO3 ), which can be formed by the following
lower temperatures; but once the temperature is high (generally
ways[24,27] :
at or above 80 ◦ C), there are some compact and dense product
layers attached to the metal surface, which restrict the transfer
Fe2+ + CO2−
3 −−−→ FeCO3 (11)
of the reactants and products. Therefore, the corrosion model
Fe2+ + 2HCO−
3 −−−→ Fe(HCO3 )2 (12) must consider whether the influence of corrosion product layers is
522

Fe(HCO3 )2 −−−→ FeCO3 + CO2 + H2 O. (13) protective or not as corrosion environments vary. Of course, every

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c 2009 John Wiley & Sons, Ltd. Surf. Interface Anal. 2009, 41, 517–523
Effect of temperature on CO2 corrosion
corrosion model is not accurate because of the varied experimental
conditions or actual industry conditions. Despite the majority of
corrosion factors being included into models such as the known
Tulsa model,[20] Ohio model,[30] , and KSC model,[5] , the prediction
of CO2 corrosion of carbon steel is still very difficult, especially at
high temperature or high pH.
Conclusions
The corrosion product layers uniformly cover the metal surfaces at
various temperatures. The crystalline sizes corresponding to the
temperature of 100 ◦ C are small in comparison with those under
other temperatures conditions. In addition, the corrosion mor-
phologies have obvious characterization at 180 ◦ C. The thickness
of corrosion product layer decreases with the increasing temper-
ature. Besides the main corrosion product being iron carbonate,
there are some limited amounts of Fe3 C or Fe3 O4 at higher or
lower temperatures. The peak fitting spectra of corrosion product
layer formed at 70 ◦ C by using XPS, in which the special interest
elements of iron, oxygen, and carbon, are detected and analyzed.
Acknowledgements
The authors want to thank the Key Laboratory Opening Fund (No.
06A40302) of Corrosion and Protection of Tabular Goods Research
Center of China National Petroleum Corporation for their support
to this work.
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