Int. J. Corros. Scale Inhib., 2023, 12, no.

3, 811–824 811

Study of the protection of carbon steel with an inhibitory

composition in hydrogen sulfide environments by electrochemical
methods
L.E. Tsygankova,1 * A.E. Abramov,1 A.A. Uryadnikov,1
T.V. Semenyuk,1 K.O. Strel’nikova,2 R.K. Vagapov2
and O.G. Mikhalkina2
1
Derzhavin State University, ul. Internatsyonalnaya, 33, Tambov, 392000,
Russian Federation
2
Gazprom VNIIGAZ LLC, Proektiruemyi proezd 5537, 15, 1, Razvilka, s.p. Razvilkovskoe,
Leninsky distr., 142717 Moscow region, Russian Federation
*E-mail: [email protected]
Abstract
The protective effectiveness of the inhibitory composition of substances (25–200 mg/L) in
relation to the corrosion of carbon steel in model stratum waters of oil and gas fields (M1 and
NACE) saturated with hydrogen sulfide (400 mg/L) has been studied. The protective
composition is a product of the interaction of fatty tallow polyamines with ethylene oxides in
an alcohol solvent. The studies were carried out by the potentiodynamic polarization and
impedance spectroscopy methods. An electrochemical diffusion technique was used to evaluate
the effect of an inhibitory composition on the penetration of hydrogen into a metal. According
to the potentiodynamic polarization data, the inhibitory composition slows down mainly the
cathodic process on the steel electrode, causing a decrease in the corrosion current with a
protective effect that increases with its concentration and reaches 87 and 94% at 200 mg/L in
M1 and NACE media, respectively. Electrochemical impedance spectroscopy has shown that
there is an increase in the polarization resistance with an increase in the concentration of the
inhibitory composition, which corresponds to a decrease in the corrosion current in both media
under study. In this case, the capacitance of the electrical double layer also decreases, indicating
the adsorption of the components of the inhibitory composition on the steel electrode. This made
it possible to calculate a surface coverage with an inhibitor, to determine the type of adsorption
isotherm, which turned out to be the Temkin isotherm, and to calculate the adsorption free
energy. The inhibitory composition reduces the penetration of hydrogen into the metal, starting
from a concentration of 100 mg/L.
Received: June 8, 2023. Published: June 26, 2023 doi: 10.17675/2305-6894-2023-12-3-1

Keywords: carbon steel, corrosion, protection, inhibitory composition, model stratum water,
hydrogen sulfide, polarization, impedance spectroscopy.
 Int. J. Corros. Scale Inhib., 2023, 12, no. 3, 811–824 812

Introduction
One of the main methods for protecting metal equipment of oil and gas fields is the use of
inhibitors. Due to the widespread occurrence of hydrogen sulfide corrosion, its inhibition has
been the subject of numerous studies that continue to this day [1–4]. In [5], data on the
effectiveness of corrosion inhibitors used in the oil and gas industry are summarized. Many
inhibitor developers create mixtures of various compounds or use condensation products of
various substances dissolved in specially selected mixed solvents. Similar products are created
at LLC INCORGAZ and AMDOR, St. Petersburg [6, 7] and exhibit universal properties,
reducing not only hydrogen sulfide, but also carbon dioxide corrosion of steel, its
hydrogenation, loss of mechanical properties, and also have a bactericidal effect on SRB.
Inhibitory compositions of the EM series, which are mixtures of imidazolines and amides,
were studied [8]. They showed high protective efficiency in hydrogen sulfide, carbonic acid
environments and environments containing both H2S and CO2, sharply reduced the
hydrogenation of steel and showed bactericidal properties with respect to SRB, i.e., fully
corresponded to universal corrosion inhibitors [9]. Universal properties are also inherent in
the inhibitory composition AMDOR IC-3, which is a condensation product of tallic acids and
polyethylenepolyamines in an alcohol-hydrocarbon solvent, the protective effect of which
exceeds 90% at a concentration of 100 mg/L, and the diffusion of hydrogen into the metal
decreases 4–9 times per depending on the content of hydrogen sulfide [10]. Typically,
inhibitory properties are exhibited by substances whose molecules contain unsaturated bonds,
aromatic rings and heteroatoms, such as O, N, S, etc. The techniques such as the density
functional theory (DFT), molecular dynamics (MD), and Monte Carlo (MC) simulations are
often applied to obtain quantitative parameters of the corrosion inhibition performance [11].
The purpose of this work is to study the protective ability of the composition, which is
the product of the interaction of fatty tallow polyamines with ethylene oxides in an alcohol
solvent, with respect to corrosion of carbon steel in model stratum waters saturated with H 2S.

Experimental
The studies were carried out at room temperature on electrodes made of carbon steel St3
with the composition, wt. %: С – 0.2; Mn – 0.5; Si – 0.15; P – 0.04; S – 0.05; Cr – 0.30;
Ni – 0.20; Cu – 0.20; Fe – 98.36. Model stratum waters M1 and NACE [12] saturated with
hydrogen sulfide (400 mg/L) were used as working solutions. H2S was obtained directly in
the working solution by introducing the calculated amounts of Na2S and HCl corresponding
to the reaction equation:
Na 2S + 2HCl = H2S + 2NaCl
The concentration of hydrogen sulfide was controlled iodometrically.
The technique of potentiodynamic polarization measurements did not differ from that
given in [12]. The protective effect of the inhibitor was calculated from the data of
polarization measurements using Formula 1:
 Int. J. Corros. Scale Inhib., 2023, 12, no. 3, 811–824 813

Z % = 100  (i 0 −iinh ) i 0 (1)

where i0 and iinh are the corrosion current densities in the absence and presence of an inhibitor
in solution, respectively. The corrosion current density was calculated by extrapolating the
Tafel sections of the polarization curves to the corrosion potential. The potentials are
recalculated to the normal hydrogen scale. The concentration of the inhibitory composition
varied in the range of 25–200 mg/L.
The impedance spectra were measured in the frequency range (ω/2π)
10 kHz – 0.05 Hz with an alternating voltage amplitude of 10 mV after 15 min exposure of
the electrodes to the solution using an electrochemical measuring complex from Solartron
(Great Britain), consisting of an SI 1255 impedance analyzer and SI 1287 potentiostat. The
results of impedance measurements were processed in accordance with the equivalent circuit
shown in Figure 1, using the ZView 3.0 program, which allows calculations for any
equivalent circuits with up to 20 elements. The criterion for evaluating circuits is the standard
deviation s; the equivalent circuit is considered satisfactory for s ≤ 5%.

Figure 1. Equivalent circuit that simulates the behavior of carbon steel at the corrosion
potential in the solutions under study saturated with hydrogen sulfide.

The study of hydrogen diffusion into the metal was carried out at room temperature
according to an electrochemical diffusion technique using a two-chamber cell, first proposed
by Devanathan [13], separated by a steel membrane 0.3 mm thick, with an area of 3.63 cm2.
A working solution was introduced into the polarization part of the cell, and a precisely fixed
volume of a titrated 0.01 N solution of potassium permanganate (40 mL) was introduced into
the diffusion part (method developed by N.V. Kardash and V.V. Batrakov [14]). The
duration of the experiments was 2 h at the corrosion potential. The amount of hydrogen
diffused through the membrane was recalculated in electrical units (iH). To quantify the
effect of inhibitors, the solid-phase diffusion coefficient γН was used:
γ H = i0,H iH (2)
where i0,H and iH are, respectively, the fluxes of hydrogen diffusion in uninhibited and
inhibited solutions (γН > 1 corresponds to inhibition of the process, γН < 1 corresponds to
stimulation of the process, γН = 0 – no effect).
The technique for analyzing corrosion products by X-ray diffraction was described
earlier in [3].
 Int. J. Corros. Scale Inhib., 2023, 12, no. 3, 811–824 814

Results and Discussion

The potentiodynamic polarization curves measured in M1 medium containing 400 mg/L H2S
are shown in Figure 2. The Tafel sections on the cathodic curves are characterized by a slope
bc close to 0.12 V, while on the anodic ones, about 0.08 V (Table 1). The corrosion potential
shifts to the negative region with the introduction of an inhibitory composition and an
increase in its concentration. This indicates that it slows down the cathodic process at the
electrode. From Table 1 it follows that the protective efficacy of the inhibitory composition
is 60% at a concentration of 25 mg/L and increases with its growth, reaching 87% at
200 mg/L.

Figure 2. Potentiodynamic polarization curves measured on a steel electrode in M1 +

400 mg/L H2S solution in the absence (1) and in the presence of the inhibiting composition,
mg/L: 2 – 25, 3 – 50, 4 – 100, 5 – 200.

Table 1. Kinetic parameters of the St3 steel electrode in M1+400 mg/L H2S solution in the absence and in
the presence of the inhibitory composition and its protective efficiency.

cinh, mg/L –Еcorr, V bc, V ba, V icorr, A/m2 Z, %

Background 0.32 0.12 0.083 1.26 –

25 0.36 0.12 0.080 0.50 60
50 0.36 0.12 0.080 0.25 80
100 0.40 0.11 0.080 0.20 84
200 0.48 0.10 0.090 0.16 87
 Int. J. Corros. Scale Inhib., 2023, 12, no. 3, 811–824 815

Potentiodynamic polarization curves in the NACE + 400 mg/L H2S medium in the
absence and presence of the inhibitory composition are shown in Figure 3, and the
corresponding kinetic parameters of the steel electrode and the protective effectiveness of
the inhibitor are in Table 2. From Figure 3 it follows that the introduction of 25 mg/L
inhibitor into the NACE medium slows down both partial electrode reactions on the steel
electrode and results in a protective efficiency of 74%. A further increase in the
concentration of the inhibitory composition leads to a slowdown of the predominantly
cathodic process and an increase in the Z value, which is 94% at a concentration of
200 mg/L.

Figure 3. Potentiodynamic polarization curves measured on a steel electrode in NACE +

400 mg/L H2S solution in the absence (1) and in the presence of the inhibiting composition,
mg/L: 2 – 25, 3 – 50, 4 – 100, 5 – 200.

Table 2. Kinetic parameters of the St3 steel electrode in NACE + 400 mg/L H2S solution in the absence
and in the presence of the inhibitory composition and its protective efficiency.

cinh, mg/L –Еcorr, V bc, V ba, V icorr, A/m2 Z%

Background 0.33 0.129 0.095 1.33 –

25 0.32 0.170 0.096 0.35 74
50 0.55 0.120 0.073 0.12 91
100 0.41 0.130 0.060 0.10 92
200 0.48 0.120 0.060 0.075 94
 Int. J. Corros. Scale Inhib., 2023, 12, no. 3, 811–824 816

The higher protective efficacy of the inhibitory composition in the NACE medium than
in M1 one is probably due to the more acidic environment in the first case, which promotes
a protonation of the inhibitor components.
The protective efficacy of the inhibitory composition is confirmed by impedance
measurements. Figure 4 shows the hodographs measured on a steel electrode in the M1
medium at the corrosion potential. They are arcs, the diameter of which increases with the
introduction of an inhibitor into the solution and an increase in its concentration. This
indicates an increase in the total resistance in the system, which contributes to a decrease in
the metal corrosion rate.
The analysis of hodographs was carried out using the equivalent circuit shown in
Figure 1. The fitting curves obtained on the basis of this circuit agree satisfactorily with the
experimental points on the Nyquist diagram, which indicates the correct choice of the
equivalent circuit. The numerical values of the elements of the equivalent circuit are given
in Table 3.

Figure 4. Nyquist diagrams of steel electrode in M1+400 mg/L H2S solution at Ecorr in the
absence (1) and in the presence of the inhibitory composition, mg/L: 2 – 25; 3 – 50; 4 – 100;
5 – 200. The dots correspond to the experimental data, whereas the solid lines correspond to
the impedance spectra fitted using the equivalent circuit.

The Nyquist diagrams measured in the NACE + H2S environment are shown in Figure 5.
As in M1 + H2S solutions, the diameter of the hodographs increases with the introduction of
an inhibitory composition and an increase in its concentration, indicating a slowdown in the
corrosion process. The numerical values of the elements of the equivalent circuit are
presented in Table 4.
 Int. J. Corros. Scale Inhib., 2023, 12, no. 3, 811–824 817

Table 3. Numerical values of elements of the equivalent circuit at Ecorr of the steel electrode in
M1 + 400 mg/L H2S solution without and with tested concentrations of the inhibitory composition.

Concentration of inhibitory composition, mg/L

Element
Background 25 50 100 200

Rs, Ω·cm2 12.4 31.3 28.2 23.2 6.9

R2, Ω·cm2 4.3 9.3 14.2 40.4 65.6
RD, Ω∙cm2 1040 1714 1491 2390 2979
τ, s 39.4 57.1 14.3 6.4 2.9
p 0.4 0.4 0.5 0.6 0.7
R1, Ω·cm2 111 471 428 491 627
Ca, μF/cm2 6.4 75.5 85.9 4.8 3.6
Ra, Ω·cm2 37.9 115.2 66.1 398.7 36.2
Cdl, μF/cm2 28.1 23.1 15.8 9.1 4.1
s 0.015 0.011 0.014 0.003 0.117

Figure 5. Nyquist diagrams of steel electrode in NACE + 400 mg/L H2S solution at Ecorr in the
absence (1) and in the presence of the inhibitory composition, mg/L: 2 – 25; 3 – 50; 4 – 100;
5 – 200. The dots correspond to the experimental data, whereas the solid lines correspond to
the impedance spectra fitted using the equivalent circuit.
 Int. J. Corros. Scale Inhib., 2023, 12, no. 3, 811–824 818

Table 4. Numerical values of elements of the equivalent circuit at Ecorr of the steel electrode in NACE +
400 mg/L H2S solution without and with tested concentrations of the inhibitory composition.

Concentration of inhibitory composition, mg/L

Element
Background 25 50 100 200

Rs, Ω·cm2 10.3 38.3 31.0 40.3 30.3

R2, Ω·cm2 6.7 33.8 45.7 40.1 37.0
RD, Ω∙cm2 1818 3266 3030 3207 2906
τ, s 13.3 15.2 6.9 16.3 15.0
p 0.5 0.5 0.6 0.6 0.6
R1, Ω∙cm2 84.1 327.8 329.9 428.0 425.6
Ca, μF/cm2 22.2 44.5 8.1 3.5 3.9
Ra, Ω∙cm2 7.5 223.9 349.5 345.4 115.3
Cdl, μF/cm2 38.7 16.5 12.2 8.4 4.7
s 0.023 0.003 0.050 0.001 0.008

Both in the M1+ H2S medium and in the NACE + H2S solution, the charge transfer
resistance in the cathodic reaction R2 is much lower than the mass transfer resistance RD.
This indicates the reduction of the depolarizer with a predominance of diffusion restrictions.
The parameter p, corresponding to the generalized finite diffusion impedance
Z D = RD th( jωτ) p ( jωτ) p , where 0<p<1, remains within 0.4–0.7 in M1, and 0.5–0.6 in
NACE media in the range of the concentrations under study of the inhibitory composition.
The p value within the limits indicated is observed in the case of non-preservation of the
number of diffusing particles in the diffusion layer or when some particles are retained for a
relatively long time at certain points of the diffusion layer [15].
Let us estimate the polarization resistance in M1+ H 2S and NACE + H2S media. For
the equivalent circuit used, the polarization resistance Rp is calculated by the formula:
Rp =  R1  ( R2 + RD ) ( R1 + R2 + RD ) (3)

Table 5 shows the values of the polarization resistance in the solutions studied, from
which it can be seen that Rp increases with the introduction of an inhibitory composition into
the initial solution and an increase in its concentration. This indicates a decrease in the steel
corrosion rate, which is consistent with the data of polarization measurements.
 Int. J. Corros. Scale Inhib., 2023, 12, no. 3, 811–824 819

Table 5. Effect of inhibitor concentration on the value of polarization resistance Rp in the M1 + 400 mg/L
H2S and NACE + 400 mg/L H2S solutions.

cinh, mg/L Rp in M1 + 400 mg/L H2S medium Rp in NACE + 400 mg/L H2S medium
0 100 80
25 370 298
50 333 298
100 408 378
200 520 372

It follows from Tables 3 and 4 that with the introduction of the inhibitory composition
into the solution and an increase in its concentration, the capacitance of the electrical double
layer decreases due to the adsorption of the components of the inhibitory composition on the
electrode surface. This makes it possible to calculate the steel surface coverage Θ with the
components of the inhibiting composition in the solutions studied according to the formula
[16]:
 = (C0 − C ) (C0 − C1 ) (4)

where C0, C and C1 are the capacitances of the electric double layer in the solution
without addition of inhibitory composition, with that and with the maximum coverage of the
electrode surface with the adsorbed particles, respectively. The value of C1 is calculated
graphically on the basis of the rectilinear dependence Cdl = Cdl (1 cinh ) and is equal to the
segment cut off on the y-axis [17]. In NACE + H2S solutions C1 = 4.0 μF/cm2, in M1 + H2S
environment C1 = 2.8 μF/cm2. The calculated values of Θ are shown in Table 6.
Table 6. Influence of concentration of the inhibitory composition on the surface coverage of steel in NACE
and M1 media containing 400 mg/L H2S.

cinh, mg/L 25 50 100 200

Θ in NACE medium 0.64 0.76 0.87 0.98
Θ in М1 medium 0.20 0.49 0.75 0.95

The relationship between the surface coverage Θ and the concentration of the inhibitory
composition was studied in accordance with the known adsorption isotherms of Temkin
Bc = exp( f Θ), Frumkin Bc = [Θ/(1–Θ)]exp( –2aΘ)], and Langmuir c/Θ = 1/B + c, where f is
the energy inhomogeneity parameter of the metal surface, B is the adsorption equilibrium
constant, a is the attraction constant characterizing the interaction between adsorbed
particles, and c is the inhibitor concentration. Linear plots of Θ vs. logcinh, ln[cinh(1–Θ)/Θ]
 Int. J. Corros. Scale Inhib., 2023, 12, no. 3, 811–824 820

vs. Θ and cinh/Θ vs. cinh correspond to the Temkin, Frumkin and Langmuir isotherms,
respectively (Figure 6).

Figure 6. Adsorption isotherms for St3 steel in M1 + 400 mg/L H2S (1) and NACE+400 mg/L
H2S (2) solutions.

As follows from Figure 6, the best correspondence to the linear dependence is observed
for the Temkin isotherm both in M1 + H2S medium and in NACE + H2S environment.
Having determined the values of f and B, it is possible to calculate the value of the free
energy of adsorption ( −Gads
0
) using the formula:

Gads
0
(
= − RT  ln B 106 ) (5),

where 106 is the water concentration in mg/L. The value of f was obtained by substituting
the found values of Θ and the corresponding concentrations cinh into the Temkin equation
and successive subtraction from the subsequent equation of the previous one, averaging the
resulting value. Substituting it into the Temkin equation allows us to calculate the value of
B (Table 7).
 Int. J. Corros. Scale Inhib., 2023, 12, no. 3, 811–824 821

Table 7. Parameters of the adsorption isotherm of the inhibitory composition on the surface of carbon steel
in the media studied. T = 298 K.

Medium NACE + 400 mg/L H2S M1 + 400 mg/L H2S

f 6.1 2.8
B, L/mg 2.0 0.075
−Gads
0
, kJ/mol 35.9 27.8

The obtained values of the free energy of adsorption indicate the physical nature of the
adsorption of the components of the inhibitory mixture with a certain amount of
chemisorption.
The influence of an inhibitory composition on the penetration of hydrogen, formed
during the electrochemical corrosion of steel, into the depths of the metal was studied using
an electrochemical diffusion technique. The composition under study causes inhibition of
the diffusion of hydrogen into the metal in the NACE medium + H 2S, only starting from a
concentration of 100 mg/L (Table 8).
Table 8. Hydrogen diffusion current (iH) through a steel membrane in NACE + 400 mg/L H2S and its
inhibition coefficient γH as a function of inhibitory composition concentration.

cinh, mg/L iH, A/m2 γH

0 0.31 –
25 0.38 0.81
50 0.34 0.89
100 0.26 1.20
200 0.18 1.75

Corrosion products begin to form on steel immediately after contact with an H2S-
containing aqueous environment. The composition and stability of corrosion products affects
both corrosion and the penetration of hydrogen into steel [4, 18, 19].
The results of our X-ray diffraction tests showed that maсkinawite (FeS tetragonal) is
formed as the main corrosion product on steel in an aqueous medium, and in the presence of
acetic acid (CH3COOH) in the model water, another form of iron sulfide (FeS cubic) is
formed in addition to it. CH3COOH, in addition to increasing the acidity of the environment
and slowing down the formation of deposits, also changes the composition and heterogeneity
of deposits, reducing the protective properties of the sulfide film in aggressive acidic H 2S
environments. Due to the different crystal structure of two forms of FeS (tetragonal and
cubic), their joint formation in the presence of CH3COOH will induce the appearance of a
less dense and uniform film of corrosion products, unable to prevent the penetration of
aggressive ions to the steel surface. In addition to complicating the corrosion situation, FeS
 Int. J. Corros. Scale Inhib., 2023, 12, no. 3, 811–824 822

formed can also adversely affect the formation of an inhibitor film on the steel surface [20–
22]. Competitive adsorption between iron sulfide and corrosion inhibitor on a steel surface
can undermine the integrity of the inhibitor film, causing increased localized corrosion in
H2S environments [22]. To form a uniform layer on the steel, a higher concentration of
corrosion inhibitor and a higher rate of its adsorption on the metal surface (compared to
reactive FeS) may be required.
A natural continuation of the study is a similar plan using model stratum waters
containing both H2S and CH3COOH.
Conclusion
1. The protective effectiveness of the inhibitory composition, which is a product of the
interaction of fatty tallow polyamines with ethylene oxides in an alcohol solvent, in
relation to the corrosion of St3 steel in model stratum waters of oil and gas fields saturated
with hydrogen sulfide (400 mg/l), was studied by electrochemical methods.
2. According to the data of potentiodynamic polarization, the inhibiting composition slows
down mainly the cathodic process, causing a decrease in the corrosion current with a
protective effect that increases with its concentration and reaches 87 and 94% at 200 mg/L
in M1 and NACE media, respectively.
3. Impedance studies indicate an increase in polarization resistance with increasing
concentration of the inhibitory composition, confirming a corresponding decrease in
corrosion current. The recorded decrease in the capacitance of the electrical double layer
made it possible to calculate the electrode surface coverage with adsorbed components of
the inhibitory composition, to determine the adsorption isotherm, and to calculate the
adsorption free energy.
4. It has been shown that the inhibiting composition reduces the penetration of hydrogen into
the metal in NACE + H2S media, starting from a concentration of 100 mg/L.
Acknowledgment
The results were obtained using the equipment of the Center for Collective Use of Scientific
Equipment of TSU named after G.R. Derzhavin. This work was supported by the Ministry
of Science and Higher Education of the Russian Federation in the frame work of agreement
No. 075-15-2021-709 (unique project identifier RF-2296.61321X0037).
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