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The Efffect of Remperature, CO2, H2S Gases and The Resultant Iron Carbonate and Iron Sulfide
The Efffect of Remperature, CO2, H2S Gases and The Resultant Iron Carbonate and Iron Sulfide
The effect of temperature, CO2, H2S gases and the resultant iron carbonate T
and iron sulfide compounds on the sour corrosion behaviour of ASTM A-106
steel for pipeline transportation
M. Asadiana, M. Sabzib, S.H. Mousavi Anijdanc,∗
a
Young Researchers and Elite Club, Science and Research Branch, Islamic Azad University, Tehran, Iran
b
Young Researchers and Elite Club, Dezful Branch, Islamic Azad University, Dezful, Iran
c
Department of Materials Engineering, Science and Research Branch, Islamic Azad University, Tehran, Iran
Keywords: In this investigation, extracted products corrosion behaviour of sour environment in oil and gas industry was
Sour corrosion studied. Of the important aspects of these products is the presence of significant amounts of CO2 and H2S in the
H2S solution of the sour products. The corrosion mechanism could also be involved during the extraction, trans-
ASTM A-106 steel portation and purification of the sour products. Therefore, the corrosion behaviour of ASTM A-106 Grade A
Potentiodynamic polarization
carbon steel, used for the transportation of oil and gas, in the presence of H2S and CO2 and at different tem-
Electrochemical impedance spectroscopy
Temperature
peratures, was studied by potentiodynamic polarization, electrochemical impedance spectroscopy techniques,
and Scanning Electron Microscope (SEM) equipped with Electron Dispersive Spectroscope (EDS). Corrosion tests
were conducted on the alloy in solutions with 3 wt% NaCl saturated with CO2 gas in the presence/absence of
200 ppm H2S gas at temperatures of 25 °C, 45 °C, 65 °C, 85 °C. Results showed that increasing the temperature of
the solution substantially increased the corrosion rate of the steel under investigation. As well, the presence of
both gases of CO2 and H2S enhanced the corrosion rate. EDS results also showed that iron carbonate and iron
sulfide compounds do not have sufficient stability at high temperatures to protect the metal surface against
corroding agents. And they could not form a uniform coating on the steel surface.
∗
Corresponding author.
E-mail addresses: hashemmousavi@gmail.com, hashemmousavi@srbiau.ac.ir (S.H.M. Anijdan).
https://doi.org/10.1016/j.ijpvp.2019.02.019
Received 10 November 2018; Received in revised form 23 January 2019; Accepted 25 February 2019
Available online 01 March 2019
0308-0161/ © 2019 Elsevier Ltd. All rights reserved.
M. Asadian, et al. International Journal of Pressure Vessels and Piping 171 (2019) 184–193
presence of water is the most common type of corrosion in oil and gas Table 1
industry as the dry CO2 would not lead to corrosion. The mechanism of Chemical composition of the steel used for corrosion analysis (wt%).
CO2 corrosion in the presence of water was explored extensively C Si Mn P S Fe
[15–18]. For this corrosion to occur, several steps should be taken.
Firstly, the CO2 gas dissolves in water and forms H2CO3 acid, which is a ASTM A-106 Grade A 0.25 0.1 0.27–0.93 0.035 0.035 Balance
Analyzed sample 0.11 0.07 0.72 0.021 0.013 Balance
comparatively weak acid, as follows [11–16]:
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M. Asadian, et al. International Journal of Pressure Vessels and Piping 171 (2019) 184–193
0.4367
× 106 = 2911 ppm H2 S
150
1 g Na2 S 2911 ppm H2 S
= x = 0.0687 g Na2 S
x g Na2 S 200 ppm H2 S
The coefficient of 1.1 was used in the above equation as it was as-
sumed that all H2SO4 were consumed and H2SO4 was the rate con-
trolling factor. Since 98% purity acid was used in this investigation,
8 ml H2SO4 of 0.1 M together with 0.068gr Na2S were added to the
electrolyte. Electrochemical analyses were performed at 1 atm and at
temperatures of 25 °C, 45 °C, 65 °C, 85 °C to understand the effect of
temperature on the corrosion rate.
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M. Asadian, et al. International Journal of Pressure Vessels and Piping 171 (2019) 184–193
Table 2
Parameters obtained from tafel polarization curves of the steel in the solution
saturated with CO2 gas and without H2S.
Temperature (oC) Corrosion Icorr (μA/cm2) Anodic Cathodic
potential (V) slope (V/ slope (V/
dec.) dec)
Fig. 2. OCP of ASTM A-106 Grade A pipeline steel in 3 wt% NaCl saturated with
CO2 and 200 ppm H2S gases.
Fig. 4. Corrosion rate for ASTM A-106 Grade A carbon steel in the solution
saturated with CO2 gas at different temperatures of the solution.
M
Corrosion Rate = 3.268 × Icorr ×
n (3)
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M. Asadian, et al. International Journal of Pressure Vessels and Piping 171 (2019) 184–193
Table 3
Parameters obtained from tafel polarization curves for the steel in the 3 wt% NaCl solution saturated by CO2 and 200 ppm H2S gases at different temperatures.
Temperature (oC) H2S (ppm) Corrosion potential (V) Icorr(μA/cm2) Anodic slope (V/dec.) Cathodic slope (V/dec)
the presence of both gases of CO2 and H2S. As can be seen in Fig. 5, structure of iron sulfide. Consequently, there are many defects in this
similar to the previous case (Fig. 4), increasing the temperature in- non-uniform layer [32–34].
creased corrosion current density. It can also be seen in this figure that Overall, H2S gas is three times more soluble than CO2 gas. But the
only active behaviour from anodic half reaction is obtained for tem- acid formed by H2S gas in the solution is three times weaker than the
peratures below 65 °C. While at 65 °C a small amount of passive-active carbonite acid. Therefore, the effect of H2S in reducing pH is almost
behaviour can be seen and at 85 °C more of this behaviour is observed. similar to CO2. Another issue is, unlike CO2 dissolution, H2S gas does
In fact, in the presence of both gases and at higher temperatures, a not need to be hydrated for the acid formation, hence for the faster
passive layer is formed on the metal surface when the potential is in- kinetics of its reaction [35]. It was claimed that the level of surface
creased. This passive layer prevents, to a great extent, corrosion rate protection against corrosion in the presence of H2S gas is highly de-
increment. There is a possibility that this layer is not stable and will be pendent on the pH of the electrolyte. In very low pH condition (below
detached from the surface after some time [31,32]. This is due to the 2), free iron ions are available in the solution and iron sulfide has a high
fact that with increasing the concentration of the sour gases, the solubility in the electrolyte. Therefore, in this pH range, iron sulfide
number of attacking ions increased and the surface of the steel was does not precipitate on the metal surface and H2S only plays an ac-
under attack more than before. Therefore, the corrosion rate after the celerating role for the iron dissolution reaction. Whereas, if the pH is
polarization tests was increased at higher concentrations of the sour between 3 and 5, due to the formation of iron sulfide layer, part of the
gases. surface would be covered and there will be higher corrosion resistance
Another point in the polarization curves is in the cases of with and for the metal. Though, if H2S concentration increases, such an increase
without H2S, both anodic and cathodic branches of the tafel curve move in concentration would increase bisulfide (HS−) ions in the solution
towards higher current densities with increasing the temperature. This and eventually weakens the film formed on the surface [32,34]. Fig. 6
implies a higher exchanged current density at higher temperatures. It clearly shows such an increase in the corrosion rate with changing the
can therefore be deducted that temperature plays a significant role on temperature. For example, at 85 °C, the corrosion rate is 93.55 mpy,
anodic and cathodic reactions. Indeed, with increasing the temperature which is a relatively high value.
the dissolution rate of Fe in the electrolyte increases together with Since electrochemical reactions are dependent on temperature, it
higher cathodic reactions on the steel surface. Moreover, increasing the can be said that the main effect of temperature is to enhance the ki-
temperature of the solution increased the slopes of anodic and cathodic netics of anodic and cathodic reactions on the surface of the electrode.
tafel curves. The slope is higher when 200 ppm H2S was present in the Such an enhancement leads to an increase in the anodic and cathodic
solution, hence the limit of cathodic current is observable. The presence currents and subsequently increases total current as well. This increase
of H2S produces oxidation agents such as HS− and S2− in the electro- in current, in the circuit from the corrosion reaction, means higher
lyte in a two steps process. Although HS− is weaker than acids such as corrosion rate at higher temperature [36,37]. As well, equilibrium
HCl or H2SO4, it is capable of reacting with Fe ions to form an iron constant (K) for the reactions on the metal surface is another important
sulfide layer. The formation of this iron sulfide layer increases the factor. The constant of a reaction is dependent on the temperature of
chance of corrosion by HS− compared to other agents that provide the surrounding environment. Therefore, it is expected that a reaction
protons. Consequently, the corrosion rate is only dependent on the will be non-equilibrium as the temperature rises and consequently its
amount of H2S, HS− ions, free metal (uncoated surface of the metal)
and temperature. Therefore, the formation of surface layer is one of the
most important factor on the corrosion rate. The growth of the layer is
dependent on the kinetics of the formation of the layer [34,35]. Only
iron carbonate precipitates are formed in case merely CO2 corrosion is
present. However, when H2S is present, different types of Fe sulfides
such as amorphous Fe sulfide, Mackinawite, Cubic ferrous sulfide,
Greigite, FeeS phases, pyrrhotite, Troilite, pyrite (FeS2) form. Among
these products, the Mackinawite layer is firstly formed on the surface by
a direct reaction. When there are several agents in the solution, a
competition is present among them to form as the surface layer. If the
amount of H2S gas is lower than CO2, the formation of iron sulfide layer
will be mixed with the formation of FeCO3 layer. Not only the forma-
tion of the layers from these two gases is dependent on the solubility of
carbonate and sulfide layer, but also the competition between these two
layers is important as well. The iron sulfide layer is an insulator which
can prevent corroding ions from entering the metal surface. In fact, it
can play a detective layer and reduces the bared metal surface from
being exposed to the corroding environment. Generally, the adhesion
and protective properties of iron sulfide layer is higher than FeCO3
layer. In spite of this, the iron sulfide layer cannot be used to fully
prevent corrosion. One of the main problems with this layer is the Fig. 6. Corrosion rate of the steel in 3 wt% NaCl solution saturated with CO2
mixing of Fe and S by non-stoichiometric ratio in the crystalline and 200 ppm H2S at 25 °C, 45 °C, 65 °C, 85 °C.
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M. Asadian, et al. International Journal of Pressure Vessels and Piping 171 (2019) 184–193
B
icorr = imperfect semi-circular rings with temperature is indicative of the effect
Rp (4)
of temperature rise and the presence of H2S gas in the corrosive en-
Where B = 2.3(ba +c b ) and ba and bc are tafel slopes for cathodic and
b b
vironment on the reduction of solution resistance (Rs) as well as on
a c
anodic reactions. lowering the corrosion resistance (Rp). It is clear from these curves that
And the impedance for the circuit is obtained as follows: no other temperature constant is added to the equivalent circuit.
2
Direct Loop Extrapolation, Fitting Curve and Equivalent Electrical
2
Rp Rp Circuit methods are used to obtain various parameters of impedance. In
Z Rs + (Z ) 2 =
2 2 (5) equivalent electrical circuit method, by assuming an equivalent circuit,
Rp wCRp2 a mathematical model that describes the kinetics of corrosion reaction
Where Z = Rs + and. Z = is build and the laboratory data are assessed based on this equation.
(wCRp)2 1 + (wCRp)2
Equation (5) is for the half circle of Nyquist plot. Rp, which is called ZPlot and ZView softwares, produced by Solarton Inc., were used in this
polarization resistance, is the diameter of this half circle [40–43]. research for this purpose.
The information obtained from electrochemical impedance tests are The Nyquist curve obtained is in the form of depressed semi-circle
shown in different ways. One of the most common ways is by Nyquist with the center of the circle below the actual axis. Usually, this beha-
curve where virtual impedance (Z″) versus real impedance (Z′) for each viour is related to the non-uniformity and roughness of the surface. To
frequency is plotted. Fig. 7 shows the Nyquist plot for virtual im- fit the data in this condition, a circuit with the maximum compatibility
pedance (Z″) versus real impedance (Z’) for each frequency of the steel and minimum error should be employed. Therefore, a Constant Phase
in the 3 wt% NaCl solution saturated with CO2. Fig. 8 also shows Ny- Element (CPE) was used instead of a capacitor in the equivalent circuit.
quist plot for the steel in the 3 wt% solution saturated with both gases at A Constant Phase Element (CPE) is considered as a parallel capacitor
different temperatures of 25 °C, 45 °C, 65 °C and 85 °C. with a resistance and its equation as follows:
As can be seen in Figs. 7 and 8, all curves obtained from the im-
ZCPE = Y 0 1 (j ) n
(6)
pedance test consist of a semi-circular one capacity ring which extends
from high frequencies to low frequencies. The changes of these Where Y0 is the representative of the capacitor characteristic in the
189
M. Asadian, et al. International Journal of Pressure Vessels and Piping 171 (2019) 184–193
Table 4
Parameters obtained from electrochemical impedance curves of the steel in the
3 wt% NaCl solution saturated with CO2 gas at different temperatures.
Temperature (oC) RSolution (Ω.cm2) RSteel (Ω.cm2) Y × 104 (sn/cm2 Ω) n
Table 5 Fig. 10. Bode curves for the steel in 3 wt% NaCl saturated with CO2 gas at
Parameters obtained from electrochemical impedance curves of the steel in the different temperatures.
3 wt% NaCl solution saturated with CO2 and H2S gases at different tempera-
tures.
Temperature (oC) H2S (ppm) RSolution (Ω.cm2) RSteel (Ω. Y × 104 n
cm2) (sn/
cm2.Ω)
190
M. Asadian, et al. International Journal of Pressure Vessels and Piping 171 (2019) 184–193
Fig. 12. Bode curves for the steel in 3 wt% NaCl saturated with CO2 and H2S
gases at different temperatures.
Fig. 14. a) SEM micrograph of the morphology of the steel surface after cor-
rosion test in a 3 wt% NaCl solution saturated with CO2 gas at 65 °C, b) EDS
spectra for this sample.
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M. Asadian, et al. International Journal of Pressure Vessels and Piping 171 (2019) 184–193
barrier that it makes to prevent corroding agents from entering the The following conclusions were obtained by conducting corrosion
metal surface. Indeed, this layer is an effective one in preventing further investigation of ASTM A-106 Grade A pipeline steel in 3 wt% NaCl
electrochemical corrosion reactions [36]. solution saturated with CO2 and 200 ppm H2S gases at various tem-
Fig. 15 shows SEM micrograph together with EDS analysis of the peratures.
steel in a 3 wt% NaCl solution saturated with both CO2 and H2S gases at
65 °C. As can be seen in this figure, a non-adhesive film is formed on the 1 The sour corrosion behaviour of ASTM A-106 Grade A pipeline steel
surface of the steel. The composition of this steel contains elements such and the kinetics of surface reactions are highly dependent on the
as C, Fe, O, and S together with small amount of Na and Cl. The pre- temperature and its changes. Increasing the temperature of the so-
sence of S on the surface film is indicative of H2S corrosion. As the lution from 25 °C to 85 °C substantially increased corrosion rate of
amount of H2S was lower than CO2, it is hard to say that H2S corrosion the steel.
was the dominant mechanism. Generally, the structure and the cap- 2 EDS analysis showed that FeCO3 and FeS compounds do not have
ability of the iron sulfide protective film is dependent on the con- sufficient stability to protect the metal surface at higher tempera-
centration of H2S [41,42]. As well, the capacity of the surface layer for tures and cannot form a uniform coating on the surface.
protection is dependent on the pH of the solution. In low pH regime, 3 Equivalent circuit of the electrical double-layer for the investigated
pH < 2, Fe has more tendency to dissolve in the solution. Therefore, pipeline steel in an environment containing CO2 and H2S sour gases
iron sulfide does not precipitate on the metal surface. In this situation, consisted of polarization resistance, solution resistance and a con-
the presence of iron sulfide leads to a higher dissolution rate of iron. stant phase element with capacitance behaviour.
But, for the pH in the range of 3–5, H2S would have a protective role on 4 Potentiodynamic polarization curves for the investigated pipeline
the surface of the electrode due to the formation of iron sulfide. In this steel in the environment containing CO2 and H2S sour gases showed
situation, the concentration of H2S has a significant effect on the pro- that with increasing temperature, both cathodic and anodic bran-
tective role of the sulfide layer. On the other hand, the concentration of ches of the tafel curve moved towards higher corrosion current
H2S is also very important as with the increase of the H2S concentra- density.
tion, the film would weaken and even the pH in the range of 3–5 cannot 5 The presence of H2S in the corrosive environment of the pipeline
protect the film [36,42]. steel formed oxidation agents such as bisulfide (HS−) and S−2 sul-
It is reported that temperature variation does not have much an fide in the electrolyte. Due to this phenomenon, the corrosion rate of
effect on the H2S corrosion. Previous findings show that this is due to the steel in the environment was increased five times.
the formation of iron sulfide layer and in fact the corrosion rate is 6 All curves and parameters related to the electrochemical impedance
controlled at the presence of iron sulfide in the surface film [43]. spectroscopy (Nyquist plot, Bode and Bode-Phase curves) indicated
192
M. Asadian, et al. International Journal of Pressure Vessels and Piping 171 (2019) 184–193
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