OTC 19277

Mechanical Properties of Natural Gas Hydrate Bearing Sediments Retrieved

from Eastern Nankai Trough
Akira Masui, Kuniyuki Miyazaki, Hironori Haneda, Yuji Ogata, and Kazuo Aoki, AIST

Copyright 2008, Offshore Technology Conference

This paper was prepared for presentation at the 2008 Offshore Technology Conference held in Houston, Texas, U.S.A., 5–8 May 2008.

This paper was selected for presentation by an OTC program committee following review of information contained in an abstract submitted by the author(s). Contents of the paper have not been
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Abstract
MH21 research consortium of Japan conducted off-shore drillings to survey gas hydrate in Tokai-oki and Kumano-nada areas
of Eastern Nankai Trough in early 2004 and recovered drill cores of gas hydrate bearing sediment successfully. Marine gas
hydrate was confirmed mainly in sandy drill cores retrieved from mud and sand alternation strata. Tri-axial compression test
on those core samples has been conducted to ascertain mechanical properties of natural hydrate bearing sediments for the first
time. The results from the tests show that with increase in pore saturation of gas hydrate, shear strength and elastic modulus
tend to arise, whereas no significant tendency was found in Poisson’s ratio in relation to hydrate saturation.

Introduction
Public attention has been drawn recently to gas hydrate or methane hydrate in common in Japan as potential energy resources
since gas hydrate was located offshore Japan. In general, clathlate compounds trapping gas molecules in the cage of water
molecules are called gas hydrate, which is stable at ceratin temperature and pressure in phase equilibrium. Gas hydrate exists
stably, therefore, in a permafrost region and/or under sea floor in deep-water along continental margins where the equilibrium
state can be met in natural. In the development of gas hydrate resources, conventional methods used for a current gas and oil
production are not necessarily applicable, because gas hydrates should be dissociated before an accumulation of methane from
a hydrate reservoir. Moreover, the endothermic reaction of gas hydrate in dissociation reducing temperature at surroundings
will cause regeneration of gas hydrate and restrain the extension of a gasification path, which will be pecurior to the gas
production from gas hydrate. Considering the unique characteristics of gas hydrate, pressure decrease and/or temperature
increase are needed to destabilize the equilibrium state of gas hydrates. Field-scale trial tests by MH21 research consortium of
Japan were conducted and more onshore field tests have been scheduled employing depressurization method1). At present,
dissociation by depressurization is a promising application to a future production compared with thermal stimulation and
inhibitors in addition. Meanwhile, dissociation of gas hydrate may reduce a mechanical strength of sediment strata, which will
cause wellbore instability directly affecting a safety and stable gas production from gas hydrates in case. Since test samples of
drill cores containing natural gas hydrate are quite limited in number, Toyoura sand containing methane hydrate which was
formed synthetically in a tri-axial compression test has been used so far to ascertain the mechanical properties of gas hydrate
bearing sediments2). MH21 research consortium conducted offshore drilling survey in Tokai-oki and Kumano-nada areas of
Eastern Nankai Trough region in early 2004 as shown in Fig.1, and confirmed marine natural gas hydrates in drill cores
recovered from mud and sand alternation strata. In this paper, experimental results from tri-axial compression tests on natural
gas hydrate core samples can be presented focusing on strength, elastic modulus and Poisson’s ratio in relation to pore
saturation of gas hydrate. Moreover, these results have been compared with previous test results obtained from tri-axial
compression tests on Toyoura sand containing synthetically formed gas hydrate.

Experimental Procedure

Drill Cores of Natural Gas Hydrate Bearing Sediments

Drill core samples of approx. 1000mm in length and 70mm in diameter which were extracted from natural gas hydrate bearing
sediments have been preserved in liquid nitrogen for the preliminary scrutiny at AIST Hokkaido centre. Clear images of cracks
and bubble holes along the side surface of the drill core samples, which were captured by X-ray CT scanner at the Hokkaido
centre can be shown in Fig.2. As shown in Fig.2, these drill core samples have been disturbed more or less by drilling
2 OTC 19277

performances along with depressurization and/or stress relaxation due to extraction from a deep seafloor. In order to remove a
disturbed part of drill cores containing natural gas hydrate, the side surface has been cut on a lathe spraying liquid nitrogen on
the surface of core samples. The size of drill core samples prepared for tri-axial tests is approx.100mm in length and 50mm in
diameter and the physical properties of those tested can be given in Table1.

Reconstituted Samples of Drill Cores

After a tri-axial compression test, the dried natural sediment of a core sample was mixed with water to arrange initial water
content and was packed into a mold to make a reconstituted sample of 100mm in length and 50mm in diameter. The
reconstitute sample was then reused to form methane hydrate synthetically in the same manner as Toyoura sand which was
used as mother material when forming synthetic methane hydrate.

Tri-axial Testing Apparatus

The tri-axial testing apparatus used for laboratory experiments has a load capacity of 200kN, and capabilities of 20MPa at the
maximum for confining pressure and back pressure. The testing apparatus is operated by a digital servo control system which
enables to computerize a total operation of the apparatus. Temperature around a test sample can be maintained through the tri-
axial test in the range of 243K to 293K with an accuracy of 0.5K circulating cell water from a cooling tank into a pressurized
vessel. Data acquisitions can be performed every second for load, lateral and vertical displacements, confining pressure, back
pressure, and temperature. The experimental set-up for a natural core sample can be shown in Fig.2. Two eddy current gap
sensors are assembled beside the sample for monitoring the distance between the side surface of the sample and each sensor to
detect lateral displacement in an opposite direction. A natural core sample is covered with a rubber membrane of 0.5mm in
thickness to isolate pore pressure from confining pressure so that a variety of pressure combinations can be arranged for a tri-
axial compression test suitable for different water depths in-situ. In the case of a reconstituted test sample, methane gas can be
injected at a pedestal end through the path which is used for the pore water path in Fig.3. Then, tri-axial compression test can
be carried out after the test sample containing synthetic methane hydrate is saturated by purging methane gas remained in pore.

Tri-axial Compression Test

Natural gas hydrate core sample preserved in liquid nitrogen is moved to a dry shipper to vaporize liquid nitrogen prior to
setting it onto a pedestal end-cap as shown in Fig.2. After a rubber membrane is set to cover the frozen core sample, cell water
is injected immediately into a tri-axial pressure vessel so that confining pressure can be applied to the test sample within a few
minutes. The confining pressure is increased up to 10MPa to minimize the dissociation of natural gas hydrate while
maintaining effective confining pressure at 1MPa by raising pore pressure together at 278K. Then, the natural core sample is
consolidated for an approximately 24 hours to restore the in-situ stress condition. Tri-axial compression test is conducted at the
strain rate of 0.1% per minute in a drained condition employing confining pressure at 10MPa and back pressure at 9MPa. Tri-
axial compressive strength can be determined from the result and the pore saturation of gas hydrate can be calculated by the
total volume of methane gas released during the dissociation which is performed by reducing back pressure at both ends of the
test sample.

Result and Discussion

Particle Size Distribution

Because mechanical properties of natural gas hydrate bearing sediments are attributed to the component particles of sediments,
the distribution of particle size was analyzed by JIS A1204 standard sieve test using screen openings of 4.5mm, 2.0mm,
0.85mm, 0.25mm, 0.125mm and 0.075mm. After a tri-axial compression test, each core sample was dried at 383K for 24hours
in the electric drier. The particle size distribution of fine component of which the size is smaller than 0.075mm in diameter
was analyzed by an electrical potential particle counter. The total distribution of particle size can be represented as cumulative
frequency which is plotted against particle size in Fig.4. In Fig.4, natural core samples are denoted by “a” to “d” and Toyoura
sand by “e”. Toyoura sand is known as standard sand in Japan and it has been used so far for our laboratory tests forming
methane hydrate synthetically. The frequency distribution curves in Fig.4 are characterized by parameters of effective size
D10, mean size D50 and uniformity coefficient Uc. Effective particle size D10 is defined as the size at which 10% of the total
content in weight passes the screen opening and 90 % remains. The size D10 and D50 are determined on the distribution
curves by readings on the particle size at 10% and 50% of cumulative frequency respectively. The uniform coefficient Uc is
given by dividing D60 by D10 and it represents the degree of uniform distribution. These parameters are given in Table2.
Since the uniformity coefficient Uc of Toyoura sand is smaller than that of natural core samples, particle component of
Toyoura sand is distributed in the narrowest range showing the steep curve of cumulative frequency against particle size. In
other words, natural hydrate core samples contain fine particles with a variety of size range in comparison to Toyoura sand. As
shown in Fig.4, the natural hydrate core samples are classified as sandy sediment similar to Toyoura sand.
OTC 19277 3

Stress and Strain Relationship of Natural Gas Hydrate Core Samples

Stress and strain relationships of natural core samples can be shown in Fig.5. Sample “c” shows strain softening which is more
apparent than other samples in Fig.5. This is due to the highest hydrate saturation Sh of sample “c” among all in Table3. In the
previous test results2) from Toyoura sand containing synthetic methane hydrate, it has been confirmed that increase in hydrate
saturation tends to stimulate strain softening. Volumetric strain of sample “c” is the highest and that of sample “b” is the
lowest in the test range of axial strain in Fig.5. The initial porosities of specimen “b” and “c” are 50.8% and 44.2%
respectively as listed in Table1. Because composition particles enable to move towards pore space, porosity and particle size
are attributed to volumetric change in specimen resulting in weak dilatancy behavior. Therefore, the change in volumetric
strain against axial strain is affected by the initial porosity of natural core samples.

Tri-axial Compressive Strength σmax

Tri-axial compressive strength of natural core samples have been determined as 3.95MPa for sample “a”, 3.82MPa for “b”,
3.52MPa for “c” and 6.11MPa for “d” as given in Table3 and those are plotted against hydrate saturation in Fig.6. The tri-axial
strength of natural core samples can be compared with the results from Toyoura sand containing synthetic methane hydrate
including reconstituted samples in Fig.6. As shown in Fig.6, the tri-axial compressive strength of natural core samples has
increased with the rise of hydrate saturation. However, in the range of hydrate saturation from 0% to approx. 23%, the tri-axial
compressive strength seems to be unchanged and/or shows the slight increase, and the trend of increase in the tri-axial
compressive strength against hydrate saturation above 23% shows the good agreement with that of synthetic hydrate samples
of Toyoura sand. Meanwhile, the strength of reconsituted core samples containing synthetic methane hydrate shows the similar
trend to the results from Toyoura sand. The results from reconstituted samples are discussed again later in the subsection
where reconstituted core samples without forming methane hydrate are denoted as “Re-b” from the natural core sample “b”
and “Re-c” from the sample “c”.

Elastic Modulus E50

Secant elastic modulus has been determined at 50% failure of a natural core sample and the elastic modulus in relation to
hydrate saturation can be shown in Fig.7 along with the results from synthetic hydrate samples, i.e. Toyoura sand and
reconstituted cores. The increase in elastic modulus E50 against hydrate saturation including the results from reconstituted
specimen shows a proportional trend as shown in Fig.7. The trend of increase in the elastic modulus against hydrate saturation
is similar to each other between natural core sample and Toyoura synthetic methane hydrate sample, however the elastic
modulus of natural core sample becomes lower than that of Toyoura sample. The difference in elastic modulus between
natural sample and Toyoura sample can be read as approx. 200MN/m2 in the range of hydrate saturation from approx. 20% to
38% as it can be seen in Fig.7. As shown in Fig.4, fine component, i.e. particle size under 0.075mm, may contribute to the
difference between natural core samples and Toyoura sand which is nil in the content of fine particles. Furthermore, the E50 of
reconstituted core sample is rather lower than that of natural core sample. This is due to the change in bonding structure of
sand particles of reconstituted core samples while the particle size component of natural samples is not changed much in
reconstituted samples.

Poisson’s Ratio ν50

Poisson’s ratio ν50 is defined as the ratio of radial strain to longitudinal axial strain at 50% failure of natural core samples
ranges approx. 0.1 to 0.2 and there is no tendency to the change in Poisson’s ratio against hydrate saturation as shown in Fig.8.
Since Poisson’s ratios of synthetic hydrate samples are scattered in the range between approx. 0.05 and 0.23 showing no
dependency on hydrate saturation, the results from natural core samples show general agreement with those from synthetic
hydrate samples.

Natural Gas Hydrate Core Samples Compared with Synthetic Methane Hydrate Samples
Due to a lack of drill core samples containing natural gas hydrate, tri-axial compression tests on Toyoura sand containing
synthetic methane hydrate has been conducted so far to ascertain mechanical properties of gas hydrate bearing sediment.
However, the validity of the test results from synthetic gas hydrate sand has not been discussed assuming that characteristics of
synthetic hydrate samples represent those of natural gas hydrate bearing sediment. Difference in between natural gas hydrate
and laboratory formed synthetic hydrate has been argued employing SEM images3). Their microscopic observational study on
gas hydrate structure concluded similarity between natural (i.e. marine and permafrost gas hydrates) gas hydrate and
synthesized gas hydrate in terms of phase distribution and grain contact. Since drill cores of marine gas hydrate sediments
were recovered during the survey cruise 2004 from Tokai-oki to Kumano-nada, tri-axial compression tests on natural hydrate
core samples have been carried out afterwards. The tri-axial strength of those natural core samples shows the good agreement
with Toyoura sand containing synthetic methane hydrate as shown in Fig.6. On the other hand, in the results of elastic
modulusE50 in Fig.7, the elastic modulus of natural gas hydrate sample is lower than that of Toyoura sand containing synthetic
methane hydrate. Stress-strain relationships between natural core sample “c” and Toyoura synthetic hydrate samples, denoted
as “TGH1”and “TGH2”, can be represented in Fig.9 showing distinctive difference in volumetric strain curves of the three. Since
hydrate saturation of the natural core samples is similar to each other, the differences in initial porosity and/or the distribution
4 OTC 19277

of particle size is attributed to the change in the behavior of volumetric strain against axial strain. Initial porosity of synthetic
hydrate specimens is approx. 38% which is lower than that of natural specimen “c” as listed in Table 1. The uniformity
coefficient Uc of specimen “c” is approx. twice as large as that of Toyoura sand denoted as “e” in Table 2, while the mean
value of cumulative frequency D50 is 0.16 for specimen “c” and 0.18 for Toyoura sand respectively. The result suggests that
the size range of component particle of Toyoura sand is narrower than that of natural hydrate cores as shown in Fig.4.
Considering that fine particles have more space to move in pore, pore space can absorb fine particles in other words, when
volume change occurs due to the movement of grain particles. Thus, the volume change caused by a dilatancy effect, therefore,
becomes more prominent in the case of Toyoura sand comparing with natural core samples of which the distribution range of
particle size is wide. As shown in Fig.10, stress and strain curves of Toyoura sand shows strong dilatancy effect on volumetric
strain when comparing with reconstituted core samples denoted as “Rec-b” and “Rec-c” without synthetic gas hydrate. These
results support the effect of particle size distribution on the characteristics of deformation behaviour. Eventually, it can be
concluded that the arrangement of particle component is essential to evaluate elasticity and to clarify deformation
characteristics of natural gas hydrate bearing sediment.

Constitutive Model for Natural Gas Hydrate Bearing Sediments

The stress-strain relationship under a constant strain rate 0.1 % per minute shown in Fig.5 can be represented by variable-
compliance-type constitutive model4).
dλ *
= {a 1 (λ * -1) -m1 + a 3 λ * m3 } • σ * n ,
dt
Eq.1
λ ε 1 σ
λ* = , λ = , λ0 = , σ* = ,
λ0 σ Ei σ c0

where Ei is initial elastic modulus and σc0 means peak strength. In this section, E50 is used as initial elastic modulus Ei. The
parameter n represents the degree of time-dependency or visco-elasticity of material. In the model, compliance λ, i.e. inverse
of elastic modulus, is the only variable that varies with time t following Eq.1. Since one has only to incorporate a subroutine
for variation of elastic modulus into a simulation code for elastic analysis, the model is easy to introduce into a numerical
simulation of mechanical behavior.
The parameter E50 depends on methane hydrate saturation as shown in Fig.7. These parameters were determined based on
previous triaxial compression tests with constant strain rate. Since the time-dependency or visco-elasticity of sand is
considered to be stronger in the presence of methane hydrate, the parameter n would depend on methane hydrate saturation.
According to laboratory triaxial compression tests with alternative strain rate4), the value of n would be estimated by the
following equation,
1
n ={ } - 1, Eq.2
log 2 (0.0019 * S h + 1.0065)

where Sh shows methane hydrate saturation. The other parameters in Eq.1, such as a1, m1, a3 and m3, were determined so that
the numerical solution fitted the experimental results shown in Fig.5, referring to the previously proposed procedure**)(Okubo
et al. 2003). Determined all of the parameters in Eq.1, the stress-strain relation under constant strain rate 0.1 % per minute can
be calculated by Eq.1. The experimental curves (thin line) and the calculated curves (thick line) for the natural core samples b
(Sh 7.7 %) and c (Sh 37.6 %) are shown in Fig.11. Though calculated stresses are slightly higher than experimental ones after
the peak, the calculated curves are approximately consistent with the corresponding experimental results. These findings
indicate that variable-compliance-type constitutive model is, to a considerable extent, applicable to stress-strain curves of
natural core samples under triaxial compression tests with constant strain rate.
Variable-compliance-type constitutive model is simple and can be applicable to various time-dependent behaviors. Hence, the
validity of the model can be appreciated by creep tests or other laboratory experiments.

Conclusions
Tri-axial compression tests were conducted on drill cores containing natural gas hydrate recovered from survey drillings at
Eastern Nankai Trough region. In the results, tri-axial compressive strength of those natural core samples shows the good
agreement with that of Toyoura sand containing synthetic methane hydrate. On the other hand, discrepancy between samples
of natural and synthetic gas hydrate can be confirmed in elastic modulus E50. This is attributed to the difference in the particle
size distribution. Reconstituted core samples are no longer consistent with natural core samples in terms of deformation
characteristics due to the changes in bonding structure of sediments. No significant tendency has been confirmed in Poisson’s
ratio of natural core sample in relation to pore saturation of gas hydrate, which is similar to the past experimental results from
Toyoura sand containing synthetic methane hydrate. Variable-compliance-type constitutive model is proposed to predict a
stress-strain relationship of natural core samples which is still quite limited in number to investigate the strength and
deformation behaviour in a production scale.
OTC 19277 5

Acknowledgements
The research has been conducted in the project of MH21 research consortium. Our special thanks and warm appreciation
should be expressed to Mr. Takao Ohno and Mr. Shigenori Nagase for their dedication to our laboratory experiments. Our
tireless appreciation must be extended towards the Agency of Natural Resouces and Energy, METI Japan for the finantial
support to the MH21 research project.

Nomenclature
Ei Initial elastic modulus
n Parameter determining time-dependency of material
Sh Methane hydrate saturation
t Time
ε Axial strain
λ Compliance
λ0 Initial compliance (Inverse of initial elastic modulus)
λ* Normalized compliance
σ Deviator stress
σc0 Tri-axial compressive strength at a certain strain rate
σ* Normalized deviator stress
σmax Tri-axial compressive strength at 0.1% strain rate
εaf Axial strain at failure
E50 Scant elastic modulus at 50% of failure
ν50 Poisson’s ratio at 50% of failure
D10 Grain size at which 10% of total grain sample in weight passes mesh opening
Uc coefficient of uniformity given by D60/D10

References
1) Yasuda, M., Dallimore, S.R., Task force for production testings of MH21 Research Consortium for Methane Hydrate resources
in Japan, “Summary of the Methane Hydrate Second Mallik Production Test 2007”, Journal of the Japanese Association for
Petroleum Technology, Vol.72, No.6, pp.603-607 (2007).

2) Masui, A, Haneda, H, Ogata, Y, and Aoki, K., "Effect of Methane Hydrate Formation on Shear Strength of Synthetic Methane
Hydrate Sediments," Proc.15th Int. Offshore and Polar Eng. Conf., Soeul, Korea, ISOPE, Vol.1, pp 364-369 (2005).

3) Stern, L, Circone, S, Kirby,S, and Durham, W., “SEM imaging of gas hydrate formation processes and growth textures, and
comparison to natural hydrates of marine and permafrost origin,” Proc.5th Int. Conf. on Gas Hydrates, ICGH, Vol 1, Paper ref.
1046, pp 300−309 (2005).

4) Miyazaki, K., Masui, A, Haneda, H, Ogata, Y, and Aoki, K., "Application of Compliance Technique to Understanding of
Stress-strain Relationship for Methane Hydrate Bearing Sediment," Proc.17th Int. Offshore and Polar Eng. Conf. OME.,
Lisbon, Portugal, ISOPE, pp. 57-62 (2007).
6 OTC 19277

Figure 1

Survey drilling into

Eastern Nankai Trough

Figure 2

Figure 3
OTC 19277 7

100

a
d
Cumulative frequency (%)

80

b
60

Figure 4
40
c

20
e
0
0.001 0.01 0.1 1 10
Particle size (mm)

8 -8
c
c
6 -6
Deviator stress (MPa)

Volumetric strain (%)

a
4 -4
d
b d Figure 5
a
2 -2

0 0
0 2 4 6 8 10 12 14
2
-2
Axial strain (%)

10
Triaxial compressive strength (MPa)

4 Figure 6
● Natural core sample
2 ○ Reconstituted sample
■ Synthetic GH sample

0
0 10 20 30 40 50 60 70
Hydrate saturation S h (%)
8 OTC 19277

1000
● Natural core sample
Elastic modulus Ｅ50 (MN/m2)

○ Reconstituted sample
800
■ Synthetic GH sample

600

Figure 7
400

200

0
0 10 20 30 40 50 60 70
Hydrate saturation Sh (%)

0.5
● Natural core sample
0.4 ○ Reconstituted sample
■ Synthetic GH sample
Poisson's ratio ν50

0.3
Figure 8
0.2

0.1

0
0 10 20 30 40 50 60 70
Hydrate saturation S h (%)

8 -16

TGH1 (Sh39.5%) c (37.6%)

6 -12
TGH2 (Sh 35.2%)
Volumetric strain (%)
Deviator stress (MPa)

4 -8 Figure 9

2 -4

0 0
0 2 4 6 8 10 12 14

-2 4
Axial strain (%)
OTC 19277 9

6 -12
Sh 0%

4 -8

Volumetric strain (%)

Deviator stress (MPa)

T1
T2
Re-c
Re-b
2 -4
Figure 10

0 0
0 2 4 6 8 10 12 14

-2 4
Axial strain (%)

6
c (Sh 37.6 %)
Deviator stress [MPa]

Figure 11

b (Sh 7.7 %)

2
Exp. results
Calc. results

0
0 2 4 6 8 10 12 14
Axial strain [%]
10 OTC 19277

Initial Porosity Particle Density Initial Water Content Bulk Density

Specimen
% g/cm3 % g/cm3
a 49.0 2.680 27.9 1.748
b 50.8 2.717 20.4 1.721
c 44.2 2.660 23.0 1.827
d 49.3 2.720 28.7 1.774

Table 1

Specimen D10 D50 Uc

mm mm %
a 0.027 0.084 3.5
b 0.045 0.14 3.6
c 0.065 0.16 2.8
d 0.076 0.18 2.7
e : Toyoura 0.120 0.18 1.6

Table 2

Sh σmax εaf E50

Specimen vol.% MPa % MN/m2 ν50

a 22.5 3.95 5.27 264.0 0.19

b 7.70 3.52 6.94 139.3 0.11
c 37.6 6.11 5.18 368.9 0.10
d 9.38 3.82 7.29 207.1 0.15

Table 3