Applied Clay Science 152 (2018) 211–220

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Applied Clay Science

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

Research paper

Performance studies of water-based drilling fluid for drilling through T

hydrate bearing sediments
⁎
Madhukar Srungavarapu, Krishan Kumar Patidar, Akhilendra Kumar Pathak, Ajay Mandal
Department of Petroleum Engineering, Indian Institute of Technology (ISM) Dhanbad, India

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

Keywords: Hydrate-bearing formation is a highly unconsolidated formation and being fragile, the hydrates get readily
Water-based drilling fluid decomposed while drilling through it. To successfully drill through the hydrates, the drilling fluid should have
Gas hydrates low mud invasion, exhibit optimum properties for wellbore stability, prevent the formation of the hydrates in the
Rheology annulus, choke lines, etc. Initial experiments were performed with the drilling fluid with the composition as
Inhibition
artificial seawater, 3.0 wt% bentonite, 3.0 wt% barite, and 0.3 wt% carboxymethyl cellulose (CMC) (wt%). The
Carboxymethyl cellulose
rheological, filtration and gelling properties were determined. The synergistic effects of xanthan gum (XG) and
Artificial seawater
CMC with different compositions were used to study rheological properties. The drilling fluid with desirable
rheological properties was further studied at low temperatures and at high pressures. The drilling fluid was
tested for hydrate inhibiting properties in a high-pressure autoclave vessel at 16.55 MPa and at 0 °C and further
tested with increasing water cut at both static and dynamic conditions. The experimental results reveal that XG
has better viscosifying properties while CMC has a better filtration loss properties. With the increase in the
concentration of the both CMC and XG, there has been an increase in viscosity, yield point, gel strength and
decrease in the filtration loss. The experimental results also show that the developed drilling fluid has good
inhibiting properties under static conditions but with an increase in water cut the risk of formation of hydrates
increases.

1. Introduction
Gas hydrates are crystalline non-stoichiometric compounds in
which water molecules enclose low molecular weight gases in a cage
like structure. Gas hydrates are stable at low temperatures (< 26 °C)
and at high pressure (> 3.8 MPa at 3 °C) conditions (Sloan and Koh,
2000). These conditions are majorly found in sediments of marine
continental margin and permafrost environments (Rogers, 2015; Sloan
and Koh, 2000). The major fraction of gas hydrate deposits are found
with the marine environments (Kvenvolden, 1993). Gas hydrates with
potential energy resources have attracted researchers & energy industry
towards development of proper drilling and production technology
(Demirbas, 2010; Makogon, 2010).
Hydrates extent as deep as 600 m from the seabed in deep marine
environments (Sorgard et al., 2001). While hydrate-bearing zones are
drilled, the change in pressure and temperature of the sediments causes
the gas hydrates to dissociate into gas and fresh water. Hong et al.
(2003) has shown that the heat transfer is one the main mechanisms of
hydrate destabilization and production from sediments. Fereidounpour
and Vatani (2015) have made a detailed study on the heat transfer by
the water based drilling fluids and found that the addition of polymers
reduces the heat transfer to hydrate-bearing sediments (HBS). Hydrate
dissociation causes change in mechanical and physical properties of
sediments. The change of properties of sediments includes in increase of
permeability, loss of cementation resulting in reduction of strength of
cementation which thus causes wellbore instability, casing running
difficulties, gasification of cementing, and personal health risks (Ning
et al., 2013; Spence and Hyndman, 2001). The dissociation process is
continued as long as heat and change in pressure is introduced into the
wellbore (Tan et al., 2005). The re-formation of hydrates in the drilling
fluid caused by the dissociated gas is another challenge to drilling fluid
circulation (Jiang et al., 2011; Teodoriu et al., 2008). Temperature and
pressure must be controlled within a reasonable range in order to in-
hibit the destabilization of gas hydrates while drilling. Simultaneously,
the drilling mud should allow to drill at controlled penetration rate. In
addition to that, the drilling fluid should inhibit the formation of hy-
drates in a fluid column and should have good rheological properties
along with low filtration loss.
Currently, the drilling fluid used is either water based or oil based.
Ning et al. (2013) have stated that the induction time for hydrate

⁎
Corresponding author.
E-mail address: ajay@iitism.ac.in (A. Mandal).

https://doi.org/10.1016/j.clay.2017.11.014
Received 12 June 2017; Received in revised form 10 November 2017; Accepted 13 November 2017
Available online 20 November 2017
0169-1317/ © 2017 Elsevier B.V. All rights reserved.
M. Srungavarapu et al. Applied Clay Science 152 (2018) 211–220

formation in the oil based drilling fluid is lower than the water based Table 1
drilling fluid as gas is readily dissolvable in oil than water. The increase Properties of xanthan gum (XG) used in the experiments.
in either bentonite or water concentration increases the risk of forma-
Properties Values
tion due to increase in the contact surface resulting in an increase of
nucleation sites (Kelland et al., 2008; Ning et al., 2013). Moreover, pH (1% w/v water) 6.3
under extremely cold water conditions, the oil-based drilling fluid be- Density 1.5 g/cm3
Ash 9.69 wt%
come thick and sluggish which results in high viscosity and increased
Nitrogen < 1.5 wt%
equivalent circulating density (ECD) causing in fracture the formation Pyruvic acid < 2.4 wt%
(Sorgard et al., 2001). Heavy metals < 0.001 wt%
The typical drilling fluids used in offshore are formulated with a
polymer as a base with 20–25% NaCl and high concentration of ther-
modynamic hydrate inhibitors (THIs) (Ebeltoft et al., 1997). These THIs 2. Experimental section
have a limited ability to prevent the formation of hydrate (Kelland
et al., 2008). The compatibility of the compounds with salts is a chal- 2.1. Materials
lenge and generally causes operational problems. The ethylene and
propylene glycols used as THIs are more expensive and needed to be The bentonite and xanthan gum used in the experiments was pur-
added in large amounts to show significant effects of suppression chased by LOBA Chemie Pvt., Mumbai, India. Ltd. The bentonite pri-
(Halliday et al., 1998). This high concentration use of thermodynamic marily consists of montmorillonite. Xanthan gum is polysaccharide
hydrate inhibitor might prevent the formation of hydrates in the well- anionic product obtained from aerobic fermentation of the bacteria
bore, but it can also affect the borehole stability by dissociating these Xanthomonas Campestris. The important properties of xanthan gum are
hydrates in the sediments. given in Table 1.
Currently, researchers are concentrating on the application of ki- Methane Gas was provided by Ultra-Pure Gases Pvt. Ltd., Mumbai,
netic hydrate inhibitors (KHIs) in the use of drilling fluid to prevent the India, with a purity of 99.5%. Carboxymethyl Cellulose (CMC), Barium
formation of these hydrates (Kelland, 2006). KHIs are water soluble Sulfate (BaSO4), Sodium Chloride (NaCl), Calcium Chloride(CaCl2) and
polymers when added in low concentrations they delay the nucleation Magnesium Chloride(MgCl2) used in this experiment were obtained
and hinder the growth of hydrate crystal by disrupting the hydrogen from Avantor Performance Materials India Ltd., Mumbai, India. The
bonding between the water and the gas molecule. Unlike THIs, these do salts procured are of 99.5% purity and properties of CMC used in the
not shift the hydrate-liquid-vapour-equilibrium (HLVE) curve (Rogers, experiments are given in the Table 2.
2015).
KHI polymers are added to the drilling fluid in the range of 0.3 wt%
to 2 wt% which changes the rheology of the fluid at low temperatures 2.1.1. Properties of bentonite used
to elevated levels. Moreover, the influence of rheology of the KHI with The physical properties of the bentonite used in the experiments
drilling fluid under high pressure is very limited (Jiang et al., 2011; were given in Table 3. The particle size distribution (PSD) of bentonite
Saikia and Mahto, 2016; Zhao et al., 2015). These KHIs are highly ex- used in the study was analyzed with Nano-S90 Zetasizer Ver. 6.34 of
pensive to prepare and have a very poor biodegradability that is not Malvern Instruments Ltd. Three different peaks (Fig. 1) were obtained
appreciated in offshore drilling (Rogers, 2015). Additionaly, the in- for different intensity and volume with mean size 505 nm (42.2%),
hibition effect of the carboxymethyl cellulose (CMC) and xanthan gum 62.93 nm (25.9%), and 2590 nm (9.4%). Bentonite clay particles dis-
(XG) which are biodegradable polymers was reported to have a similar tributed in water ranges in size from 30 nm to 3200 nm with an average
effect to that of KHIs. Ganji et al. (2007) reported that the addition of size 279.8 nm. The results of particle size distribution analysis are given
xanthan gum decreased the promotion effect of sodium dodecyl sulfate in Table 4.
(SDS) on the formation of hydrate and also increased the induction time The XRD diffractogram of the bentonite is shown in Fig.2. The figure
of sample when compared with the sample without xanthan gum. With indicates that it is rich in montmorillonite with kaolinite as clay mineral
the increase in the concentration of xanthan gum, same effect was components accompanying with quartz as the main impurity plus other
found with greater increase in induction time. Kelland et al. (2008) minerals.
observed that with the addition of 0.5 wt% xanthan gum to the sample Abdou et al. (2013) & Abdou and El-Sayed Ahmed (2011) in-
increased the induction from 200 min to 1200 min. A similar effect was vestigated the effect the particle size of bentonite on the rheology of the
observed with another sample whose induction time increased from drilling fluid. They observed that with a constant 7.5 w/v % bentonite
100 min to 1100 min. Xiaolan et al. (2011) stated that carboxylmethyl concentration, the Apparent Viscosity (AV), Plastic Viscosity (PV), Yield
cellulose showed inhibition effect on gas hydrates due to the presence Point (YP), Gel Strength and Thixotropic nature of fluid decreased with
of (eOH) group and ether active groups that interacted with a water increase in the particle size. This is because of the fact that finer the
molecule to inhibit the hydrate formation. The details of hydrate for- grain size, the higher is the surface area of the bentonite clay which
mation and dissociation characteristics in presence of different extra- controls the rheological properties of the fluid. Bentonite particles with
neous materials have been discussed in our earlier studies (Saw et al., higher surface area possess higher swelling tendency compared to
2012, 2013; Kakati et al., 2014, 2015). coarser particles. Higher amount of particles (in case of fine particles)
In this work, the study the rheology of the drilling fluid with dif- causes net higher amount of interactions, which in-turn increases the
ferent additives and with varying concentrations was performed, se- viscosity and gel strength.
parate investigations on change of rheology at high pressures and low
temperatures was also performed. A discrete rheological study was also Table 2
performed to understand the rheological changes due to calcium and Properties of carboxylmethyl cellulose (CMC) used in the experiments.
magnesium ions which are frequently observed in formation fluid. The
Properties Values
hydrate formation tendency of drilling fluid was observed under static
inhibition study including the conditions of water encroachment into pH (1% w/v water) 7.13
drilling fluid that simulates the kick conditions. The study concludes Viscosity (1% w/v water at 20 °C) 1800 mPa s
Viscosity range HV (high viscosity)
with the discussing the significant observations.
Chloride < 0.25 wt%
Heavy metals < 0.002 wt%

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M. Srungavarapu et al. Applied Clay Science 152 (2018) 211–220

Table 3 use of Hamilton Beach Spinner. Filtration properties of drilling fluids

Properties of bentonite used in the experiments. were tested using the hydraulic Fann API filter press. The drilling fluid
is subjected through a porous membrane filter paper at a pressure dif-
Properties Values
ferential of 0.68 MPa for 30 min.
pH (2% w/v water) 10.5 Rheological studies at room conditions were performed with OFITE
Density 2.5 g/cm3 800 8-speed electronic viscometer equipped with bob and cup ar-
Swelling power 26 ml
rangement. The bob rotations per minute (RPM) is regulated by the
Sedimentation value 1.8 ml
controller to give the dial reading at 8 different shear rates ranging from
5.11 s− 1 to 1021.38 s− 1. During the experimental work three replicate
10 100 1000 runs were conducted for each drilling fluid sample to verify the re-
12 12
PSD of Bntonite Clay
producibility of the experimental data. The reproducibility of the ex-
10 10
perimental runs is within the acceptable limits with standards devia-
Intensity (%)

8 8
tion ± 0.002 to 0.003. The graph is plotted between the shear stress
6 6
and shear rate on either log-log scale or standard scale to determine the
4 4
type of curve. Curve fitting method is used to determine other im-
2 2 portant parameters such as consistency index [Pa sn], minimum yield
0 0 stress [Pa] and flow index.
10 100 1000 Individual rheology measurement at low temperature and at high
Size (r. nm) pressure was performed with Bohlin Gemini 2, manufactured by
10 100 1000 Malvern Instruments U.K Ltd. The maximum safe pressure and tem-
8 PSD of bentonite clay 8 perature application of rheometer is 4.9 MPa and −20 °C to 90 °C re-
spectively.
Volume (%)

6 6
4 4
2 2
0 0
10 100 1000
Size (r. nm)
Fig. 1. Particle size distribution of bentonite clay in aqueous suspension.
Table 4
Particle size distribution results of bentonite clay in water.
Peak(s) Size (r.nm) % Intensity
Peak 1 62.93 14.4
Peak 2 505.0 84.2
Peak 3 2590.0 1.4
2.2. Apparatus and experimental procedure
Most of the offshore water based drilling fluids employ sea water
due to its economic viability. To simulate the sea water for the ex-
periments, sodium chloride was added to distilled water to a salinity of
3.5 wt%. Iscan and Kok (2007) has shown that inter-particular energy
between clay and water depends upon the concentration of bentonite
and at 3 wt% of bentonite, non-Newtonian suspension behavior is
visible and follows Herschel-Bulkley model. Hence, 3 wt% bentonite
concentration was fixed for all drilling fluid formulations. Control of
hydrostatic pressure while drilling hydrate-bearing sediments (HBS) is
highly important, hence the use of managed pressure drilling (MPD)
was suggested in the both published and unpublished literature (Fossil
and Sangesland, 2004; Hannegan, 2005, 2006). Managed pressure
drilling keeps the bottom hole hydrostatic pressure in the range of
50–100 psi (0.34–0.68 MPa) higher than formation pressure. To sup-
port MPD, the barite concentration was set at 3 wt% to obtain drilling
fluid weight as 8.94 ppg (= 1.07 SG) which gives the maximum 100 psi
overburden pressure at 1700 m from sea level. Liyi et al. (2014) has also
suggested that the optimum relative density of the drilling fluid should
be in the range of 1.05–1.2 SG and fluid loss no > 15 ml for 30 min at
0.68 MPa pressure differential.
The drilling fluid test samples were prepared using simulated sea-
water, 3 wt% bentonite concentration, 3 wt% barite along with varying
CMC and xanthan gum concentration from 0.3 wt% to 0.6 wt% with the
The equipment used for the study of hydrate formation is Vinci
Video Hydrate Cell, designed by the Vinci Technologies, France is
shown in Fig. 3. The system consists of a constant volume stainless steel
hemispherical hydrate cell with a capacity of 250 cm3. The working
temperature range was from −10 °C to 60 °C and the with a maximum
working pressure capacity of 20.7 MPa. The pressure sensor was con-
nected to the inlet line of autoclave just after the isolation valves with
the measuring accuracy of ( ± ) 0.01 MPa. The temperature sensor sits
inside the cell and has the measuring accuracy of ( ± ) 0.1 °C. The
temperature of the cell was controlled by the thermostatic bath and the
bath temperature was controlled by the user with help of computer
interface. A magnetic stirrer with an adjustable rotation speed ranging
% Pd from 0 to 1000 RPM is equipped within the autoclave cell to agitate the
test fluid.
25.9 Experimental procedure followed for the kinetic hydrate studies:
42.2
9.4
1. The test fluid of volume 120 cm3 was filled into the hydrate cell at
30 °C, the cap of the cell was placed on the top and secured tightly.
2. The cell was then placed in the thermostatic bath which was
maintained at desired temperature. Then cell was allowed to cool
down to the desired level.
3. The cell was then pressurized with methane gas up to desired
pressure. Gas injection caused an increase in temperature of the cell
and it was again cooled down to the desired level.
4. Based upon the type of experiment, the magnetic stirrer was pow-
ered to agitate the test fluid at constant 1000 RPM.
5. The algorithm based interface recorded the real-time pressure and
temperature with the interval of 10 min. The experiment was car-
ried out till pre-estimated time.
3. Results and discussions
3.1. Drilling fluid formulations and rheology
The important criteria for drilling fluid is to have sufficient visc-
osity, yield strength, cutting carrying capacity and low filtration
properties in order to have good wellbore stability, reduce interactions
between formation sediments and drilling fluid. Iscan and Kok (2007)
shown that the addition of CMC to drilling fluid reduces the fluid loss
property. They have stated that use of 1 g of CMC in 350 ml (i.e.
0.285 wt%) along with bentonite and barite is the most optimum value
to reduce filtration losses. To perform the experiments, initially two
drilling fluid formulation were prepared respectively as, DF-1: Artificial
sea water + 3 wt% Bentonite + 3 wt% Barite + 0.3 wt% CMC; DF-2:

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M. Srungavarapu et al. Applied Clay Science 152 (2018) 211–220

Fig. 2. XRD diffractogram of bentonite used in the ex-

periments.

(a)

(b)

Fig. 3. Schematic diagram of gas hydrate apparatus used in the experiments.

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M. Srungavarapu et al. Applied Clay Science 152 (2018) 211–220

Table 5
Rheological properties of DF-1 & DF-2 at surface conditions.

Drilling fluid K (Pa sn) n PV (MPa s) YP (Pa) AV (MPa s) FL (ml) YP/PV ratio (1000 s− 1) Gel (10 s/10 min) (Pa/Pa)

DF-1 0.087 0.678 8 2.4 10 9.8 0.3 0.478/0.67

DF-2 0.609 0.548 17 9.1 26.5 7.8 0.535 0.5/1.675

1000 DF-2 1000

DF-1

100
100

Shear Stress (Pa)

Shear stress (Pa)

10

10

DF-3
1
DF-4
0.1 DF-5
DF-6
DF-2
0.1
0.01
0.01 0.1 1 10 100 1000 10000
0.01 0.1 1 10 100 1000
Shear rate (1/s)
Shear rate (1/s)
Fig. 4. Shear stress - shear rate plots of DF-1 & DF-2.
Fig. 5. Shear stress - shear rate plot of DF - 2, 3, 4, 5 & 6.

Artificial sea water + 3 wt% Bentonite + 3 wt% Barite + 0.7 wt%

CMC. The rheological properties of DF-1 & DF-2 are given in Table 5.
Fig. 4 shows the shear stress – shear rate curves plotted for the DF-1
and DF-2. The shape of the curves obtained was similar to the curves
plotted by Benyounes et al. (2010) for bentonite-CMC mixtures and can
be accurately matched with the power-law equation given as follows:
τ = K (γ ) n
where τ, K, γ and n are shear stress [Pa], consistency index [Pa sn],
shear rate [1/s] and flow index respectively. With the increase in the
CMC concentration, decrease in the values of flow index and increase in
consistency index was observed. Mahto and Sharma (2004) described
high yield point to plastic viscosity ratio (YP/PV ratio) value indicates
the shear thinning behavior and it is highly desirable for the drilling
fluid to suspend the cuttings (i.e prevent falling of cuttings under
gravity effect) at static conditions while show the property of New-
tonian behavior when circulation resumes. The flow index values ran-
ging from 0 to 1 denotes shear thinning behavior while 0 indicates high
shear thinning behavior and 1 indicates the Newtonian behavior. It can
be easily anticipated that the flow index and YP/PV ratio are inversely
proportional for shear thinning liquids. The hydrates extend to the
depth of 600 m below sea bed can be successfully isolated with the
surface casing. The outer diameter of the surface casing range from 16″
to 20″ causing very low annular velocities. Plastic viscosity is directly
proportional to mud weight of the drilling fluid. For efficient and faster
drilling, lower plastic viscosity and apparent viscosity was desired.
Experimentally it has been found that DF-1 & DF-2 was unable to hold
added barite due to very low yield point (and gel strength). Addition to
that, both drilling fluids displayed low YP/PV ratio and due to these
reasons DF-1 and DF-2 were not considered for the further evaluation.
Xanthan gum (XG) was used to improve the yield point and gel
strength of the drilling fluid. In order to make analysis, 4 different kinds
of formulation were used to test the influence of XG and CMC on
(1) rheology. The different formulations that were prepared respectively
are; DF-3: Artificial sea water + 3 wt% Bentonite + 3 wt% Barite
+ 0.3 wt% CMC + 0.3 wt% XG; DF-4: Artificial sea water + 3 wt%
Bentonite + 3 wt% Barite + 0.4 wt% CMC + 0.4 wt% XG; DF-5:
Artificial sea water + 3 wt% Bentonite + 3 wt% Barite + 0.6 wt%
CMC + 0.4 wt% XG and DF-6: Artificial sea water + 3 wt% Bentonite
+ 3 wt% Barite + 0.4 wt% CMC + 0.6 wt% XG.
Various rheological parameters were studied for each drilling fluid
such as plastic viscosity, apparent viscosity, yield point and gel strength
are listed in the Table 6. Fig. 5 is the log-log plot of shear rate – shear
stress of the DF-3, DF-4, DF-5, DF-6 & DF-2, which was used for the
comparative purposes. Furthermore, it was evident that the rheological
behavior observed from the DF-3, 4, 5 & 6 can be described accurately
with Herschel-Bulkley Equation:
τ = τ0 + K (γ ) n (2)
where τ0 is the minimum yield stress [Pa] that has to be applied in
order to cause shearing action in the drilling fluid.
It was found that with the increase in the XG polymer concentration
resulted in an increase in yield stress (τ0), plastic viscosity, apparent
viscosity, gel strength and the YP/PV ratio (compare DF-4 & DF-6). In

Table 6
Rheological properties of DF- 3, 4, 5 & 6.

Drilling fluid τo (Pa) K (Pa sn) n PV (mPa s) YP (Pa) AV (mPa s) FL (ml) YP/PV ratio (1000 s− 1) Gel (10 s/10 min) (Pa/Pa)

DF-3 1.326 1.321 0.426 12 13.4 26 9.3 1.117 4.3/5.74

DF-4 2.82 2.23 0.41 18 21.06 40 8.5 1.17 8.14/9.1
DF-5 3.117 3.23 0.403 24 29.2 54.5 8.1 1.2 9.1/10.5
DF-6 6.67 5 0.356 23 39.2 64 8.4 1.7 14.36/17.2

215
M. Srungavarapu et al.
contrast, a simultaneous decrease in flow index ‘n’ was also observed.
Similarly, with the increase in the CMC polymer concentration the same
behavior was observed though with lesser magnitude (compare DF-4 &
DF-5).
The YP/PV ratio of DF-3 was almost equal with DF- 4 & 5, however,
it was considered advantageous due to low plastic viscosity and ap-
parent viscosity. Saikia and Mahto (2016) stated that the apparent
viscosity below 30 mPa s would yield a high penetration rate. Zhao
et al. (2015) successfully formulated and tested the drilling fluid that
displayed the yield point of 19.5 Pa at 2 °C without any addition of
inhibitors. Though DF-6 has better YP/PV ratio, high yield point
(> 19.5 Pa) results in high ECD causing the fracture of the low-pressure
formations. DF- 4 & 5 has good filtration loss control than DF-3 but it
was undermined by the high apparent viscosity (> 30 mPa s). Ad-
ditionally, it was found that DF-3 had satisfactorily held barite in sus-
pension for > 72 h which is clearly evident of suspending drill cuttings
at static condition.
3.2. Properties at low temperature
With the increase in the depth of the seabed, the hydrostatic pres-
sure increases, and the temperature decreases. However, a constant
temperature was found till seabed after a certain increase in depth
(Forrest et al., 2005). The lowest temperature experienced in the deep-
water drilling was around 2 °C to 4 °C in most parts of the offshore
where deep-water drilling operations were active except in the North
Sea, including the Gulf of Mexico, the West Africa and the South China
Sea (Zhao et al., 2015). The lowest temperature used in the experiment
was fixed at near to − 1.7 °C which is lower than conventional sea bed,
for better understanding of low-temperature rheology. Table 7 shows
the rheological parameters of the DF-3 sample at different temperatures
ranging from 30 °C to −1.7 °C. Fig. 6 shows the shear rate – shear stress
curves of DF-3 at different temperatures.
With decrease in temperature all the rheological parameters have
increased except YP/PV ratio. The plastic viscosity had increased from
12 mPa s to 30.6 mPa s and is at the permissible limit. The minimum
yield stress (τ0) increased from 1.326 Pa to 4.72 Pa along with increase
in yield point from 13.4 Pa to 26.8 Pa. The YP/PV ratio had decreased
constantly at low temperature, which indicated that cutting carrying
efficiency decreased with decrease in temperature and plastic viscosity
is affected higher than yield point. This is due to the increased cohesion
forces at low temperature between the particles which tend to increase
in plastic viscosity. Drilling fluids formulated by Saikia and Mahto
(2016) & Zhao et al. (2015) has plastic viscosity range of
16 mPa s–20 mPa s and yield point ranging from 14.12 Pa–19.5 Pa at
2 °C. DF-3 has shown plastic viscosity of 19.5 mPa s and yield point
18.41 Pa at 2.76 °C which is well within the range. Hence, the obtained
rheological properties have a satisfactorily performance.
3.3. Properties at high pressure
The hydrostatic pressure exerted by drilling fluid depends upon the
depth of circulation and its weight. The rheology of the drilling fluid
certainly changes upon the application of high pressures. DF-3 was
subjected to the pressures of 2.44 MPa and 4.9 MPa. The rheological
parameters calculated are listed in Table 8. Fig. 7 shows the shear rate –
Table 7
Rheological properties of DF-3 at low temperatures.
Temperature (°C) τo (Pa) K (Pa sn) n PV (MPa s)
30 1.326 1.321 0.426 12
14.5 2.75 1.52 0.44 16.5
2.76 3.95 1.33 0.4742 19.5
− 1.72 4.72 1.97 0.4811 30.6
216
Applied Clay Science 152 (2018) 211–220
100
Shear Stress (Pa)
10
30°C
14.5°C
2.76°C
-1.72°C
1
0.01 0.1 1 10 100 1000
Shear rate (1/s)
Fig. 6. Shear stress shear rate plot of DF-3 at low temperatures.
shear stress curves of DF-3 at different pressures.
Yield stress, plastic viscosity, yield point, apparent viscosity and YP/
PV ratio showed an increasing trend with an increase in pressure.
While, consistency index had shown a decreasing trend with increase in
pressure. The plastic viscosity showed a slight increase and was rela-
tively in the range. Briscoe et al. (1994) has stated a similar trend for
plastic viscosity and yield point with increase in pressure for water-
based drilling fluid. The increase in YP/PV ratio indicated that high
pressures have affected yield point to a greater extent than plastic
viscosity. Plastic viscosity is dependent upon the weight of the mud and
water based mud has low compressibility due to which the change in
PV was minimum even with the application of pressure.
3.4. Contamination of drilling fluid by Ca2 + & Mg2 + ions
Bentonite naturally composes of montmorillonite clay which has a
high surface area or high activity. Montmorillonite clay readily absorbs
water dispersing itself and increasing the viscosity. This material can be
electrically unbalanced by addition of magnesium, iron or calcium ions
to replace aluminum ion. The addition of Ca2 + and Mg2 + greatly re-
duces the hydration and dispersion of clay in water. During drilling, the
formation water contains calcium and magnesium ions which could
enter the borehole and changes the performance of the drilling fluid
(Caenn et al., 2011). To test the ability of the drilling fluid to prevent
the change in rheology, experiments were performed with the addition
of the calcium chloride and magnesium chloride salts at different
concentrations into the drilling fluid. The added salt concentrations into
the drilling fluid were in line with Jiang et al. (2011). The concentra-
tion of contaminants added is listed in Table 9. The measured para-
meters including the yield point, yield stress, plastic viscosity, apparent
viscosity, gel strength, fluid loss, consistency index and flow index are
given in Table 10.
The effect of contamination on rheological properties was small and
this drilling fluid was resistive towards calcium and magnesium
YP (Pa) AV (MPa s) YP/PV ratio (1000 s− 1)
13.4 26 1.117
16.82 34.06 1.02
18.41 38.81 0.94
26.8 58.63 0.874
M. Srungavarapu et al. Applied Clay Science 152 (2018) 211–220

Table 8
Rheological properties of DF-3 at high pressures.

Pressure (MPa) τ0 (Pa) K (Pa sn) n PV (mPa s) YP (Pa) AV (mPa s) YP/PV ratio (1000 s− 1)

0.1 1.326 1.321 0.426 12 13.4 26 1.117

2.44 4.36 3.24 0.35 12.5 19.6 33 1.568
4.9 10.07 2.77 0.36 14.5 26.3 42 1.81

bentonite. A similar effect is described here based upon the rheological

observations. The interaction of added ions with bentonite was reduced
due to adsorption of XG on bentonite and additionally XG and CMC
being a slightly anionic polymer would had readily interacted with ions
100 causing reduced net positive charge on ions which reduced the floc-
Shear Stress (Pa)

culation power of cations. The cation and anionic polymer interaction

was evident as the CMC being an anionic polymer has interacted added
ions that resulted in slight increase in filter loss.
Similarly, an experiment was performed on the influence calcium
and magnesium ions on bentonite. Two samples were prepared; Sample
10 1: Artifical sea water + 0.4 wt% CaCl2 + 0.4 wt% MgCl2 + 3 wt%
Bentonite & Sample 2: 0.4 wt% CaCl2 + 0.4 wt% MgCl2 along with
0.3 wt% XG + 3 wt% Bentonite. It was observed that precipitation of
0.1 MPa the bentonite happened in sample 1 within initial 20 min but whereas
2.44 MPa in sample 2 the precipitation was not detected at the same time. This is
4.9 Mpa due adsorption of XG over the bentonite which inhibits the interaction
1 of cation and bentonite which causes the precipitation.
0.01 0.1 1 10 100 1000
Shear Rate (1/s) 3.5. Hydrate inhibition studies
Fig. 7. Shear stress - shear rate plot of DF-3 at high pressures.
Three main experimental methods were followed to evaluate the
hydrate inhibition of the test sample i.e. at a constant temperature;
Table 9 constant pressure and with a constant volume (Liu et al., 2016). The
Drilling fluid and contamination concentration.
constant volume method was used in this experiment. The initial op-
Notation Drilling fluid and contamination conce`ntration erating temperature and pressure were set at 0 °C and 16.55 MPa re-
spectively. Fereidounpour and Vatani (2015) stated that 10 h (600 min)
C-0 DF-3 is sufficient time for drilling hydrate-bearing sediments and cementing
C-1 DF-3 + 0.3 wt% MgCl2 + 0.1 wt% CaCl2
for complete isolation. Jiang et al. (2011) & Kelland et al. (2008) stated
C-2 DF-3 + 0.5 wt% MgCl2 + 0.2 wt% CaCl2
C-3 DF-3 + 0.8 wt% MgCl2 + 0.4 wt% CaCl2 that the period > 1000 min was considered to be sufficient to under-
stand the inhibition effect of the test sample. Hence, the experiment was
performed till 1100 min to provide sufficient time to understand the
contamination. All the parameters except consistency index were found hydrate formation and inhibition studies. The shearing power of the
to increase with an increase in the concentration of contaminants. Such magnetic stirrer was not sufficient to keep the drilling fluid in the dy-
behavior was found to be synonymous with Amoco (1994) & Jiang et al. namic condition and hence the static condition was used to determine
(2011). Calcium and magnesium ions have caused flocculation of the inhibition efficiency of drilling fluid. Ning et al. (2010) reported
bentonite was that made it behave as inert solids in suspension which that the static study has sufficiently indicated the formation of hydrates
has apparently increased the plastic viscosity. Controversially, Sami in the drilling fluid. Hydrate formation is a crystallization and exo-
(2015) showed that an increase in the concentration of magnesium ions thermic process. The occurrence of a sudden rise in temperature and
decreases both the plastic viscosity and apparent viscosity in water- drop in pressure during the experiment was the indication of the nu-
based drilling fluid. Bourgoyne et al. (1986) described this effect based cleation of hydrates and time taken from the start of the experiment till
upon the concentration of contamination. Initially, at low contamina- the nucleation of hydrate was defined as induction time.
tion (from formation water and sea water) the rheological properties The same steps as described in the experimental procedure were
(i.e. viscosity and yield point) tend to increase due to flocculation of the followed to perform the experiment. The DF-3 was charged into the cell
bentonite but at high concentration of contamination (from drilling of to understand the hydrate inhibition studies. Fig. 8 shows the time,
salt domes/anhydrides), additional precipitation of clay was observed pressure and temperature plot of the experiment. Even though there
which makes the drilling fluid to lose its properties. Kelland et al. was a slight reduction in pressure which indicates the dissolution of
(2008) described that the adsorption of xanthan gum over the clay methane gas, there was no either sudden drastic drop in pressure or rise
surface has reduced the interactions with the calcium ions and in temperature and the plots were almost parallel indicating no

Table 10
Rheological properties of DF-3 at different concentration of contaminants.

Notation τo (Pa) K (Pa sn) n PV (mPa s) YP (Pa) AV (mPa s) FL (ml) YP/PV Ratio (1000 s− 1) Gel (10 s/10 m) (Pa/Pa)

C-0 1.326 1.321 0.426 12 13.4 26 9.3 1.117 4.3/5.74

C-1 2.07 0.94 0.485 14 13.88 28.5 10 0.991 4.3/6.22
C-2 2.28 0.975 0.481 15 13.4 29 10.5 0.893 4.3/6.22
C-3 2.21 1.08 0.47 15 13.88 30 10.5 0.925 4.3/6.22

217
M. Srungavarapu et al. Applied Clay Science 152 (2018) 211–220

25 20 10 20
Temperature Temperature
Pressure 18 Pressure 18
20
16 16

14 14

Temperature (°C)
Temperature (°C)

Pressure (MPa)
Pressure (MPa)
15
12 12
5
10 10 10

8 8
5
6 6

4 4
0
0
2 2

-5 0 0
0 200 400 600 800 1000 1200 0 200 400 600 800 1000 1200
Time (min) Time (min)
Fig. 8. Static hydrate inhibition test for DF - 3. Fig. 10. Static hydrate inhibition test of DF-3 at 66.6 v/v% water cut.

formation of hydrates during the duration of 1100 min. This was also
confirmed by the visual examination after the completion of the ex-
periment. This was the indication of the drilling mud inhibiting the
formation of hydrate.
Well, kick is unscheduled, unwanted entry of the formation fluids
into the wellbore. Low mud level while drilling, piston effect while
tripping the drill string, drilling to highly porous and permeable rocks,
drilling through abnormal pore pressure zones causes the formation
fluids to enter the wellbore allowing them to mix with the drilling fluid
causing undesirable changes in the drilling fluid (Taylor and Lilly,
1983). Tan et al. (2005) described that the gasification of mud while
drilling results in fall of hydrostatic pressure causing a further influx of
formation fluids (gas and water) into the wellbore. Ning et al. (2010)
shown increased tendency of formation of hydrates in oil-based drilling
with increased water cut due to increase in nucleation sites and a de-
crease in critical radius of nucleation. To simulate the effect of the
formation water the DF-3 and artificial sea water were mixed in the
ratio of 2:1 indicating the water cut of 33.3%. This resultant sample of
volume 120 cm3 was again charged into the cell for static hydrate
studies. The same initial conditions of 0 °C and 16.55 MPa were
maintained to understand the inhibition effect of hydrate formation
under static conditions. Fig. 9 shows a plot of temperature, pressure and
time. Similar to the previous experiment there was no drastic pressure
drop or either sudden increase in temperature for the duration of
25
Temperature
Pressure
20
Temperature (°C)
1100 min. It has been found that even at 33.3% water cut, the drilling
fluid (and artificial sea water) has shown good inhibition properties at
static conditions. Likewise, there was the only absorption of gas into the
drilling mud and even with visual inspection after the experiment, there
was no formation of hydrate crystals in the solution.
Further, DF-3 was mixed with formation water in the ratio of 1:2
indicating the water cut of 66.6%. This resultant sample of volume
120 cm3 was again charged into the cell hydrate studies. The same
initial conditions of 0 °C and 16.55 MPa were maintained to understand
the inhibition effect of hydrate formation under static and dynamic
conditions.
Fig. 10 shows a plot of temperature, pressure and time under static
conditions. It was clearly evident that initially, pressure decreased till
104 min was due to the initial dissolution of natural gas which is de-
fined as gas solution time. A sudden change in pressure-slope at
104 min indicates the hydrate formation. Till 1000 min the pressure
slope has constantly changed within the period 104–228 min,
228–743 min and 743–1000 min of indicating the rate of growth of
hydrate was not constant due to stochastic nature of hydrate formation.
At 1015 min it was observed that the partial dissociation has hap-
pened, re-growth of hydrates from 1036 min to 1096 min. Interestingly,
two depressions obtained in the pressure curve were exactly at 1005 psi
(6.93 MPa) at 1015 and 1096 min respectively. The bentonite is the
promoter of formation of hydrates due to large nucleation sites it pro-
vides for hydrate formation while the salt is an inhibitor because it
reduces the availability of water molecules for hydrate formation.
20
Formation of hydrate by methane gas and water expelled the salt in the
18 solution resulting in the formation of the high concentration of salt in
the remaining solution. As the concentration of the salt increased, it
16
shifted the equilibrium line towards the high pressure and low tem-
14 perature side. When the pressure in the system has reached to 1005 psi

Pressure (MPa)

15
12
(6.93 MPa) the phase equilibrium line would have shifted to the point
where hydrate phase was not possible to exist and hence a temporary
10 10 dissociation has happened resulting in the pressure increase. The re-
8
growth of the hydrate showed that above 1005 psi (6.93 MPa) the
5
system temperature and pressure was well within the stability phase
6 equilibrium. Upon observation, at static conditions barite was found to
4
be majorly settled at the bottom layer due to low gel strength leaving
0 sea-water, bentonite, and polymer in the solution. The dissolution of
2 the gas had readily happened in the test solution which may have
-5 0
caused the formation of hydrates. Fig. 11 shows the formation of the
0 200 400 600 800 1000 1200 hydrate in the drilling mud.
Time (min) Further again, DF-3 was mixed with artificial sea water in the ratio
of 1:2 (66.6 v/v% water cut) was subjected to dynamic study with the
Fig. 9. Static hydrate inhibition test of DF-3 at 33.3 v/v% water cut. rotation of the magnetic stirrer at 1000 RPM to reduce the stochastic

218
M. Srungavarapu et al. Applied Clay Science 152 (2018) 211–220

nucleation and crystal growth. Fig. 13 shows the DF-3 (along with
66.6 v/v% water cut) immediately after the experiment which showed
absence of gas hydrate in the test sample.
Makogon and Holditch (2001) shown that with hydrate volume
formed under the static conditions was greater than the volume formed
under dynamic conditions even with the use of inhibitor reagent in
natural gas and salt water system. This was due to the formation of
microcrystals as a film at the gas-water interface which was weak and
permeable causing water molecules without inhibitor easily diffused
through the film and into the gas phase where the hydrate crystals grew
rapidly. Whereas in dynamic conditions, inhibitor quickly adsorbed to
the surface of the microcrystal and prevented further growth. The si-
milar effect can be explained in the experiments above for the static and
dynamic states with the formation of microcrystals of the gas-water
interface in a static condition causing diffusion of water molecules
through it and quick adsorption of polymer on any nucleated crystal in
Fig. 11. Red circle shows the formation of hydrate in the drilling mud within the auto- dynamic state may have prevented the growth resulting in low pressure
clave for DF-3 at 66.6 v/v% water cut at static conditions. (For interpretation of the re- drop.
ferences to colour in this figure legend, the reader is referred to the web version of this
The inhibition activity of both CMC and XG has been compared with
article.)
the existing kinetic hydrate inhibitors (KHI's). The KHI's show the
properties of higher inhibition in dynamic conditions as compared to
20 20 static conditions (Rogers, 2015). When compared, the inhibition
Temperature
Pressure 18 properties shown by CMC and XG differed under static and dynamic
conditions. To an extent, this can be attributed to the mechanism of
15 16 inhibition which can be different than that of current KHI's.
14
Temperature (°C)

Pressure (MPa)

10 12 4. Conclusions
10
The rheology study of the drilling fluid was studied along with the
5 8 influence of Carboxymethyl Cellulose and Xanthan Gum. Further, the
6 change in rheology was also studied at low temperatures and high
pressures for DF-3. Additionally, hydrate inhibition studies was also
0 4 carried out with the DF-3 along with consideration of water en-
2
croachment. Following conclusions may be drawn from this research
study.
-5 0
0 200 400 600 800 1000 1200
1. The CMC-based drilling fluid has shown the behavior of the power-
Time (min) law but along with xanthan gum, it showed Herschel-Bulkley
nature. With the decrease in temperature, DF-3 has shown an in-
Fig. 12. Dynamic hydrate inhibition test of DF-3 at 66.6 v/v% water cut.
crease in yield stress, plastic viscosity, yield point, apparent visc-
osity and flow index. Similarly, with an increase in pressure, DF-3
has shown an increase in yield stress, plastic viscosity, yield point,
apparent viscosity and a decrease in flow index.
2. The gel strength, apparent viscosity, yield point and plastic viscosity
increased with the increase in contamination by calcium and mag-
nesium ions but the rheological change was minimum under the
concentration found in sea water and formation fluids.
3. Xanthan gum and Carboxymethyl cellulose has shown the hydrate
inhibition nature both static and dynamic conditions but whereas
the inhibition mechanism might be different due to difference in
inhibiting pattern in both static and dynamic study. With the in-
crease in water content i.e. kick into the drilling fluid has increased
the chances of the formation of hydrates. However the drilling fluid
under dynamic study was less affected by the hydrate formation
than static study due to active adsorption of polymer under dynamic
Fig. 13. DF-3 with 66.6 v/v% water cut at dynamic test shows absence of any hydrate
crystals.
state.

nature and to understand the hydrate inhibition of the drilling fluid.
Fig. 12 is the time, temperature, pressure relation under dynamic
conditions. It can be clearly seen that the pressure and temperature
plots were almost parallel to each other throughout the experiment.
Upon visual examination, no presence of the hydrate formation ob-
served and sample was steerable. It was evident that the XG and CMC
have shown certain hydrate inhibition properties which restricted the
Acknowledgement
The authors gratefully acknowledge the financial support given by
the Earth System Science Organization, Ministry of Earth Sciences,
Government of India (MoES/36/OOIS/Extra/65/2016), to conduct this
research. Authors would also like to acknowledge M. Natarajan and V.
Chauhan for XRD analysis of bentonite clay at IRS, ONGC, Ahmedabad.

219
M. Srungavarapu et al.
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