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LABORATORY STUDIES ON THE EFFECTS OF HYDROGEN
EXPOSURE ON POROSITY, PERMEABILITY, AND CHEMICAL
COMPOSITION OF TERRIGENOUS RESERVOIR ROCKS: A CASE
STUDY OF THE BOBRIKOVSKII FORMATIONS IN THE NORTHEAST
VOLGA-URAL OIL AND GAS PROVINCE
Elmuradov T.F.
Mamirov J.X.
Tashkent State Technical University named after Islam Karimov
https://doi.org/10.5281/zenodo.14287788
Abstract:
This article outlines the methodology for conducting laboratory
investigations into the effects of hydrogen on reservoir rocks. It details the
stages of sample analysis and the instruments employed during the
experiments. A comparative evaluation of the porosity and permeability of core
samples was undertaken, revealing a 4.6% decrease in porosity and a 7.9%
reduction in permeability following hydrogen exposure. Correlation analysis
indicated a typical shift in the relationship between these characteristics: post-
exposure, the variability of values increased while the correlation coefficient
decreased, suggesting alterations in the void structure. The findings suggest that
the observed reductions in porosity and permeability are attributed to slight
compaction due to effective stresses. Chemical analyses indicated no significant
changes in the composition of primary oxides before and
Keywords:
hydrogen; subsurface gas storage; reservoir rock; properties
of porosity and permeability; chemical makeup of rocks; fundamental oxides.
Introduction.
Recently, there has been a growing focus on eco-friendly
production technologies and the reduction of carbon dioxide emissions,
including the exploration of alternative energy sources to replace hydrocarbons.
In publication [1], the authors highlight the importance of addressing global
warming and discuss technologies for capturing and disposing of carbon dioxide.
They emphasize that Russia should adopt these technologies through
government programs, drawing on international experiences.
Hydrogen is
anticipated to serve as one of the alternative fuels, raising challenges related to
its production and transportation. Articles [2-4] outline various production
methods for hydrogen, each with differing levels of energy efficiency and
environmental impact. The authors advocate for technologies that do not
produce carbon dioxide emissions. Additionally, publications [5-7] indicate that
transporting hydrogen necessitates densification (liquefaction) and enhanced
safety for tanks and transport systems.
A critical consideration in hydrogen
energy is the selection of storage facilities. Scientific articles [8-10] indicate that
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salt caverns may be suitable for storing hydrogen-methane mixtures, but they
have both advantages and disadvantages. While salt caverns offer excellent
sealing properties, they require significant labor to create, incur high costs, and
have limited storage capacity due to structural collapse under external
pressures.
Some researchers propose utilizing existing underground gas storage
facilities (UGS) traditionally used for natural gas [11, 12]. For larger volumes,
depleted gas fields, aquifers, or currently operational methane storage facilities
are recommended.
A significant challenge in hydrogen storage is the
embrittlement of steel well strings and downhole equipment. Articles [13-15]
provide evidence that exposure to hydrogen can lead to physicochemical
changes in commonly used steel grades, resulting in cracking and deterioration
of mechanical properties. Such effects can lead to unexpected emergencies in
wells and equipment.
The metabolic activity of hydrogen-consuming bacteria
can also pose issues. Experts [16-18] have noted that certain bacterial species in
reservoirs can convert hydrogen into hydrogen sulfide, an aggressive gas that
can damage well structures and equipment.
When hydrogen is stored in reservoir beds, it can chemically react with
the minerals in the rock matrix and the cap rock above. Authors of articles [19-
21] present data showing that hydrogen can interact with pyrite and aluminum-
containing minerals, as well as with dissolved carbon dioxide and sulfates,
leading to the formation of methane and hydrogen sulfide. These reactions can
alter the porosity and permeability of the formation. Publications [22-24]
indicate that hydrogen can cause a twofold change in the porosity of core
samples, with these effects being dependent on the lithological characteristics of
the rocks. Thus, it is recommended to store gas primarily in terrigenous
reservoirs free of clay and carbonate impurities. Similar to traditional
underground gas storage for methane, storing hydrogen can create a complex
geodynamic situation at the operational sites. As shown in articles [25-27],
fluctuations in formation pressures during gas injection and withdrawal can
cause surface deformations. Therefore, it is essential to establish geodynamic
monitoring systems in these UGS. An analysis of the literature reveals that the
effects of hydrogen on the porosity and permeability of reservoir rocks, as well
as on the chemical composition of the rock matrix, have not been sufficiently
studied. This highlights the importance of examining the impact of hydrogen on
reservoir properties and the chemical changes in the rocks of the investigated
formation. The study focuses on the terrigenous deposits of the Bobrikovskii
horizon in the Volga-Ural oil and gas province, where gas is stored in the
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Karashurskoe UGS in the Republic of Udmurtia [28-30]. A methodology was
developed for analyzing core samples, and a unit was created for the long-term
exposure of samples to hydrogen. The results of lithological and petrographic
studies of thin sections of the core samples are presented, along with a
comparative analysis of the laboratory results concerning the porosity,
permeability, and chemical composition of the rock matrix.
Methodology.
The influence of hydrogen injection on the natural
properties of reservoirs was studied using the Bobrikovskii terrigenous
formations as a case study—a geological div designated for underground gas
storage in the Volga-Ural oil and gas province. Due to the inability to use core
samples from the At the Karashurskoe UGS, core samples were collected from a
similar Bobrikovskii formation at one of the oil fields in the northeastern part of
the Volga-Ural oil and gas province for laboratory experiments (Fig. 1). The core
was extracted from sections with the highest porosity and permeability,
specifically at a depth closest to the production zone in the Karashurskoe UGS,
ranging from 1,488.4 to 1,489.8 meters. A total of twenty-four core columns
were drilled from the original core material (Fig. 1), with half having standard
dimensions (3 cm in length and diameter) and the other half featuring non-
standard dimensions (6 cm in length and 3 cm in diameter). The non-standard
samples were used to evaluate the stress-strain properties of the rocks through
static testing before and after hydrogen exposure. Any samples displaying
visible cracks were excluded from further analysis, resulting in a final total of
twenty samples. After extraction, the samples underwent standard preparation,
which involved soaking in an alcohol-benzene mixture for 20 days using a
Soxhlet apparatus followed by
drying. Figure 1 illustrates the
prepared core samples, which
were categorized into five groups
of four samples each (Table 1).
Each
group
contained
two
standard samples and two “long” samples. The intention is to compare the
results of determining reservoir properties (porosity and permeability) as well
as stress-strain properties (elastic modulus, Poisson’s ratio, tensile and
compressive strength) before and after hydrogen exposure for both the
standard and “long” samples from each group.
Fig.1. Source core material and samples after drilling out
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Table 1
Geometric characteristics of core samples and their porosity
and permeability determined before and after exposure to
hydrogen
Group
numbe
r
Samp
le
numb
er
Lengt
h
h
, cm
Diamet
er
d
, cm
Before
exposure
to
hydrogen
After
exposure
to
hydrogen
Absolute
change
Relative
change
Kp
, %
Kper
,
mD
Kp
, %
Kper
,
mD
Kp
, %
Kper
,
mD
Kp
,
%
Kper
,
%
1
1
6.03
3.00
22.4 720
1
19
5.89
3.00
23.1 848
21.3 757
–1.8
–91
–7.79 –10.73
1
11/
2
3.03
3.02
23.3 759
1
2/1
3.01
3.00
22.4 739
22.3 692
–0.1
–47
–0.45 –6.36
2
4
5.89
2.99
22.4 664
2
12
5.84
3.00
22.2 706
21.5 646
–0.7
–60
–3.15 –8.50
2
2/2
2.90
3.00
22.9 686
2
14
2.96
2.99
22.9 686
22.5 644
–0.4
–42
–1.75 –6.12
3
6
6.03
3.01
21.3 604
3
15
6.01
2.99
21.4 518
20.7 495
–0.7
–23
–3.27 –4.44
3
13
2.98
2.99
23.0 643
3
5/1
2.87
2.99
22.8 644
21.1 603
–1.7
–41
–7.46 –6.37
4
7
5.97
2.99
22.1 612
4
3
6.02
3.00
22.6 634
22.0 618
–0.6
–16
–2.65 –2.52
4
11/
1
3.00
3.02
22.7 717
4
8/1
2.98
3.00
22.4 669
19.4 603
–3.0
–66
–
13.39
–9.87
5
16
5.9
2.99
22.3 496
5
21
5.89
3.02
21.6 463
21.0 448
–0.6
–15
–2.78 –3.24
5
2/5
2.93
3.00
22.5 611
5
8/2
2.91
3.01
22.3 655
21.7 625
–0.6
–30
–2.69 –4.58
Average value
22.4 656
21.3 612
–1.07
–44.6
–4.74 –6.46
Table 2 outlines the comprehensive research program for the sample studies.
The research consists of the following stages:
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Stage 1: Following the standard preparation of the samples, their porosity and
gas permeability were measured under conditions similar to atmospheric
pressure: open porosity (Kp) and absolute permeability (Kper). The assessment
of reservoir properties was conducted in accordance with GOST 26450.2-85
using a PIK-PP unit (AO Geologiya). To ensure accurate measurements, the
samples were subjected to a minimum overburden pressure of 2.5 MPa, which
prevented gas from flowing around the sides of the samples. This phase of the
study aimed to identify variations in the reservoir properties of the core samples
and assess the representativeness of the sample selection.
Table 2
Key stages of the research program, along with the equipment used and the
parameters measured for each group of four samples.
Sta
ge
Content of
research
stage
Un
it
use
d
Deter
mine
d
para
meter
s
1
Samples are extracted and dried, open
porosity and absolute gas permeability are
determined at effective stresses close to
atmospheric conditions (overburden pressure
2.5 MPa)
PIK
-PP
K
p
e
r
,
K
p
2
Lithological and petrophysical studies of thin
sections of core samples
Polarisi
ng
microsc
ope
Leica
DM
2700P
Lithol
ogical
and
petroph
ysical
prope
rties
3
For three crushed samples, the chemical
analysis of rock is performed, the com-
Spect
rosca
Mass
fracti
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position of the main rock-forming oxides:
Fe2O3, MnO, TiO2, Al2O3, SiO2, CaO, MgO,
Na2O, K2O, P2O5, Stot
n
MAK
S-GV
ons
of
oxide
s
4
From each group, one “long” sample, one
standard sample and part of the crushed core
are placed in a cylinder, into which hydrogen is
then injected. Sam- ples are kept in the
cylinder for 7 days
Cylinder
for
injecting
hydrogen
and
keeping
samples
5
For samples removed from the cylinder, the
porosity and gas permeability are determined
at effective stresses close to atmospheric
conditions (overburden pressure 2.5 MPa)
PIK
-PP
K
p
e
r
,
K
p
6
For samples extracted from the cylinder,
chemical analysis of the rock is per-
formed, composition of the main rock-
forming oxides: Fe2O3, MnO, TiO2, Al2O3,
SiO2, CaO, MgO, Na2O, K2O, P2O5, Stot
Spec
trosc
an
MAK
S-GV
Mass
fracti
ons
of
oxide
s
Stage 2: Identification of the minerals present in the rock being analyzed. Stage
3: Prior to hydrogen exposure, studies were carried out, and some samples were
crushed and thoroughly mixed for further analysis. Three crushed core samples
were examined, assuming their compositions would be similar due to the
crushing and mixing process. Chemical analysis of the primary oxides was
conducted without hydrogen influence, following GOST 5382-2019, specifically
clause 7 (weight loss on ignition – LOI) and clause 23 (X-ray spectral method for
element determination) using the MAKS-GV X-ray fluorescence spectrometer.
Stage 4: The samples underwent prolonged exposure to hydrogen using a
system that included a hydrogen cylinder, a pressure regulator with pressure
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sensors, and a sealed chamber (Fig. 2). Hydrogen was supplied from a
compressed gas cylinder with a volume of 40 dm³ and a total gas volume of 6.3
m³ (Fig. 2). The hydrogen characteristics in the cylinder included:
- Hydrogen volume fraction (dry gas) of at least 99.99%;
- Total oxygen and nitrogen volume fraction not exceeding 0.01%;
- Water vapor mass concentration at 20 °C and 101.3 kPa not more than 0.2
g/m³;
- Cylinder pressure at 20 °C of 14.7±0.5 MPa.
Given the high pressure of the hydrogen, a regulator was attached to the
cylinder, equipped with two sensors to monitor the gas pressure at the inlet and
outlet. The reduced gas pressure was approximately 0.6-0.7 MPa. For the
interaction with hydrogen, core samples were placed in a specially designed
cylinder (Fig. 2) with openings for gas supply and removal. Each study group
included one standard sample, one “long” sample, and a sample of crushed rock
moistened with distilled water, contained in a sieve to prevent loss during gas
flow. The regulator and cylinder were connected after a specific volume of
hydrogen was introduced to displace the air. Following this, both valves were
closed, allowing the rock to be exposed to hydrogen for seven days, with the gas
being refreshed every 24 hours. In total, five groups of samples—comprising five
standart, five “long,” and five crushed rock samples—were exposed to hydrogen
to assess changes in chemical composition. Stages 5 and 6: After hydrogen
exposure, porosity and gas permeability were measured again, along with a
chemical analysis of the primary oxides.
Fig. 2. Diagram of the unit for containing core samples exposed to hydrogen:
1 – Hydrogen cylinder;
2 – Valves;
3
5
2
Н
2
6
7
8
1
2
Н
2
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3 – Pressure sensors;
4 – Pressure regulator with valve;
5 – Cylinder housing core samples;
6 – Sieve with crushed rock;
7 – Standard core sample (diameter: 3 cm, length: 3 cm);
8 – “Long” core sample (diameter: 3 cm, length: 6 cm).
Results:
The results for
open porosity and absolute
permeability
of
the
samples (Stage 1), along
with
their
geometric
characteristics,
are
summarized in Table 1.
The
porosity
of
the
samples
ranged
from
21.3% to 23.3%, while the
permeability
varied
between 463 mD and 848
mD, with average values of
22.4% and 653.7 mD, respectively.
Fig.3. Dependence of permeability on porosity of core samples
before (1) and after (2) exposure to hydrogen
The correlation between absolute gas permeability and open porosity of the
core samples is depicted in Fig. 3 (blue circles). This graph illustrates a strong
relationship between these two characteristics, with a correlation coefficient of
0.68, indicating the homogeneity of the samples selected for analysis. Figure 4
presents images of some thin sections of the core samples studied (Stage 2). The
analysis of these thin sections revealed the following key findings:- The samples
are primarily composed of fine-grained silty sandstones with a quartz and
feldspathic-quartz mineral composition. The rock structure is fine-grained silty-
psammitic, with grain sizes ranging from 0.05 mm to 0.2 mm, and 10-30% of the
grains are in the silty fraction measuring 0.1-0.16 mm. Grains are irregular,
subisometric, elongated, and semi-rounded, with a microlayered texture
resulting from the orientation of some elongated fragments. The rock primarily
consists of quartz grains (82-95%), feldspar grains (up to 5%), and mica (up to
1
2
y
= 152.4e
0.064
х
R
= 0.38
y
= 12.67e
0.175
х
R
= 0.68
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8%). The quartz grains exhibit an irregular elongated shape and may show signs
of regeneration (0.003-0.015 mm). Some grains have dissolved around the
edges, leading to uneven contours. Feldspar is mainly represented by
plagioclase, which shows weak pelitization and partial dissolution. Mica includes
muscovite blades and some chlorite flakes. The rock primarily features
indentation cementation, which is a cement-free contact connection between
quartz grains and fragments, characterized by a conformal structure. Accessory
minerals include pyroxene grains measuring 0.08-0.18 mm. Authigenic minerals
consist of isolated hydromica flakes smaller than 0.05 mm and calcite crystals
measuring 0.25-0.3 mm (accounting for less than 1%). Post-sedimentation
transformations have led to indentation structures and the formation of
conformal structures due to quartz regeneration and the compaction of
fragments.
The void space within the rock is approximately 3-5% and is unevenly
distributed, consisting of irregularly shaped, intergranular isolated pores of
presumed secondary origin, ranging from 0.06 to 0.25 mm in size. Articles [21,
31, 32] indicate that quartz particles, under the mining and geological
conditions of the UGS, show
minimal
interaction
with
hydrogen. The results of chemical
analysis of the rock (stage 3) are
presented in Table 3 and Fig.5. As
can be seen from these data, the
samples
have
the
chemical
composition characteristic of a
terrigenous reservoir. Figure 5
shows the averaged composition
of oxides for three samples of
crushed
rock,
while
the
composition with and without silicon oxide is plotted separately, since its
content is much higher than that of other oxides. The chemical composition of
the investigated samples is dominated by silicon oxide, the amount of which is
on average 96.64 %, the amount of other oxides, together with weight
loss on ignition, is 2.01 % (Fig.5,
a
).
Fig.4. Photos of the investigated thin sections of core samples N 1
(
a
,
b
) and N 4 (
c
,
d
):
a
,
c
– without analyzer;
b
,
d
– with analyzer
Table 3
d
200 µm
200 µm
200 µm
200 µm
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Results of the chemical composition analysis of rocks before and after
hydrogen exposure.
Samp
le
numb
er
Content in
rock, %
Mass fraction of a chemical element
in terms of oxide
LOI
Fe –
Fe2O3
tot
Mn –
MnO
(II)
Ti
–
Ti
O2
Al
–
Al2
O3
Si –
SiO2
Ca
–
Ca
O
Mg
–
Mg
O
Na
–
Na
2O
K
–
K2
О
P
–
P2
O5
S
–
St
ot
Before exposure to
hydrogen
1
0.8
1
<
0.01
0.28 < 0.1 96.44
0.32
0.13 0.20
0.22
0.02 0.23
1.0
8
2
0.7
7
<
0.01
0.28 < 0.1 96.83
0.29
0.03 0.22
0.21
0.02 0.22
1.0
9
3
0.7
5
<
0.01
0.24 < 0.1 96.65
0.25
0.02 0.06
0.20
0.02 0.25
1.1
0
Avera
ge
value
0.7
8
0.27
96.64
0.29 0.0
6
0.16
0.21
0.02 0.23
1.0
9
After
exposure
to
hydrogen
1
0.9
8
0.01
0.28 < 0.1 95.01
0.46
0.11 0.14
0.25
0.02 0.29
2.5
8
2
0.7
2
<
0.01
0.24 < 0.1 95.73
0.25
0.16 0.16
0.14
0.02 0.21
1.1
8
3
0.7
5
0.01
0.23 < 0.1 97.62
0.31
0.10 0.11
0.14
0.02 0.18
1.2
6
4
0.8
2
<
0.01
0.25 < 0.1 95.64
0.24
<
0.1
0.22
0.21
0.02 0.32
1.2
3
5
0.7
2
<
0.01
0.21 < 0.1 97.11
0.28
<
0.1
0.25
0.26
0.02 0.44
1.1
3
Avera
ge
value
0.8
0
0.01
0.24
96.22
0.31 0.1
2
0.18
0.20
0.02 0.29
1.4
8
Absolu
te
chang
e
0.0
2
–
0.02
–0.42
0.02 0.0
6
0.01
–
0.01
0.00 0.06
0.3
9
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As shown in Fig. 5b, iron oxide ranks
second in abundance after silicon
oxide, with a composition of 0.78%.
The samples also contained the
following oxides in descending
order: calcium oxide (0.29%),
titanium oxide (0.27%), sulfur
oxides (0.23%), potassium oxide
(0.21%), sodium oxide (0.16%),
magnesium oxide (0.06%), and
phosphorus oxide (0.02%).
After prolonged exposure of the
samples to hydrogen (Stages 4 and
5), changes in reservoir properties
can be compared before and after
exposure (refer to Table 1, Fig. 3
with red dots, and Fig. 6). To
facilitate comparison, each graph in
Fig. 6 includes a dotted line representing equal values. By comparing the
experimental values to this line, one can easily determine whether a specific
characteristic has increased or decreased following hydrogen exposure. Points
below the line indicate a decrease in the rock property, while points above the
line indicate an increase. Additionally, Fig. 6 features a linear approximation
function starting from the origin. The coefficient for the variable x in this
function helps quantify the extent of the changes in each characteristic. Table 3
displays the results of the chemical composition analysis of the rock before and
after exposure to hydrogen (Stage 6). For easier data interpretation, Fig. 7
illustrates the composition of the main oxides in percentage and their absolute
changes.
Discussion of Results:
Comparing the porosity and permeability results
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of core samples before and after hydrogen exposure (see Fig. 5) indicates that
after exposure
Fig. 6. Comparison of porosity (a) and permeability (b) of core samples before
and after hydrogen exposure:1 – Line of equal values; 2 – Approximation line.
Exposure to gas resulted in a
decrease in porosity and permeability
by 4.6% and 7.9%, respectively. This
indicates that the samples became
more compacted after hydrogen
exposure. According to the authors,
this compaction occurred due to the
weakening of the rocks under
hydrogen's influence. Additionally,
when measuring the porosity and
permeability of the samples after this
exposure, an overburden pressure of
2.5 MPa caused further compaction,
even though the samples had already
experienced compressive loading
during the initial measurements
before hydrogen exposure. It is likely
that this exposure compromised the
strength of the intergranular contacts,
leading to a weakening of the rock
matrix. The correlation between changes in both porosity and permeability after
hydrogen exposure is understandable, as changes in the volume of void space
affect rock compressibility. This, in turn, results in variations in porosity and
permeability in response to changes in effective stress. In addition to the
correlation trends illustrated in Fig. 6, it was observed that the relationship
between permeability and porosity changed significantly after hydrogen
exposure (see Fig. 3): the correlation coefficient decreased, and the variability in
permeability values increased, indicating that permeability did not decline
significantly with reduced porosity.
To sum up, it is important to examine the results of the chemical analyses
of crushed rock samples before and after hydrogen exposure (Table 3, Fig. 7).
Figure 7 presents the average values of basic oxides for three samples prior to
hydrogen exposure and five samples afterward. The changes in chemical
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composition before and after exposure are minimal, with some values increasing
and others decreasing. The exception is silicon oxide, which remains at a
maximum concentration in the rock. Overall, these changes could be attributed
to variations in sample composition or measurement errors. Thus, the
comparison of chemical analysis results indicates that hydrogen's effect on the
chemical composition of core samples is minor. This suggests that the geological
formation studied (the Bobrikovskii horizon) could be suitable for storing a
hydrogen-methane mixture. However, this conclusion would require further
verification through more detailed studies involving a larger sample size and
longer hydrogen exposure (up to one month or more).
Conclusion:
This study examines the methodology and findings from
laboratory investigations into the effects of hydrogen exposure on the reservoir
properties and chemical composition of terrigenous reservoir rocks, focusing on
t
h
e
B
o
b
r
i
k
o
v
s
k
i
i
h
o
r
i
z
o
n
i
n
The authors developed an experimental unit and a specialized program
for analyzing core samples, allowing for the examination of reservoir
properties, density, dynamic characteristics, stress-strain behavior, and
chemical composition before and after hydrogen exposure. The
methodology was tested on terrigenous core samples from the
Bobrikovskii formation in a Volga-Ural oil field.
Lithological and petrophysical analyses revealed that the core samples
were predominantly composed of quartz grains, with minor amounts of
feldspar and muscovite.
The experiments assessed the reservoir properties of the core samples
before and after hydrogen exposure, showing a decrease in porosity
and permeability by 4.6% and 7.9%, respectively.
The authors attribute the reduction in porosity and permeability to the
weakening of rocks due to hydrogen exposure. Additionally, when
measuring these properties after exposure and applying an overburden
pressure of 2.5 MPa, further compaction occurred, despite prior
compressive loading during initial measurements. The hydrogen
exposure likely disrupted the strength of intergranular contacts,
contributing to rock weakening. It is important to note that these
reductions in porosity and permeability are not substantial enough to
significantly impact gas injection and removal, especially since
hydrogen is much more mobile than natural gas.
Comparing the chemical analysis results for basic oxides indicated that
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changes in the chemical composition of rocks before and after
hydrogen exposure were minimal, possibly due to sample composition
variations or measurement errors. These findings suggest that the
formation is chemically resistant to hydrogen, supported by the high
silicon oxide content (96.64%), which does not interact with hydrogen
under the studied conditions.
Overall, the analyses of porosity, permeability, and chemical composition
demonstrate that hydrogen's influence on the reservoir rock is negligible. The
Bobrikovskii horizon in the Volga-Ural oil and gas province appears suitable for
storing a hydrogen-methane mixture. However, further validation is needed
through more comprehensive studies involving a larger number of samples and
extended hydrogen exposure.
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