Paper No.

C2020-14413

Fe3O4, FeCO3 or FeS - Which Corrosion Product Will Prevail at High Temperature in CO2/H2S
Environments?

Shujun Gao, Bruce Brown, David Young, Srdjan Nesic, Marc Singer
Institute for Corrosion and Multiphase Technology,
Department of Chemical & Biomolecular Engineering, Ohio University
342 West State Street
Athens, OH, 45701
USA

ABSTRACT

Sweet (CO2) and sour (H2S) corrosion have continuously been a challenge in oil and gas production
and transportation. Yet, some key issues are still not well understood, especially at high temperature
production conditions. A CO2/H2S ratio of 500, which has been used (often inaccurately) to determine
which corrosion mechanism is dominant, is probably even less valid at high temperature. The nature of
the corrosion products forming at high temperature in CO2/H2S environments and their effects on the
corrosion rate are not known. Finally, the impact on pipeline integrity of environmental changes
between sweet and sour production conditions (simulating reservoir souring) has not been well
documented. CO2, H2S, and CO2/H2S corrosion experiments were conducted at 120oC to investigate
corrosion mechanisms and corrosion product layer formation at high temperature. The results show
that the corrosion products were still clearly dominated by H2S under the pCO2/pH2S ratio of 550.
Formation of Fe3O4, FeCO3, and FeS corrosion product layers had a direct impact on the measured
corrosion rates and was dependent on the gas composition and on the sequence of exposure (CO2
then H2S and vice versa). Compared with H2S corrosion alone, the presence of CO2 could retard Fe3O4
formation in CO2/H2S mixture environment. No obvious change in steady state corrosion rate was
observed when the corrosion environment was switched from CO2 to H2S and vice versa.

Key words: high temperature corrosion, CO2/H2S, iron oxide, iron carbonate, iron sulfide

INTRODUCTION

Carbon dioxide (CO2) and hydrogen sulfide (H2S) are the two acid gases that are commonly associated
with oil and gas industry. The presence of CO2, H2S, and free water can cause severe internal
corrosion problems in wells and pipelines, which poses serious challenges to process safety,
equipment integrity, eco-system and human health.1-3 Moreover, corrosion environments become ever
harsher as more and more wells are drilled to deeper depths that contain oil and gas at high
temperature and high pressure (HTHP) conditions.4-6

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1
 CO2 and H2S corrosion have been widely studied and significant progress has been made in the past
decades in determining the controlling mechanisms.7-10 However, there are still some key issues that
are poorly understood, especially when it comes to high temperature, as described in the following text.
In 1983, Dunlop et al.,11 proposed a CO2/H2S ratio of 500 to determine whether the corrosion would be
dominated by CO2 or H2S at 25oC. This ratio has been widely quoted and applied in other industry
documents.12-13 However, its validity has also been challenged if used under different conditions that
25oC.14 In addition, the terminology used to determine which gas will have a “dominant” effect on
corrosion is very confusing. Whether it is based on the argument of “corrosion rate” or “corrosion
product” is still unclear. Consequently, how this ratio can be applied in deciding which mitigation
method, steel type or corrosion prediction tool to use still remains uncertain. A simple question to
address here is whether or not the CO2/H2S ratio of 500 is valid at high temperature (research question
#1). While the answer to this question is obviously “no”, a reflection on the validity of a simple critical
CO2/H2S ratio is still useful.
Previous studies have shown that Fe3O4 can form in both CO2 and H2S environments at high
temperatures.15-18 Generally, Fe3O4 formed at high temperature can be considered as a protective
layer.19 However, in a recent experimental study performed at high temperatures using an autoclave,
the uniform steady state corrosion rate in “CO2-only” environment was around 0.1 mm/yr,15 while that in
an “H2S-only” environment was shown to be approximately 2 mm/yr16. Why was a much higher
corrosion rate observed in an “H2S-only” environment (research question #2)?
Most studies focus on CO2 or H2S corrosion alone,20-23 or mixed CO2/H2S corrosion.24,25 Little is known
when the corrosion environment switches from sour (H2S) to sweet (CO2) or from sweet to sour. For
example, CO2 gas can be injected into a sour reservoir to reduce the oil viscosity and enhance the oil
recovery.26 Similarly, if H2O is injected into a sweet well, some microorganisms such as sulfate reducing
bacteria (SRB) can be developed and produce H2S.27 What is the impact of this environmental change
on pipeline integrity? Can aged pipeline still be used or do they need to be replaced?28 Therefore, it is
necessary to investigate the corrosion behavior of mild steel with environmental change from sweet to
sour and vice versa (research question #3).
In order to address the above stated three research questions, CO2 and/or H2S corrosion experiments
were conducted at 120oC. Linear polarization resistance (LPR), X-ray diffraction (XRD), and scanning
electron microscopy with energy dispersive X-ray spectroscopy microanalysis (SEM/EDS) methods
were employed to investigate the validity of the CO2/H2S = 500 ratio, the role of the Fe3O4 layer in
corrosion, and the effect of environmental transitions.

EXPERIMENTAL PROCEDURE

High temperature experiments were carried out in a 7 L Hastelloy † autoclave, as shown inError!
Reference source not found.. Linear polarization resistance (LPR) measurements were conducted
using a conventional three-electrode configuration. The working electrode was a cylindrical API 5L X65
mild steel, whose chemical composition is shown in Table 1. Due to the lack of a reliable reference
electrode at high temperature in an H2S environment, a commercial Zr/ZrO2 high temperature, high
pressure pH probe was used as a pseudo reference electrode. It could serve as a reference electrode
as long as its potential was stable under the operating conditions, but the exact potential was still
unknown.29 The counter electrode was a Pt-coated Nb cylinder. LPR corrosion rate was measured
about every two hours at a scan rate of 0.125 mV/s between 5 mV vs. OCP. Some square X65
specimens were also hung on a stabilized shaft for additional analysis. A central impeller, with a 1000
rpm rotating speed, was used to well mix the solution during the experiment. The electrolyte was 1
wt.% NaCl aqueous solution.

†
Trade Name
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2
 Figure 1 Experimental autoclave set up.

Table 1 Chemical composition of API 5L X65 carbon steel (wt%).

Cr Mo S V Si C P Ni Mn Fe
0.14 0.16 0.009 0.047 0.26 0.13 0.009 0.36 1.16 Balance

The testing parameters and experimental design are shown in Figure 2. The experimental condition
was 120oC, 55 bar CO2 and/or 0.1 bar H2S, with an initial pH of 5.0 calculated according to an in-house
water chemistry model.30 Five separate experiments were conducted. First, experiments with 55 bar
CO2 only and 0.1 bar H2S only were carried out. Then, a CO2 and H2S gas mixture was tested for 4
days at the CO2/H2S ratio of 550. Finally, H2S was added to CO2 environment after 4 days of exposure
and tested for another 4 days, and vice versa, to investigate the environment change between sweet
and sour conditions on the corrosion behavior of mild steel.

Figure 2 Experimental design.

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3
 EXPERIMENTAL RESULTS

Corrosion rates

The LPR corrosion rates of carbon steel in 55 bar pCO2 and/or 0.1 bar pH2S environments at 120oC are
shown in Figure 3. All the initial corrosion rates were around 10 mm/yr. Then, the corrosion rates
quickly decreased down to a stable value in the first day. However, the steady-state corrosion rates
varied in different environments. The CO2-only environment has the lowest stable corrosion rate at
approximately 0.15 mm/yr, while the highest stable corrosion rates, about 2 mm/yr, appeared in the
H2S-only environment. In CO2/H2S mixture environment, the stable corrosion rate was in between,
around 0.7 mm/yr, which is closer to that observed for the CO 2-only environment. When introducing 0.1
bar pH2S into 55 bar pCO2 environment, the corrosion rate immediately increased to 0.7 mm/yr, then
also quickly decreased back to almost the same value as the one before adding H2S. Similar behavior
was observed when adding CO2 into an H2S-only environment.

Figure 3 LPR corrosion rate of carbon steel in 55 bar CO2 and/or 0.1 bar H2S environments,
120oC, initial pH 5.0, 4 (or 4+4 for H2S/CO2 transition experiments) days, B=23 mV/decade.
The averaged LPR corrosion rate was compared with WL corrosion rate, as shown in Figure 4. A good
agreement can be observed in all the environments by using a B value of 23 mV/decade.

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 Figure 4 Comparison between average LPR corrosion rate WL corrosion rate, 120oC, 55 bar CO2
and/or 0.1 bar H2S, initial pH 5.0, 4 (or 4+4 for H2S/CO2 transition experiments) days, B=23
mV/decade.

Corrosion products

The corrosion morphologies and cross-sections of steel specimens were examined by XRD and
SEM/EDS, as shown in Figure 5 to Figure 11. Pure FeCO3 formed in the CO2-only environment. Large
bulk FeCO3 crystals can be observed on the surface. The layer thickness was about 12 µm (Figure 7).
In the H2S-only environment, XRD and SEM show hexagonal pyrrhotite crystals with different sizes
covering the steel surface. The cross-section shows there was also an inner Fe3O4 layer (~ 25 µm)
formed, which was not detected by XRD due to the limited depth of X-ray penetration. The formation of
the thermodynamically less stable Fe3O4 at high temperature in H2S environment has been confirmed
in various studies.16, 30, 31

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 Figure 5 XRD patterns of corrosion products on the steel surface in different environments,
120oC, 55 bar CO2 and/or 0.1 bar H2S, initial pH 5.0, 4 (or 4+4 for H2S/CO2 transition experiments)
days.

Figure 6 SEM morphologies (a) and (b) 55 bar CO2, (c) and (d) 0.1 bar H2S, 120oC, initial pH 5.0, 4
days.

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 Figure 7 Cross-sections and EDS mapping results (a) 55 bar CO2, (b) 0.1 bar H2S, 120oC, initial
pH 5.0, 4 days.
In a CO2 and H2S mixture environment under the pCO2/pH2S ratio of 550, only iron sulfide was
observed. The major iron sulfide phase was pyrrhotite with small amount of mackinawite. The pyrrhotite
crystals were much smaller and not as dense as observed in the H2S-only environment. The layer
thickness also decreased from tens of microns to less than 5 µm. There was also a thin inner
layer (< 0.5 µm) containing oxygen. However, it is not clear if this layer next to the surface is Fe3O4 or
FeCO3. In either case, it seems that the high pressure CO2 (55 bar) could retard Fe3O4 formation
compared with the H2S-only experiment. An additional experiment at lower pCO2=10 bar was
performed to confirm this phenomenon, as shown in Figure 8 and Figure 9. Clearly, it can be seen that
a thin Fe3O4 appeared as the inner layer at a lower pCO2. The thickness was around 8 µm, which is still
below the one formed in H2S only environment (~ 25 µm). Additionally, the pyrrhotite crystal size and
total layer thickness also increased compared with that in 55 bar CO2 environment.

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 Figure 8 SEM morphologies (a) and (b) 55 bar CO2 and 0.1 bar H2S, (c) and (d) 10 bar CO2 and 0.1
bar H2S, 120oC, initial pH 5.0, 4 days.

Figure 9 Cross-sections and EDS mapping results (a) 55 bar CO2 and 0.1 bar H2S, (b) 10 bar CO2
and 0.1 bar H2S, 120oC, initial pH 5.0, 4 days.

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 In the next experiment, the specimens were tested in 55 bar CO2-only environment for 4 days; then, 0.1
bar pH2S was introduced. After days of exposure, some mackinawite could be detected in the XRD
pattern, while the major phase was still FeCO3. It can be seen from Figure 10 that mackinawite
precipitated as a thin layer on the void sites within the FeCO3 layer. EDS mapping results in Figure 11
also confirmed this was a thin sulfide layer formation. In contrast, after adding 55 bar pCO 2 into 0.1 bar
pH2S environment, no obvious change in corrosion product can be observed compared with that in
H2S-only environment. The corrosion products still were constituted of an inner Fe3O4 layer and an
outer pyrrhotite layer. The only difference between images in Figure 10 and Figure 8 was that most
pyrrhotite was observed as larger, bulker crystals as compared to thin, flaky crystals. This could be due
to the increase of exposure time (8 days vs. 4 days).

Figure 10 SEM morphologies (a) and (b) 55 bar CO2 then adding 0.1 bar H2S, (c) and (d) 0.1 bar
H2S then adding 55 bar CO2, 120oC, initial pH 5.0, 4 + 4 days.

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 Figure 11 Cross-sections and EDS mapping results (a) 55 bar CO2 then adding 0.1 bar H2S, (b)
0.1 bar H2S then adding 55 bar CO2, 120oC, initial pH 5.0, 4+4 days.

Surface profilometry

The surface profilometry of the steel was examined after removing the corrosion products. The typical
images are shown in Figure 12. No obvious localized corrosion was observed for this series of
experiments (Figure 2). Therefore, all were considered as uniform corrosion in the tested CO 2 and/or
H2S environments, which is in good agreement with the previous study.30

Figure 12 Surface profilometry after removing corrosion products (a) 55 bar CO2 then adding 0.1
bar H2S, (b) 0.1 bar H2S then adding 55 bar CO2, 120oC, initial pH 5.0, 4 + 4 days.

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10
 DISSCUSION
CO2/H2S ratio
According to Figure 5, Figure 8Figure 9, iron sulfide mainly formed in the CO2 and H2S mixture
environment with partial pressures under the pCO2/pH2S ratio of 550 at 120oC. The corrosion product
was still dominated by H2S. Obviously, the 500 ratio as a transition point between CO2 and H2S
corrosion is not valid at this high temperature. However, it does not mean only H2S corrosion mitigation
must be taken without the consideration of CO2. The corrosion rate also should be considered, as
shown in Figure 3. Yet, the corrosion rate in the mixed CO2 and H2S environment was much closer to
that in a CO2-only environment (Figure 3), which could suggest that the corrosion rate was controlled
by CO2 even though no FeCO3 corrosion product was detected. Anyhow, the use of the 500 pCO2/pH2S
ratio for making important decisions should be applied with strong caution in the oil and gas industry
and further investigation under different conditions is required.

Role of the Fe3O4 layer

In most cases, the corrosion rate could be closely related to the corrosion product layer formation.
Comparing H2S-only and CO2/H2S mixture (10 bar and 55 bar pCO2) experiments, the thickness of the
inner Fe3O4 layer decreased from 25 µm to essentially zero. It can be concluded that high pressure
CO2 can retard Fe3O4 formation at high temperature in H2S environment. Meanwhile, the corrosion rate
followed a similar decreasing trend, from 2 mm/yr to 0.7 mm/yr (Figure 3). It seems that Fe3O4 layer
was not protective in the H2S-only environment. However, without H2S, Fe3O4 was shown to be very
protective layer31 at high temperature, with a stable corrosion rate below 0.4 mm/yr.
Therefore, the high corrosion rate must also be related to the presence of the iron sulfide layer. Since
Fe3O4 is thermodynamically less stable than iron sulfide, it has been demonstrated that Fe3O4
continuously forms at the steel/Fe3O4 interface, and converts to iron sulfide at the Fe3O4/FeS interface
via Reaction (1) and (2).31
3Fe 2+ +4 H 2O → Fe3O4 + 8H + + 2e −
(1)
Fe3O4 + 3H 2 S + 2 H + + 2e − → 3FeS + 4 H 2O
(2)

Effect of environment change

When H2S was injected into CO2 environment, the LPR corrosion rate increased from 0.15 mm/yr to 0.7
mm/yr. The rise was also observed when CO2 was injected to an H2S-only environment (Figure 3). This
could be attributed to the pH decreasing with acid gas injection. The corrosion rate is hypothesized to
quickly decrease back to the previous level due to the presence of already formed FeCO3 or Fe3O4/FeS
layer. Therefore, the environmental change had almost no effect on the steady corrosion rate once the
original corrosion product has formed. After another 4 days, iron sulfide (mackinawite) precipitated
when H2S was added to the CO2 environment while no FeCO3 precipitation was observed when CO2
was added to the H2S environment, as iron sulfide is more kinetically and thermodynamically favored
than FeCO3 under the testing conditions.32,33 However, longer term experiments are necessary to
determine whether the FeCO3 layer will convert to FeS and consequently affect the general and
localized corrosion rates.

CONCLUSIONS

The corrosion behavior of mild steel in 55 bar pCO2 and/or 0.1 bar pH2S environment at high
temperature was studied for the first time. The main conclusions can be drawn as follows:

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11
 • The CO2/H2S ratio of 500 as the transition point between CO2 and H2S corrosion is not valid at
high temperature. The corrosion products were still dominated by H2S under the CO2/H2S ratio
of 550. Industrial application of this ratio needs more investigation.
• High pressure CO2 can retard Fe3O4 formation in H2S environment. The high corrosion rate in
an H2S-only environment could be related to the continuous Fe3O4 formation and conversion to
FeS.
• No obvious change in steady state corrosion rate was observed when the environment was
switched from sweet (CO2) to sour (H2S) and vice versa in short term experiments.

ACKNOWLEDGEMENTS

The author also 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, PTT, Saudi Aramco, SINOPEC (China Petroleum),
and TOTAL.

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Requests for permission to publish this manuscript in any form, in part or in whole, must be in writing to
NACE International, Publications Division, 15835 Park Ten Place, Houston, Texas 77084.
The material presented and the views expressed in this paper are solely those of the author(s) and are not necessarily endorsed by the Association.
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