Engineering Failure Analysis 146 (2023) 107079

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Engineering Failure Analysis

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

The synergistic effect of temperature, H2S/CO2 partial pressure

and stress toward corrosion of X80 pipeline steel
Xiaoguang Huang a, Longchi Zhou a, Yukun Li a, Zhongzhe Du a, Qihui Zhu a,
Zhongying Han b, *
a
College of Pipeline and Civil Engineering, China University of Petroleum, Qingdao 266580, China
b
School of Petroleum Engineering, China University of Petroleum, Qingdao 266580, China

A R T I C L E I N F O A B S T R A C T

Keywords: In this work, the H2S / CO2 coexistence environment was simulated in a high-temperature and
H2S/CO2 high-pressure reactor. The influence of H2S/CO2 partial pressure (0/1.2, 0.7/1.2 and 2.0/1.2
X80 MPa), temperature (50, 100 and 150 ◦ C) and applied stress (30%, 70% and 90% σ s) on the
Corrosion rate
corrosion rates of natural gas pipeline steel X80 was investigated by the weight loss measure­
Temperature
ments combined with the SEM, EDS and XRD techniques. The results show that the corrosion of
Stress
X80 steel under pure CO2 condition is much more serious than that under H2S/CO2 coexistence.
The corrosion stability of amorphous film can be improved by the formation of amorphous Cr
(OH)3 in the presence of H2S, which provides better surface protection than in the pure CO2
environment. The corrosion of X80 steel in H2S/CO2 coexistence is dominated by H2S corrosion
and the corrosion rates increase with the increase of H2S partial pressure. The corrosion rate
firstly increases with the increase of temperature, and the highest corrosion rate occurs near 100
◦
C under the existing experimental conditions. After that, the corrosion rate began to decrease.
The applied stress significantly affects the corrosion rate, and high stress speeds up the corrosion
process of X80 steel in the H2S/CO2 coexistence environment.

1. Introduction

The exploitation of deep condensate gas fields and high-sulfur gas reservoirs in China causes an increase in the content of H2S, CO2
and other corrosive media in the natural gas, which intensifies the corrosion and stress corrosion cracking risk of the pipeline and
seriously affects the transmission safety of natural gas [1,2]. In the process of natural gas transmission, water vapor always condenses
on the top and side walls of the pipeline due to the change in ambient temperature and pressure. The dissolution of H2S and CO2 gas
condensate water lead to the thin liquid film corrosion on the inner wall. When the condensate water converges and accumulates at the
bottom of the pipeline, the corrosion could be accelerated after the dissolution of H2S and CO2 [3,4]. Since the natural gas pipelines are
working under pressure, surface corrosion will cause stress concentration and increase the risk of stress corrosion cracking. Hence, it is
very necessary to analyze the corrosion behavior and provide protective measures for natural gas pipelines in the H2S/CO2 coexistence
environment.
When it comes to the corrosion of natural gas pipelines, we have to mention the serial research of Schmitt et al. in CO2 corrosion as

* Corresponding author.
E-mail address: hanzhying@upc.edu.cn (Z. Han).

https://doi.org/10.1016/j.engfailanal.2023.107079
Received 12 October 2022; Received in revised form 3 January 2023; Accepted 16 January 2023
Available online 20 January 2023
1350-6307/© 2023 Elsevier Ltd. All rights reserved.
X. Huang et al. Engineering Failure Analysis 146 (2023) 107079

early as the 1990s. Schmitt’s investigation into the corrosion mechanism of carbon steel in oxygen-free carbon dioxide solutions was
very instructive for CO2 corrosion protection of natural gas pipelines [5–7]. Since the 2010s, Nesic group members have been working
on the CO2 corrosion mechanism and corrosion inhibition of mild steel in gas transportation systems [8–10]. However, the above
research mainly focused on pure CO2 corrosion. In fact, natural gas pipelines often contain mixtures of CO2 and H2S, so the corrosion of
pipelines induced by the H2S/CO2 mixture also needs attention. It is generally believed that H2S/CO2 condensate aqueous solution
causes obvious corrosion under pipeline scale, and the corrosion characteristics are affected by the condensation rate of steam [11]. In
terms of the corrosion mechanism, Dong et al. concluded that the corrosion process mainly depended on the adsorption characteristics
of corrosive anions [12]. From this perspective, the partial pressure of H2S/CO2 naturally affects the corrosion rate and corrosion
mechanism [13,14]. Therefore, how to form a corrosion inhibition between the solution and the pipeline, reduce the adsorption of
corrosive anions and improve the charge transfer resistance in the chemical reaction, has become a better selection for corrosion
protection of pipeline [15,16]. Meanwhile, the compactness and stability of corrosion products affect the corrosion process. Smith
et al. [17] believed that sulfide was more stable in chemical properties than FeCO3. If H2S exists in the corrosion environment, it always
dominates the corrosion process instead of CO2. However, it is more widely accepted that when H2S and CO2 coexist, they produce the
competitive and synergistic effects on the corrosion mechanism of the pipeline, that is, the partial pressure ratio of H2S/CO2 de­
termines the corrosion mechanism and control state under the coexistence conditions [18–20].
Nevertheless, there is still a relative lack of corrosion behavior research on natural gas pipelines in different H2S/CO2 partial
pressure conditions, especially for the pipelines above X80 grade, which have become the present mainstream transmission pipelines
of natural gas. Therefore, in this work, the high-temperature reactor is used to simulate the corrosive medium environment, and the
factors affecting the corrosion behavior, corrosion product film structure composition, and corrosion mechanism of API X80 natural
gas pipeline steel in the H2S/CO2 coexistence environment are extensively studied, to provide an experimental reference for the safety
of high sulfur natural gas transportation.

2. Experimental procedure

2.1. Materials

The experimental pipeline steel X80 was produced by Tianjin Steel Pipe Co., Ltd, with chemical content and Metallographic
structure shown in Table 1 and Fig. 1, respectively. FCZ high temperature-pressure magnetomotive reactor was used to simulate the
corrosive environment. The working diagram is shown in Fig. 2. The static weight loss method of the hanging piece was adopted to
calculate the corrosion weight loss rate under a no-stress state, and the piece size is 50 × 10 × 3 mm. The sample was loaded by four-
point bending to measure the effects of stress levels on the corrosion rate. The hanging piece and bending sample are polished step by
step with 400, 600, and 1000 sandpaper respectively to eliminate the influence of machining. The experimental solution is a simulated
solution of the working condition in which chemical solutes are dissolved in deionized water. The solute ratio is calculated from the
test results as follows: Cl- 50000 mg/L, Ca2+ 15000 mg/L, Mg2+ 6000 mg/L, Na+ 1500 mg/L, K+ 1000 mg/L, pH = 4.5, total pressure
20 MPa.The experimental items and test conditions are shown in Table 2. Items 1–3 in Table 2 are used to analyze the influence of H2S
partial pressure (0/0.7/2.0 MPa) on the corrosion rate, and items 3–5 are comparative experiments at different temperatures (50 /100
/150 ◦ C), and items 3, 6, 7 and 8 constitute the comparative experiments under different stress levels.

2.2. Experimental procedure

All the specimens were grinded by a series of water sandpapers and finally polished by a 5 µm diamond paste. All the specimens
were successively rinsed with deionized water, acetone, and cleaned with distilled water before the tests. The weight loss samples were
assembled on a special fixture, and the samples under four points bending were placed in the reactor together with their loading
devices. After the samples were arranged, the nitrogen was filled into the reactor until the pressure reaches 20 MPa, and the state was
maintained for 2 h to remove the oxygen, after then the reactor was heated by the electric heating device to the required temperature.
What follows, H2S and CO2 are pumped in respectively according to the preset partial pressure in the system, and then total pressure in
the reactor was maintained at 20 MPa.
When all the experiments were finished, the samples were washed to remove the corrosion products on the surface with the solution
(500 ml HCl + 20 g hexamethylenetetramine + 500 ml distilled water). After that, the samples were washed with absolute ethanol and
dried for the corrosion rate measurement. The surface morphology of the corrosion sample was observed by Cambridge S360 scanning
electron microscope, the phase structure of the corrosion product was analyzed by Shimadzu XRD-6000 X-ray diffractometer, and the
composition of the corrosion product was analyzed by League 2000 energy spectrometer.

Table 1
Chemical compositions of X 80 steel (wt %).
Material C Ni Si Mn Cr Mo P S Cu Fe

X 80 0.048 0.268 0.195 1.717 0.219 0.184 0.012 0.002 – bal

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X. Huang et al. Engineering Failure Analysis 146 (2023) 107079

Fig. 1. Metallographic structure of X80 steel.

Fig. 2. Setup of the high-temperature and high-pressure reactor.

Table 2
Experimental items and the corresponding testing conditions.
Item Investigating Stress H2S content(g/m3)-partial pressure CO2 volume ratio (%)-partial pressure Temperature Corrosion time
factors (MPa) (MPa) (◦ C) (h)

1 H2S content 0 0 6%-1.2 100 168

2 0 50-0.7 6%-1.2 100 168
3 0 150-2.0 6%-1.2 100 168
4 Temperature 0 150-2.0 6%-1.2 50 168
5 0 150-2.0 6%-1.2 150 168
6 Stress level 30% σs 150-2.0 6%-1.2 100 168
7 70% σs 150-2.0 6%-1.2 100 168
8 90% σs 150-2.0 6%-1.2 100 168

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X. Huang et al. Engineering Failure Analysis 146 (2023) 107079

3. Experimental results and analysis

Weight loss tests were adopted on to measure the corrosion rate in different H2S/CO2 environments. The corrosion rates under
different conditions are listed in Table 3. All the specimens were weighed for the original weights W0 and the final weight W1 before
and after the tests by a digital balance with a precision of 0.0001 g. The corrosion rates are calculated by Eq. (1) [21].

Vcorr = 8.76 × 104 × ΔW/(ρSt) (1)

where Vcorr is the corrosion rate (mm/a), ΔW = W0-W1 is the weight loss, ρ is the mass density (g/cm3), S is the exposed surface area of
the specimen (cm2), and t is the immersion time (s).

3.1. Effect of H2S partial pressure on corrosion behavior

Fig. 3 shows the corrosion morphology of the X80 samples under 100 ◦ C and different H2S partial pressures when the partial
pressure of CO2 was maintained at 1.2 MPa. When comparing the SEM images of corrosion product in Fig. 3 (a), (b), and (c), the surface
corrosion in a pure CO2 environment is more severe than that in presence of H2S. Under low magnification conditions, the corrosion
products in pure CO2 corrosion are in coarse particles, and the adhesion of the corrosion product film is weak and loose. Under high
magnification conditions, a large number of regular grains in a block or rectangular shape can be observed on the surface, and local
corrosion on the surface is very serious. The corrosion status in Fig. 3 (b) is the gentlest and the corrosion product exhibits a uniform
thin film with some local corrosion dimples. Corrosion status in Fig. 3(c) is as similar to Fig. 3 (b), but slightly serious. The surface
corrosion statuses under different partial pressures are consistent with the calculated corrosion rates listed in Table 3. Pots et al. found
that the influence of H2S content on corrosion behavior under the coexistence of H2S and CO2 depends on the partial pressure ratio
PCO2 /PH2S [22]. It can be concluded that a small amount of H2S can effectively inhibit CO2 corrosion. However, with the increase of
H2S content in the system, the corrosion process is dominated by H2S corrosion and the corrosion rate gradually increases with the
increase of partial pressure [18,23].
Fig. 4 shows the EDS and XRD results of corrosion products on the sample surface under different H2S partial pressures. According
to the energy spectrum analysis and XRD diffraction results in Fig. 4, the main component of corrosion film is FeCO3 when PH2S = 0.
However, the element of O and Fe are much higher than C, which shows the Fe2O3 existence in the corrosion product. Also, the peak of
the Ca element in Fig. 4(a) points to CaCO3. Since CaCO3 has a less protective effect on the substrate than FeCO3, the inclusion of
CaCO3 and Fe2O3 affects the protection of FeCO3 film and then results in a higher corrosion rate. When H2S partial pressure increases to
0.7 MPa and 2.0 MPa, as PCO2 /PH2S < 20, the corrosion reaction in the system is mainly H2S corrosion, and the corrosion product is
mainly composed of FeS [22]. The formed FeS film has a stronger adhesion and protection, so the corrosion rate in the system con­
taining H2S is lower than that in pure CO2 corrosion. The increase of H2S partial pressure accelerates the deposition of FeS1-x product
film on the surface. However, the higher H2S partial pressure reduces the pH value of the system. These two factors work together,
resulting in the acceleration of corrosion in a higher H2S partial pressure [24].
Fig. 5 demonstrates the cross-sectional backscattered electron images and EDS line scanning analysis of corrosion scales on the

Table 3
Corrosion rate corresponding to each group.
Item Sample No. W0 (g) W1 (g) ΔW (g) Corrosion rate (mm/a) Average corrosion rate (mm/a)

1 11# 11.3357 11.1208 0.2149 1.0732 1.0899

12# 11.6069 11.3815 0.2254 1.0994
13# 11.5431 11.3194 0.2337 1.0971
2 21# 11.2936 11.2623 0.0313 0.1569 0.1515
22# 11.3081 11.2763 0.0318 0.1587
23# 11.2989 11.2712 0.0277 0.1388
3 31# 11.3412 11.2822 0.0590 0.2896 0.3005
32# 11.4731 11.4106 0.0625 0.3136
33# 11.3328 11.2733 0.0595 0.2982
4 41# 11.3162 11.2618 00,544 0.2381 0.2635
42# 11.3291 11.2668 0.0623 0.2724
43# 11.2926 11.2288 0.0638 0.2799
5 51# 11.3322 11.2432 0.0890 0.4436 0.2866
52# 11.6123 11.5727 0.0396 0.1931
53# 11.3204 11.2758 0.0446 0.2230
6 41# 44.8963 44.7566 0.2063 0.3111 0.3108
42# 44.7863 44.6492 0.1371 0.3061
43# 44.6425 44.5018 0.1407 0.3152
7 51# 44.7894 44.6355 0.1539 0.3436 0.3335
52# 44.6128 44.4678 0.1450 0.3130
53# 44.8246 44.6704 0.1542 0.3439
8 41# 43.9874 43.8087 0.1787 0.4062 0.3724
42# 45.1026 44.9544 0.1482 0.3286
43# 44.6398 44.4691 0.1707 0.3824

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X. Huang et al. Engineering Failure Analysis 146 (2023) 107079

Fig. 3. Surface corrosion morphology of the samples under different H2S partial pressure.

steels. As shown in Fig. 5(d-f), the scales on X80 steel under different PCO2 /PH2S ratios all had an obvious elemental irregular dis­
tribution after 180 h tests. The outer scale of pure CO2 corrosion (Fig. 5 a, d) mainly exhibits a two-layer distribution, the outer layer
contained C, Fe and O elements (FeCO3), the inner scale mainly contains Fe, S, C and O elements (mixture of FeCO3, CaCO3 and Fe2O3).
However, when the system was filled with H2S, H2S corrosion gradually become prominent and dominated the corrosion process. As
shown in Fig. 5 (e, f), the C content decreases and S content increases in surface corrosion product when PH2S increases, and the C
content is very low when PH2S = 2.0 MPa. The EDS line scanning analysis is consistent with the XRD results.

3.2. The influence of temperature

To investigate the influence of temperature on corrosion, comparative experiments were carried out at 50, 100, and 150 ◦ C,
respectively. The pressure condition remains unchanged, i.e., PH2S = 2.0 MPa, PCO2 = 1.2 MPa and total pressure 20 MPa. The
experimental results show that the corrosion rate (0.2635 mm/a) at 50 ◦ C and (0.2866 mm/a) at 150 ◦ C are both less than that at 100
◦
C (0.3005 mm/a), as shown in Fig. 6. Corrosion is most likely to occur at about 100 ◦ C under the pressure condition set in the
experiments.
Fig. 7 demonstrates the surface corrosion morphology under temperatures. At 50 ◦ C, the surface is uniformly distributed with a
dense corrosion product layer of small irregular grain in close connection. When the temperature reaches 100 ◦ C, the corrosion product
converts to a loose flocculent layer which has extremely poor protection. When the temperature rises to 150 ◦ C, the surface is covered
with a relatively dense crystalline corrosion product layer. The surface corrosion morphology is consistent with the measured
corrosion rate. Fig. 8 shows the EDS and XRD results of corrosion products under different temperatures. Except for the diffraction peak
of matrix Fe, the main EDS peak of the corrosion product corresponds to FeS, which greatly determines the property of the corrosion
product film. There exist different inclusions, for example, a small amount of iron, chromium, and calcium oxide in the reaction
products under different temperatures, but these elements cannot produce an obvious effect on the corrosion rate.
In fact, the temperature-affected corrosion is an extremely complex process. In short, it can be seen as the interaction of activation
energy of corrosion reaction, film-forming mechanism, pH value, and solubility of H2S/CO2. Evidently, activation energy increases,

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X. Huang et al. Engineering Failure Analysis 146 (2023) 107079

Fig. 4. EDS and XRD results of the corrosion product under different H2S partial pressures.

Fig. 5. Cross-sectional backscattered electron images and elemental distributions in the cross-section of the corrosion scales on (a, d) PH2S = 0 MPa;
(b, e) PH2S = 0.7 MPa, and (c, f) PH2S = 2.0 MPa.

and corrosion accelerates with the increase in temperature, however, the increase in temperature reduces the solubility of H2S/CO2
gas. What’s more, temperature also affects the film-forming mechanism of corrosion products and makes it possible for the film to
inhibit corrosion [25]. Besides, corrosion can also be affected by the compactness, grain size, and composition of the corrosion
products, and the adhesion between the corrosion products and the matrix. Combined with all the above reasons, the corrosion rate of
X80 steel increases first and then decreases with the increase in temperature, and the corrosion rate reaches its maximum near 100 ◦ C.

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X. Huang et al. Engineering Failure Analysis 146 (2023) 107079

Fig. 6. Corrosion rates of X80 under different temperatures.

Fig. 7. Surface corrosion morphology of X80 under different temperatures.

3.3. The influence of stress

The four-point bending loading method (constant strain method) was used to load the stress. The pure bending deformation occurs
in the sample section between the inner fulcrums in the four-point loading device, and the upper and lower sides are subject to uniform
longitudinal compressive and tensile stresses respectively. The maximum stress of the pure bending section can be respectively
elevated to 30% σs, 70% σs, and 90% σs by controlling the value of load F. Fig. 9 gives the corrosion rates of the samples under different
applied stresses, it can be seen that the corrosion rate increases with the increase of the applied stress.
Fig. 10 shows the corrosion morphology of the sample surface under different stress levels. With the increase of applied stress, the
film thickness of corrosion products increased significantly, the grains of corrosion products became larger, the connection between
grains became looser, and the corrosion rate increased. When the applied stress reaches 90% σs, there are obvious hydrogen bubbles on
the surface, and the corrosion product film has large particles and poor adhesion. However, no obvious stress corrosion cracking
phenomenon was found on the surface under different stresses, indicating that X80 steel is less sensitive to stress corrosion cracking
under high temperature and high pressure.

4. Discussions

From Fig. 4 (b) and (c), it can be seen the Cr enrichment phenomenon in both cases. Fig. 11 gives the high-resolution XPS spectrum
of the Cr element in corrosion product film with 0.7 and 2.0 MPa H2S partial pressures, respectively. The peak results show that Cr2p3/2
has obvious binding energy peaks near 576.2, 577.3, and 585.4 eV, which correspond to Cr2O3, Cr (OH) 3, and Cr2O3, respectively. This
indicates that Cr mainly exists in the combined state of Cr (OH) 3 and Cr2O3 in the corrosion product film. The co-deposition of
amorphous Cr (OH) 3 and FeS can form a clay-like mixture layer in the corrosion product film, which makes the FeS layer more stable.
Therefore, surface corrosion protection can be more prominent.
The influence of applied stress on corrosion behavior is obvious. However, in real service conditions, the stress level of the pipeline
is generally not so high, but its accelerated effect on the corrosion process can not be ignored. More seriously, if the pipeline has
pressure fluctuations or is subject to external dynamic loads, the pipeline may undergo alternating stresses and suffer corrosion fatigue

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X. Huang et al. Engineering Failure Analysis 146 (2023) 107079

Fig. 8. EDS and XRD results of corrosion product under different temperature.

Fig. 9. Corrosion rates of the samples under different applied stresses.

failure [26–28]. When the stress changes alternately, even if the stress level is very low, the corrosion products on the pipeline surface
constantly fall off during repeated pulling and pressing. A typical feature of low-stress corrosion fatigue failure is that the corrosion
product film cannot be effectively formed. This may be a very dangerous situation for natural gas transmission.

5. Conclusions

In this work, combined with SEM, EDS, and XRD techniques, the synergistic effects of H2S partial pressure, temperature, and
applied stress on the corrosion rate and corrosion mechanism of X80 pipeline steel were investigated. It is concluded that:
(1)The corrosion rate of pure CO2 is higher than that in H2S/CO2 coexistence. The stability of corrosion production film can be
improved by the formation of amorphous Cr (OH)3 in the presence of H2S, which provides better surface protection than in the pure
CO2 environment.
(2)When the partial pressure ratio PCO2/ PH2S < 20, the corrosion process of X80 steel is mainly dominated by the H2S corrosion
reaction. The corrosion rate under high H2S partial pressure is greater than that under a lower H2S partial pressure.

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X. Huang et al. Engineering Failure Analysis 146 (2023) 107079

Fig. 10. Surface corrosion of the samples under different stress levels.

Fig. 11. XPS spectra and decomposition of peaks for Cr2p3/2 in outer corrosion production layer in different H2S partial pressure.

(3) The corrosion rate first increases and then decreases with the increase of simulated temperature in the range from 50 ◦ C to 150
◦
C, and the highest corrosion rate occurs near 100 ◦ C. Applied stress has a great influence on the corrosion rate and higher stress leads
to the acceleration of the corrosion process. No trace of stress corrosion cracking was found on the sample surface, and the X80 steel

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exhibits high-stress corrosion cracking resistance under a high-temperature and high-pressure H2S/CO2 coexistence environment.

CRediT authorship contribution statement

Xiaoguang Huang: Conceptualization, Methodology, Investigation, Writing – original draft. Longchi Zhou: Data curation,
Writing – review & editing. Yukun Li: Project administration, Supervision. Zhongzhe Du: Investigation. Qihui Zhu: Validation,
Visualization. Zhongying Han: Validation, Resources, Visualization, Funding acquisition.

Declaration of Competing Interest

The authors declare that they have no known competing financial interests or personal relationships that could have appeared to
influence the work reported in this paper.

Data availability

No data was used for the research described in the article.

Acknowledgements

The research work was supported by the Fundamental Research Funds for the Central Universities of China (No. 22CX03029A), the
Natural Science Foundation of Shandong Province (No. ZR2020ME092) and the National Natural Science Foundation of China (No.
U1762216).

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