Cementing Drilling Muds Monitoring Deepwater Wellbore

Smart Cementing Materials and Drilling Muds
for Real Time Monitoring of Deepwater

Wellbore Enhancement
RPSEA Ultra-Deepwater Program
Final Report – PHASE 1

(Rheological Properties, New Slurries with Fluid Loss Properties, New Slurries with enhanced
Sensing and Reduced Fluid Loss Properties)
Project No. 10121-4501-01
C. Vipulanandan and R. Krishnamoorti

Center for Innovative Grouting Materials and
Technology (CIGMAT)
University of Houston
June 2013
Project 10121-4501-01 / UH-CIGMAT 1 Final Report PHASE 1

Table of Contents
Page
Table of Contents.................................................................................................................... 2
Abstract…………………....................................................................................................... 3
1. Introduction..……………...................................................................................................... 3
2. Objectives..……………...................................................................................................... 10
3. Theory and Concept……...................................................................................................... 10
4. Materials and Methods..….................................................................................................... 11
4.1 Oil Well Cement……………………………………………………………………. 11
4.2 Drilling Muds………………………………………………………………………. 14
5. Results and Discussion..….................................................................................................... 16
5.1 Smart Cement……………………………………………………………………. 17
5.2 Smart Drilling Muds………………………………………………………………… 32
6. Conclusions………………………………………………………………………………... 51
7. Bibliography ….…………………………………………………………………………… 52

ABSTRACT
In this study, series of experiments were performed to evaluate the behavior of oil well
cements and drilling mud with and without modifications. For the cement, tests were performed
from the time of mixing to hardened state behavior. During the initial setting of the cement, the
electrical resistivity changed with time based on the type and amount of additives used in the
cement. During the curing of the cement, initial resistivity reduced by about 10% to reach a
minimum resistance and maximum change in resistance within the first 24 hours of curing varied
from 50 to 300%. Effect of adding silica fume, bentonite, barite and fly ash with and without
carbon fibers to cement hydration and changes in resistivity have been quantified. Based on the
current study, a new quantification concept has been developed to characterize the curing of the
cement based on the changes in the electrical resistivity in the first 24 hours of curing. When the
cement was modified with less than 0.1% of carbon fibers, the piezoresistive behavior of the
hardened cement was substantially improved without affecting the rheological properties and
setting properties of the cement. For the carbon fiber modified smart cement, the resistivity
change at peak stress was about 400 times higher than the change in the strain. Addition of metal
nanoparticles such as iron and nickel also improved the piezoresistive behavior of hardened
cement compared to the multiwall nano-carbon tubes. Effect of several additives on controlling
the water loss in the cement has been quantified. Also the effect of temperature on the curing and
hardened carbon fiber modified cement behavior was also investigated. Contamination of the
cement slurry with bentonite (drilling mud) can be detected based on the increase in the
resistivity of the cement. Change in bentonite content in the water based drilling mud was
sensitive to the changes in electrical resistivity. When the bentonite content in the drilling mud
was changed from 2% to 6% the resistivity reduced by 40%. Contamination of the water based
drilling mud with salt can be detected based ton the reduction in resistivity. Addition of up to
0.2% carbon fiber, with and without surfactants, also made the oil based drilling mud and
synthetic drilling mud sensitive to the resistivity. Several additives have been tested to reduce the
fluid loss in all types of drilling muds.
Hence electrical resistivity can be used as the sensing properties for both cement and
drilling mud. Addition of up to 0.2% carbon fibers made the smart cement and smart drilling
mud with relatively high sensing properties to monitor the performance. For example, since the
resistivity of water based 6% bentonite drilling mud is over 400% higher than the initial
resistivity of cement slurry, movement of the drilling mud and cement can be identified during
the installation of the oil well. Selecting electrical resistivity as the monitoring parameter unifies
the data collection process during the installation and the entire service life of the oil wells.
1. INTRODUCTION
As Deepwater exploration and production of oil and gas expands around the world, there
are unique challenges in well construction beginning at the seafloor. Also preventing the loss of
fluids to the formations and proper well cementing have become critical issues in well
construction to ensure wellbore integrity because of varying downhole conditions (Labibzadeh et
al. 2010; Eoff et al. 2009; Ravi et al. 2007; Gill et al. 2005; Fuller et al. 2002). Moreover the
environmental friendliness of the mud and cements is a critical issue that is becoming
increasingly important (Durand et al. 1995; Thaemlitz et al. 1999; Dom et al. 2007). Lack of mud
and cement returns may compromise the casing support and excess cement returns cause

problems with flow and control lines (Ravi et al. 2007; Gill et al. 2005; Fuller et al. 2002). Hence
there is a need for minimizing fluid losses by proper placement and monitoring of the drilling
mud and cementing operation in real time. Unexpected fluid losses could be addressed real-time
by changing the compositions of the drilling mud and/or cement slurry if real-time monitoring
becomes available.
Successful deepwater cementing requires minimum fluid loss with drilling mud and
cement slurry unit weights compatible with the formation (Eoff et al. 2009; Griffith et al. 1997).
There are number of challenges associated with installation of casings in deepwater. The
challenges include low fracture gradients resulting from young unconsolidated sands and shallow
drilling hazards such as shallow water flows or hydrate formations, bottom-hole temperature and
pressure, rapidly varying geological formations, fluid loss and no real-time monitoring of the
operations. Recent case studies in the Gulf of Mexico (GOM) have documented using specially
formulated lightweight foamed cement slurry to avoid cement sheath damage caused by shallow-
water flow. At present there is no technology available to monitor the cementing operation real
time from the time of placement through the entire service life of the borehole. Also there is no
reliable method to determine the length of the competent cement supporting the casing.
1.1 OIL WELL CEMENT
Oil well cementing is done to provide a protective seal to the casing, prevent lost
circulation and blowout and to promote zonal isolation. The standards of API suggest the
chemical requirements determined by ASTM procedures and physical requirements determined
in accordance with procedures outlined in API RP 10B and ASTM. There are several classes of
cements which could be used for oil well cementing.
Cement slurry flow ability and stability are the major requirements of oil well cementing.
Oil-well cements (OWCs) are usually made from Portland cement clinker or from blended
hydraulic cements. OWCs are classified into grades based upon their Ca3AlnOp (Tricalcium
Aluminate – C3A) content: Ordinary (O), Moderate Sulphate Resistant (MSR), and High
Sulphate Resistant (HSR). Each class is applicable for a certain range of well depth, temperature,
pressure, and sulphate environments. OWCs usually have lower C3A contents, are coarsely
ground, and may contain friction-reducing additives and special retarders such as starch and/or
sugars in addition to or in place of gypsum.
Cements such as class G and class H, considered to be two of the popular cements, are
used in oil well cementing applications. These cements are produced by pulverizing clinker
consisting essentially of calcium silicates (CanSimOp) with the addition of calcium sulphate
(CaSO4) (John, 1992). Class H cement is produced by a similar process, except that the clinker
and gypsum are ground relatively coarser than for a Class G cement, to give a cement with a
surface area generally in the range 220-300 m2/kg (John, 1992). Cementing is an important
operation at the time of oil well construction (Backe et al., 1997). When admixtures are added
with cement, tensile and flexural properties will be modified. Also admixtures will have effect on
the rheological, corrosion resistance, shrinkage, thermal conductivity, specific heat, electrical
conductivity and absorbing (heat and energy) properties of oil well cement (Bao-guo, 2008). Oil
well cement slurry is used several thousand feet below the ground level and hence determining
cement setting time is always a challenge.

Table 1. Composition of Cements (Zhang, 2010, Zhou,1996 & John, 1992)
Type of Surface area
Cement C3S C2 S C3 A C4AF Gypsum (m2/kg)
Class H 52-64 16-24 0.6-3 11-15 1.8 220-300
Class G 56-58 18-19 1-2 11-15 -- 270-350
Portland
Cement 50 25 12 8 3.5 320 - 380
C3S – Tricalcium silicate; C2S – dicalcium silicate; C4AF –Tetracalcium aluminoferrite
1.1.1 Modifiers: Modifiers (additives) are used in cement slurry could to control the flowability,
setting properties and enhance the solidified behavior. Typical modifiers used in OWC slurries
can be categorized as follows:
a. Setting time and thickening time altering additives: The setting time can usually be increased
by reducing the proportions tricalcium aluminate (C3A). Accurate control of the thickening time,
the time after initial mixing at which the cement can no longer be pumped, is crucial in the oil
well cementing process. The thickening time is usually controlled by using retarders. The
addition of carbohydrates such as sucrose can significantly extend the thickening time or even
prevent setting completely. Other retarders used in well cementing include cellulose derivatives,
organophosphates and inorganic compounds. The thickening time of OWC slurries was also
found to increase with the addition of polyvinyl alcohol (PVA) latex. Ligno-sulfonates and
hydroxyl carboxylic acids are retarders that have been used with OWCs. Salts of carbonates,
aluminates, nitrates, sulphates, thiosulphates, as well as alkaline bases such as NaOH, KOH,
NH4OH have been used to accelerate the setting time.
b. Weighting agents: Density altering additives (weighting agents or extenders) are used to achieve
specific density requirements. Weighting agents add weight to the slurry to achieve higher
density, while extenders are low specific gravity materials that are used to reduce the slurry
density and to increase slurry yield. For instance, Barite, sand and microsand have relatively high
specific gravity and are finely divided solid materials used to increase the density of OWC
slurry. Barite (BaSO4) is the most commonly available weighting agent in oil/ gas well
cementing. Hematite, calcium carbonate, siderite, limonite, manganese tetraoxide, sand and
micro-sand are other types of weighting agents used in cement slurries. Also bentonite is used to
avoid segregation of heavy constituents of cement slurry.
c. Additives to enhance mechanical properties: The compressive strength and the shear bond
strength were modified with the addition of salts and metal oxides. An increase in flexural
strength and in energy absorption before fracture was achieved by incorporating relatively small
amounts of polymer latex together with short fibers. Various types of polymeric and glass fibers
have been used to modify the solidified cement properties.
d. Other Extenders: Bentonite helps in fluid loss control but the hardened cement sheath becomes
less resistant to corrosive fluids due to permeability issues. Fly ash resists corrosive fluids.
Sodium silicates provide sufficient viscosity to allow the use of large quantities of mix water
without excessive free water separation. Silica fumes aids in obtaining low-density cement
systems with a high rate of compressive strength development and improves fluid loss control.
Foaming agents are used to reduce the modulus and permeability. Surfactants are used improve
the flowability and wetability of the cement slurry.
1.1.2 PIEZORESISTIVE BEHAVIOR

Banthia (1994) observed that strength and durability of concrete was improved by the
addition of small amounts of fiber-reinforcement. Due to the fiber’s high resistance to wear, heat,
and corrosion, carbon fiber-reinforced concrete in particular has been shown to have excellent
durability properties. Also, Chung (1996) reported that addition of carbon fiber to cement
provided the strain-sensing ability and increased the tensile and flexural strengths, tensile
ductility and flexural toughness, and decreased the drying shrinkage.
Chung (2001) studied that an increase of the measured electrical resistivity of carbon
fiber-reinforced cement paste during resistivity measurement was induced by electric
polarization. By increasing the conductivity of the cement paste through the use of carbon fibers
that were more crystalline, the increase of the fiber content, or the use of silica fume instead of
latex as an admixture, this effect can be diminished. The conductivity of the composite and the
Table 2. Literature review on piezoresistive studies
Modificat- Resistivity
Reference Materials Tests Result Remarks
ion change
Compressive,
Compressive, Ultrasonic
Cement, tensile strengths
Chung et al. Fiber of tensile and waves effect on
silica -- increased,
(2008) size 5mm flexural improving the
fume flexural strength
strength dispersion
decreased
Resistivity
4% of change was
Vipulanandan Portland Piezoresistive
Short Compressive more than 30 Compressive
& Garas Cement, properties
carbon test times the strain. strength modified
(2005) sand changed
fiber Less than 100
Ω.cm at 4% CF
Cement,
0.6% of Tensile strength
Reza et al. silica Tensile Tensile strength
carbon -- increased by 3
(2004) fume, strength test increased
fiber times
sand
6% of Resistivity
Tensile
Vipulanandan Polyester Short Tensile change was Tensile strength
properties
& Sett (2004) resin, sand carbon strength test more than 50 modified
changed
fiber times the strain.
Cement,
Manuela & 0.15% of Hydration time, Curing effect on
sand, Setting time Conductivity
Raffaele carbon percolation, conductivity was
silica test 0.1 (Ω.cm)-1
(2004) fiber curing studied
fume
Cement, 0.5 & 1% Thermo The linearity
Chung et al. The see back
latex, carbon electric power -- and reversibility
(1999) effect increased
silica fiber measurement of the see back

fume & see back effect is
coefficient increased
Cement, 0.5% Tensile strength Studied the effect
Chung et al. Tensile
silica carbon 3x10e-05 Ω.m increased by of water reducing
(1999) strength test
fume fiber 56% agent
2.6 to Electric
5.91x10e-04 to
Chung et al. Cement & 7.4% Tensile resistance Tensile strength
1.86x10e-04
(1999) water carbon strength test increased upon was sensed
Ω.m
fiber tension
Value of
electrical conductivity was
Cement,
conductivity increased to a
Abo El-Enein sand and
- - - was influenced peak at 1-3 hours
et al. (1995) silica
by addition of of hydration and
fume
silica fume then decreased
gradually
Cement, Mechanical
Carbon Compressive,
silica are Resistivity is properties of Adding carbon
fiber of tensile and
mostly varied from cement slurry fibers made the
Remarks 0.125% to flexural tests
used as 3x10e-05 to 100 are increased materials
7.4% is are mainly
base Ω.cm with addition of piezoresistive
used. done.
materials. fibers.
extent of polarization were increased by Intercalation of crystalline fibers. It was concluded that
when the four-probe method was used, voltage polarity switching effects were dominated by the
polarization of the sample itself, but when the two-probe method was used, voltage polarity
switching effects were dominated by the polarization at the contact sample interface.
Reza (2003) proved that with the addition of a small volume of carbon fibers into a
concrete mixture produced a strong and durable concrete and made the product as a smart
material. It is recommended that these techniques could be used as nondestructive testing
methods to assess the integrity of the composite.
Vipulanandan et al. (2004, 2005) studied the piezoresistive behavior of cementitious and
polymer composites. The studies showed that the changes in resistivity with the applied stress
were 30 to 50 times higher than the strain in the materials.
1.2 DRILLING MUDS

Drilling mud is used for cuttings removal, suspension of cuttings, release of cuttings at
seafloor, minimizing formation damage, reducing filtration rate, cooling and the lubrication of
the drill bit and drill string, buoyancy support of the drill string and corrosion prevention.
Drilling mud consists of two phases namely the liquid phase (water or oil) which is the base and
the solid phase which is the clay and additives.
In general, composition of drilling mud is selected based on the guidelines set by the
American Petroleum Institute (API). The drilling mud systems are broadly characterized as
water, oil and synthetic based muds.

(a) Water-based muds (WBM): The basic composition of water based muds is water, clay and
additive chemicals. The most common of clay used is bentonite and is frequently referred to as
‘gel’ in the oilfield applications. Gel likely makes reference to the fact that while the fluid is
being pumped, it can be very thin and free-flowing (like chocolate milk), though when pumping
is stopped, the static fluid builds a "gel" structure that resists flow. When an adequate pumping
force is applied to "break the gel", flow resumes and the fluid returns to its previously free-
flowing state. Many other chemicals like potassium salts are added to a WBM system to achieve
various effects, including: viscosity control, shale stability, enhance drilling rate of penetration,
cooling and lubricating of equipment.
(b) Oil based muds (OBM): These are classified as invert emulsion or oil-based muds.
(i). Oil-based muds: are formulated with only oil as the base/liquid phase and are often used as
coring fluids. These systems might pick up water from the formation but no additional water or
brine is added. Specialized oil-based mud additives include: emulsifiers and wetting agents
(commonly fatty acids and amine derivatives), high-molecular weight soaps, surfactants, amine
treated organic materials, organo clays and lime for alkalinity.
(ii). Invert emulsion muds: They are water-in-oil emulsions generally with calcium chloride
brine as the emulsified phase and oil as the continuous phase. They may contain as much as 50%
brine in the liquid phase. Concentration of additives and brine content/salinity are varied to
control rheological, filtration and emulsion stability.
(c) Synthetic oil based muds (SBM): Synthetic fluids are designed to perform like other oil
based muds, without causing environmental hazards. Primary types of synthetic fluids are esters,
ethers, polyalpha olefins and isomerized alpha olefins. They are environmentally friendly, can be
discharged offshore and are non-sheening and biodegradable.
Various types of modifiers (additives) have been used to enhance the performance of the
drilling mud as described below:
(i) MODIFIERS: Drilling mud is composed of many modifiers (additives) based on the
application and required property enhancements. The following section outlines the functionality
of the modifiers added to the drilling muds:
a. Enhance cutting, cleaning and minimize water loss: It is the basic requirements of
drilling mud. Bentonite is a clay material used for such applications. Its functions are to
reduce water seepage or filtration in to permeable formation, increase hole cleaning
capacity, form thin filter film of low permeability, provide hole stability in loose
formations, avoid or overcome loss of circulation. The suspension of bentonite clay must
be prepared in fresh water; brine can significantly affect its ability to minimize water
loss. Its dosage varies with the major purpose of its use.
b. Control density: Barite (BaSO4) is added to increase the density and specific gravity of
the mud in order to control formation pressure as unbalanced formation pressures will
cause an unexpected influx of pressure in the wellbore possibly leading to a blowout from

pressured formation fluids. Also Hematite (Fe2O3) and Galena (PbS) are used as
weighting additives to increase the specific gravity to achieve very heavy drilling muds.
c. Control Acidity and pH: Caustic soda (NaOH) is used to control the acidity of the mud.
Addition of NaOH increases the pH of the mud. But care must be taken while adding it to
water since NaOH with water reacts exothermically causing sudden increase in
temperature, increase in viscosity of the bentonite mud and decomposition of polymers.
(0.15% dosage). Also Caustic Potash (KOH) is used to increase pH of those muds which
are treated with potassium and also to solubilize lignite.
d. Viscosity modifiers: Sodium carboxymethyl cellulose (CMC) is used to increase

viscosity and reduce filtration loss. Its effectiveness decreases as concentration of salt in
mud increases. It is also used to thin those muds that are treated with calcium. Also Mica
is added to avoid loss circulation by plugging large gaps in rock formations. (dosage is
upto 5% depending on severity of loss circulation). Xanthan Gum is a water soluble
polysaccharides, produced by bacterial action on carbohydrates and is often used to
enhance the viscosity properties of the mud at low shear rates while not affecting the
flowability of the mud at high shear rates. This exceptional shear-thinning property is
unique to xanthan gums and does not get significantly affected by the presence of salt.
e. Control swelling of clay: Common salt is used in the form of brine solution for
inhibition to prevent swelling of clay in the production zone thus maintaining porosity
and permeability (dosage is 3% or more).
f. High temperature stabilizer: Lignite/Leonardite is used as a mild dispersant and thinner

to basically control the flow. It also provides high temperature stability (up to 260°C) and
acts as a deflocculant to reduce attraction between clay particles.
g. Control biological activities: Bactericide is added to prevent bio-degradation of natural

organic additives added to polymer muds such as the CMC and the Xanthan Gum.
h. Reduce foaming: foaming agents added to reduce the foaming action of the mud and
therefore prevent the significant transport barrier to muds caused by the foams.
The quantity of modifiers used in the drilling mud will vary based on the drilling conditions.
But due to the complex nature of installing wells in the ultra deepwater it is critical to
monitor, in real time, the advancement of the fluid fronts (drilling mud and cement slurry) to
better control the fluid losses in various rock formations and to minimize the loss of fluids to
optimize the cementing operation. At present there is no direct real-time observation method
available to determine the location of the advancing cement slurry front in the borehole making
the casing installation very subjective and challenging. Also there is no reliable method to
determine the length of the competent cement supporting the casing and no real-time monitoring
of the cemented casing performance over the service life of the well.

2. OBJECTIVES
The overall objective of this research study was to develop smart drilling mud and smart
cement slurry (enhance sensing properties) that can be integrated with real-time monitoring of
the operations for improving the wellbore integrity.
The two objectives for the PHASE 1 (TASK 5) of the study are as follows:
(1) develop smart cement slurry (SCS) and smart drilling mud (SDM) with enhanced sensing
capabilities for real-time monitoring of the changes in electrical resistivity during installation
and service life of the well.
(2) control fluid loss by modifying the drilling mud and cement slurry without affecting the
sensing properties.
3. THEORY AND CONCEPTS
It was very critical to identify the sensing properties for the cement and drilling mud that
can be used to monitor the performance. After years of studies and based on the current study on
oil well cements and drilling muds, electrical resistivity () was selected as the sensing property
for both cements and drilling muds. This makes it unique since same monitoring system can be
used to evaluate the performance of the cement and drilling muds. Hence two parameters
(resistivity and change in resistivity) will be used to quantify the sensing properties as follows:
R =  (L/A) =  K ……………………………………………………..(1)
Where R = electrical resistance

L = Linear distance between the electrical resistance measuring points
A = effective cross sectional area
K = Calibration parameter is determined based on the resistance measurement method
Normalized change in resistivity with the changing conditions can be represented as follows:
/ = R/R ……………………………………………………………... (2)
In TASK 5 (PHASE 1) the sensitivity of the materials () to changes (composition,

curing, stress, fluid loss and temperature) has been quantified. Correlating the changes such as
composition, curing, stress, cracking, fluid loss and temperature to the resistivity () (Eqn. (1))
and change in resistivity () (Eqn. (2)) will support the monitoring of the material (cement and
drilling mud/fluid) behavior.

4. MATERIALS AND METHODS
4.1 Cement
In this study commercially available Class G and Class H oil well cements were used.
Representative compositions of the two cements are summarized in Table 1. Also a typical XRD
pattern of Class H cement is shown in Fig. 1, where major constituents of the cement have been
identified. Effect of carbon fiber modification to the cements with and without additives such as
silica fume, fly ash, bentonite, nanoparticles, meta-kaolin and water reducing agents were
investigated. Only selected results are included in this report.
(a) Sample Preparation

The samples were prepared in accordance with API standard. For the initial mixing, a
high speed propeller-type mixer was used. Varying amounts of carbon fibers (0.075% to 0.2%)
were added with the cement mix as base modification. Also various other additives were added
with respect to the desired result. Additives were added to the water in the mixer with the mixing
intervals of 20 s at 4000 rpm. Cement, water and additive were mixed at the speed of 4000 rpm
for 3 min and 35 seconds at the speed of 1200 rpm. The water/cement ratio in all formulation in
this study was varied from 0.38 to 0.44. Total of four wires were placed in the mold with two
wires on each side of the specimen (Fig. 3). The vertical distances between any two wires were
the same. Embedment depth of the conductive wire was 1 inch. In order to have consistent
result, at least three specimens were prepared for each type of mix.
Figure 1. Typical X-ray-Diffraction (XRD) Pattern for Class H Oil Well Cement

For setting time monitoring and compressive loading tests, cylinders with diameter of 2 inches
and a height of 4 inches were prepared. For quick results monitoring, two-probe method was
chosen. During the initial stages of setting, conductivity and API resistivity meters were used to
determine the curing cement resistivity and using Eqn. (1) the calibration parameter K was
obtained with time.
(b) Resistivity
(a) (b) (c)

Figure 2. Different instruments used for measuring the resistivity: (a) Conductivity meter,
(b) Soil resistivity meter (two and four probe), (c) Digital resistivity meter
(i) Conductivity Probe: Commercially available conductivity probe was used to measure the
conductivity (inverse of resistivity) of the fluids (Fig. 2(a)). In the case of cement, this meter was
used during the initial curing of the cement. The conductity measuring rang was from 0.1S/cm
to 1000 mS/cm representing a resistivity of 10,000 Ω.m to 0.1 Ω.m
(ii) Digital Resistivity Meter: This is used in the Petroleum industry to measure resistivity. It
measures resistivity in the range of 0.01 Ω.m to 400 Ω.m (Fig. 2(c))
(iii) Four and Two Probe Method: As shown in Fig 2(b), this device is used to measure the
resistivity of soils. In this study it was used to measure the resistivity of curing cement and
drilling mud. Measures resistivity in the range of 0.01 Ω.m to 1000 Ω.m (Fig. 2(b))
Specimen
Ohm-meter
Figure 3. Ohm-Meter with Typical Wire Placement in the Oil Well Cement Specimen

Two Wire Method: The standard ohm-meter was used to measure the resistance between any
two wires attached to the mold. The change in resistance was measured continuously using the
Hewlett Packard 34420A NanoVolt/Micro Ohm meter which has a least count of 1 μΩ for
electrical resistance. This configuration is first calibrated using the same liquid (cement slurry or
drilling mud) to determine the parameter K in Eqn. (1). Typical variation of parameter K with
time is shown in Fig. 4.
Figure 4. Typical Calibration for the parameter K in the Two Wire Method
(c) Viscosity
Standard viscometers, including Fann (high strain rate) and Brookfield (lower strain rate),
were used to quantify the viscous properties (yield point, plastic viscosity) of various cement and
drilling mud mixes. The viscometers were calibrated using several standard solutions.
(d) Setting Time

The Vicat setting test (ASTM C191) was used to determine the initial and ﬁnal setting
times for hydrating cementitious mixtures. It measures the change in the penetration depth of a
plunger with a diameter of 1.13±0.05 mm under a constant applied load (300 g) as increasing
structure formation acts to reduce the extent of penetration into the specimen. The test is used to
determine the initial and ﬁnal setting times at penetration depths of 25 mm and 0.5 mm
respectively.
(e) Curing Conditions

Specimens were cured at room condition (temperature of 23±2˚C) and at higher
temperatures (oven cured) based on the selected testing condition.

(f) Compression Test (ASTM C39)
The cylindrical specimen was capped and tested at a predetermined controlled
displacement rate. The dimension of the specimen was measured using a Vernier caliper. In
order to measure the strain, a commercially available extensiometer (accuracy of 0.001% strain)
was used. The change in resistance was monitored using the two probe method and the parameter
in Eqn. (2) was used relate the changes in resistivity to the applied stress.
(g) Fluid Loss

High pressure/High temperature (HPHT) device was used to study the effect of fluid loss
in the cement. Fluid loss was measured after 30s, 1 min, 5 min, 10 min, 15 min, 20 min and 30
minutes. The test was stopped when gas blow out was observed from the bottom part of the cell.
Gas blowout was determined by the increase in the pressure level in the bottom cell indicating
that the gas was flowing through the cement slurry to the bottom the test cylinder. Fluid loss
amount, blow out time and fluid loss rate were measured and compared at different applied
pressures.
4.2 Drilling Mud

(a) Water Based Mud (WBM):
This is one of the most widely used drilling mud. The current study is focused on
determining the sensing properties of the drilling muds with and without modifications.
(i) Bentonite Content

Based on the 72 data collected from the literature the amount of bentonite used in water based
drilling mud varied from 0.5% to 14% as shown in Fig. 5. The standard deviation, variance and
coefficient of variation (COV (%)) were 3.3, 10.6 and 66% respectively. Over 50% of the data
represented 1% to 8% of bentonite in the water based drilling fluid mud. Increasing the bentonite
content in the drilling mud increased the yield stress and the plastic viscosity of the mud.
20
Maximum=14%
15
Minium=0.5%
15 Average=5
11
σ=3.3
Frequency
σ2=10.8
10
8 8 Cov (%)=65.6
6 No.of Data=72
5 4 4
3 3 3
2 2 2
1
0
0
0.5 2 3 4 5 6 7 8 9 10 11 12 13 14 14+
Bentonite (%)
Figure 5. Histogram of bentonite used in drilling mud

(ii) Yield Stress (o)
More than 50 data on yield stress for water based drilling mud were collected from the literature
and the reported minimum and maximum values were 0 and 79 (lb/100ft2) respectively. The
standard deviation, variance and COV (%) were 13.7, 185 and 209% respectively (Fig. 6). Also
the experimental results from the current study are compared with data from literature in Fig. 6.
For the current study, the average o of drilling mud with 2%, 4% and 6% of bentonite content
were 6, 16 and 24 (lb/100ft2) receptively. Yield stress (o) of drilling mud increased by 120%
when the bentonite content changed from 2% to 4%. Also the yield stress (o) of the drilling mud
increased by 300% when the bentonite content increased from 2% to 6%.
90
80 Previous Studies Maximum=79 pa
Minium=0.0 pa
Yield Stress ( o) (pa)
70 Current Studies
Average=6.6 pa
60
σ=13.7 Ib/100ft2
50 Cov (%)=208.7
40 No.of Data=58
30
20
10
0
0 2 4 6 8 10 12 14 16
Bentonite (%)
Figure 6. Variation of Yield Stress with Percent of Bentonite in Drilling Fluid Mud
In this study several Wyoming bentonite contents (2%, 4%, 6% and 8%) mixed with
water were studied. Also a typical XRD pattern of the Wyoming bentonite used in this study is
shown in Fig. 6, where major constituents of the bentonite used in this study have been
identified.
(b) Oil Based Mud (OBM): Both mineral oil and vegetable oil were used in preparing oil based
drilling mud for this study. Also based on literature review, 4% of bentonite was added to the
mix. Also the amount of oil in the drilling mud was varied to investigate the sensing properties of
the OBM.
(c) Synthetic Fluid (SBF): Ester based synthetic fluids were used to study the behavior. The
ester in the drilling fluid was varied to investigate sensing parameters for the fluid.
(iii) Modifiers: Several modifiers including surfactants, carbon fibers and fluid loss reducing
agents (salts, gum), starch and barite were use in this study.

Figure 6. Typical X-ray-Diffraction (XRD) Pattern for the Bentonite (Poly Gel)
(b) Methods
Viscosity: FANN viscometer (strain rate of 512 and 1024 sec-1) and Brookfield viscometer were
used to characterize the drilling mud behavior with shearing strain rate.
Fluid Loss: Standard fluid loss device was used to quantify the fluid loss with time and pressure.
Resistivity: The same devices that were used to measure the resistivity of cement were used to
measure resistivity of the drilling mud/fluids.
5. RESULTS AND DISCUSSIONS
The main focus of this study was to enhance the sensing capabilities of the various types
cement slurries from the time of mixing to solidified state. Both Class H and Class G oil well
cements were used to demonstrate the potential of making the material more piezoresistive and
sensing without significantly affecting the rheological properties. Although several modified
cement slurries were studied only the performance of selected materials are presented. The test
results form the unmodified cement was used as the baseline for comparison. Also various types
of drilling muds were modified and tested to quantify the sensitivity of the changes.

5.1 Smart Cement
(a) Density
The average density of each cement mix were measured immediately after mixing. The
water-to- cement (w/c) ratio was 0.35. As summarized in Table 3, addition of 0.075% of carbon
fiber had minimal effect on the density. Also density of the cement slurries with 5% foam was
11% less than the normal oil well cement. Whereas density of cement slurry with 5% silicate was
2% higher than the density of normal oil well cement. This difference was because of the
relatively higher density of silicate and lower density of foam compared to water.
Table 4. Densities of oil well cement (class H) with different additives (kg/m3)
0% 0.075% Port-
Time in Carbon Carbon *1% *5% land *1% *5%
hours fiber fiber Foam Foam* cement Silicate Silicate Remarks
Densities
varied
0 2019 2026 2000 1805 1992 2032 2064
from 1805
to 2064
Additives
Water affected
Density
Carbon Water loss was density
Remarks Water loss was
fiber loss higher and water
(Curing at was higher Lowest lower Highest
reduced was than loss
room than with density than oil initial
the water very normal during
condition) carbon well density.
loss high oil well curing at
cement
cement room
condition.
*Percentage of foam/silicate based on the weight of cement
(a) Rheological Properties
The effect of different additives on plastic viscosity and yield point of API class H cement
slurries was studied. Additives include the following:
 bentonite
 barite
 silica fume
 fly ash

All additives were weighed by weight of cement. Standard API high speed mixer was used at
4000 and 1200 rpm to mix the slurries. Slurries were mixed without and with 0.1% carbon fiber
based on weight of cement (BOWC). FANN standard viscometer (strain rate of 512 and 1024
sec-1) was used to determine the shear stress – strain rate relationships for the various cement
mixes and the responses are shown in Fig. and Fig. .

Table 5. Effect of Carbon Fiber Addition on the Rheological Properties of Cement
Plastic Yield Point YP/PV Remarks

Composition Carbon Fiber Viscosity (PV) (YP) ratio
(BOWC) (cPs) (lb/100 tf^2)
0% CF 71 24.25 0.34 Minor changes in
38% w-c - No the plastic
0.1% CF 65 22.25 0.34 viscosity. Reduced
additive the YP.
0.2% CF 73 19.75 0.27
38% w-c - 0.5% 0% CF 86 118.5 1.38 Bentonite increased
the PV, YP and
Bentonite 0.1% CF 92 108.5 1.2 YP/PV ratio
0% CF 68 21 0.3 Barite reduced the
PV, YP and YP/PV
38% w-c - 4% Barite 0.6 ratio. Carbon fibers
0.1% CF 64 38 reversed the trends.
0% CF 88 47.75 0.55 Silica fume
38% w-c - 5% Silica increased the PV,
0.53
fume YP and YP/PV
0.1% CF 94 50.5 ratio
0% CF 67 39.25 0.58 Fly ash increased
38% w-c - 5% Fly the YP with and
Ash 0.6 without carbon
0.1% CF 85 51 fibers
Varied Additives with and
Mainly Varied from from without carbon
fibers had varying
Remarks 0.1% Varied from 21 to 118.5 0.27 to rheological
Carbon 65 to 94 cPs cPs 1.38 properties
Fiber
(i) Fibers
Carbon Fiber: The Bingham plastic relationships for cement with and without carbon fibers are
compared in Fig. 7. Addition of 0.2% carbon fiber to the cement slurry with a w/c ratio of 0.38
increased the plastic viscosity by 2 cps and reduced the yield point by 4.5 lb/100 ft2 (Table 5).
Also the ratio of YP/PV reduced from 0.34 to 0.27. With 0.1% carbon fiber the effects on the
rheological properties were less and the ratio of YP/PV remained unchanged.
(ii) Filers
Bentonite: The Bingham plastic relationship for cement with 0.5% bentonite is shown in Fig. 8.
Addition of 0.5% bentonite (also could be considered as contamination from the drilling mud)
increased both the plastic viscosity and yield point. Addition of 0.1% carbon fiber to the cement
slurry with 0.5% bentonite and a w/c ratio of 0.38 increased the plastic viscosity by 6 cps (Fig. 9)
and reduced the yield point by 10.5 lb/100 ft2 (Table 5 and Fig. 10). Also the ratio of YP/PV was
increased from 0.34 to 1.38 with the addition of 0.5% bentonite. With 0.1% carbon fiber ratio of
YP/PV was reduced.

Barite: The Bingham plastic relationship for cement with 4% barite is shown in Fig. 8. Addition
of 4% barite reduced both the plastic viscosity and yield point of the cement with w/c ratio of
0.38. Addition of 0.1% carbon fiber to the cement slurry with 4% barite and a w/c ratio of 0.38
reduced the plastic viscosity by 3 cps (Fig. 9) and reduced the yield point by 3 lb/100 ft2 (Table 5
and Fig. 10). Also the ratio of YP/PV was reduced from 0.34 to 0.3 with the addition of 4%
barite. Addition of 0.1% carbon fiber increased the ratio of YP/PV to 0.6 compared to the cement
only mix.
Silica fume: The Bingham plastic relationship for cement with 5% silica fume is shown in Fig.
8. Addition of 5% silica fume increased both the plastic viscosity and yield point of the cement
with w/c ratio of 0.38. Addition of 0.1% carbon fiber to the cement slurry with 5% silica fume
and a w/c ratio of 0.38 increased the plastic viscosity by 17 cps (Fig. 9) and the yield point by 24
lb/100 ft2 (Table 5 and Fig. 10). Also the ratio of YP/PV was increased from 0.34 to 0.55 with
the addition of 5% silica fume. Addition of 0.1% carbon fiber increased the ratio of YP/PV to
0.53 compared to the cement only mix.
Fly ash: The Bingham plastic relationship for cement with 5% fly ash is shown in Fig. 8.
Addition of 5% fly ash reduced both the plastic viscosity and but increased the yield point of the
cement with w/c ratio of 0.38. Addition of 0.1% carbon fiber to the cement slurry with 5% fly
ash and a w/c ratio of 0.38 increased the plastic viscosity by 18 cps (Fig. 9) and increased the
yield point by 12 lb/100 ft2 (Table 5 and Fig. 10). Also the ratio of YP/PV was increased from
0.34 to 0.58 with the addition of 5% fly ash. Addition of 0.1% carbon fiber increased the ratio of
YP/PV to 0.6 compared to the cement only mix.
Figure 7. Variation of Shear Stress- Strain Rate Bingham Relationships for Cement with
and without Carbon Fibers

Figure 8. Variation of Shear Stress- Strain Rate Bingham Relationships for Cement with
and without Carbon Fibers
Figure 9. Comparison of Plastic Viscosity with Admixtures and 0.1% Carbon Fibers

Figure 10. Comparison of Yield Point with Admixtures and 0.1% Carbon Fibers
(b) Setting Behavior
(i) Resistivity
Based on the current study and past experience of the researchers, the change in
resistivity with time can be represented as shown in Fig. 11. Hence several parameters can be
used in monitoring the curing (hardening process) of the cement. The parameters are initial
resistivity (initial), minimum resistivity (minimum), time to reach the minimum resistivity (tmin),
resistivity after 24 hours of curing (24) and percentage of maximum change in resistivity [(24-
min) /min]100%. The test results from various cement compositions are summarized in Table 6.
The initial resistivity of cement with w/c ratio of 0.38 and 0.44 were 0.98 Ω.m and 1.33 Ω.m, a
35% increase in the resistivity. Also the time to reach the minimum resistance was reduced by 30
minutes when the w/c ratio increased from 0.38 to 0.44. The maximum change in resistivity for
cement with w/c ratio of 0.38 and 0.44 were 67% and 306% respectively. These observed trends
clearly indicate the sensitivity of resistivity to the changes occurring in the curing of cement
(Table 6).
(i) Fibers
Carbon Fiber: Addition of 0.2% of carbon fiber (CF) to cement with w/c ratio of 0.38 reduced
the resistivity to 0.94 Ω.m, a 4% reduction from the neat cement with w/c ratio of 0.38. The
maximum change in resistivity in the first 24 hours with 0.2% CF was 52% and the time to reach
the minimum resistivity was 70 minutes. Addition of CF to the cement with a w/c ratio of 0.44
had minimal effect on the initial resistivity but reduced the maximum change in resistivity after
24 hours (Table 6).

(ii) Filers
Silica fume: With 10% silica fume and w/c ratio of 0.38, the initial resistivity was 1.11 Ω.m, a
13% increase in resistivity compared to the cement only mix. The time to research minimum
resistivity was 50 minutes and was not affected by the addition of up to 0.2% CF. The maximum
resistivity change was 87%. With and without CF, the observed trends were similar, hence
addition of carbon fibers had minimal effect on the curing of the cement with 10% silica fume.
Bentonite: With 2.5% bentonite and w/c ratio of 0.38, the initial resistivity was 1.26 Ω.m, a 28%
increase in resistivity compared to the cement only mix. Addition of 0.1% CF didn’t affect the
initial resistivity. The time to research minimum resistivity was 190 minutes and adding 0.1% CF
reduced it to 90 minutes. The maximum resistivity change was 120%. With 0.1% CF, the
maximum resistivity change was 214%. Hence adding carbon fibers influenced the resistivity of
the curing cement with 2.5% bentonite.
Barite: With 4% barite and w/c ratio of 0.38, the initial resistivity was 1.97 Ω.m, a 100%
increase in resistivity compared to the cement only mix. Addition of 0.1% CF reduced the intial
resistivity to 1.32 Ω.m. The time to research minimum resistivity was 40 minutes and was not
affected by the addition of 0.1% CF. The maximum resistivity change was 111% and with
carbon fiber addition it was 124%. Addition of carbon fiber influenced the resistivity changes in
the curing cement with 4% barite.
Fly ash: With 5% fly ash and w/c ratio of 0.38, the initial resistivity was 0.83 Ω.m, a 15%
reduction in resistivity compared to the cement only mix. Addition of 0.1% and 0.2% CF
increased the initial resistivity. The time to research minimum resistivity was 30 minutes and
adding CF didn’t affect the time to research the minimum resistivity. The maximum resistivity
change was 255%. With 0.1% and 0.2% of CF, the maximum resistivity change was reduced to
135% and 128% respectively.
 24
/min
initial
tmin 24
Curing Time (hrs.)
(hr)(Hr)
Figure 11. Typical resistivity–time relationship during the curing process

Table 6. Resistivity Change with Curing Time for Oil Well Cement (class H)
with different additives and Carbon Fibers
Initial Minimum 1Hour 24Hour

tmin [(24-min)
Mix proportions resistivity resistivity resistivity resistivity
(min) /min]100%
(Ω-m) min(Ω-m) (Ω-m) 24(Ω-m)
Cement (C) 0.98 0.86 70 0.87 1.43 67%

C+0.2%CF 0.94 0.85 70 0.88 1.30 52%
W/C=0.38 C+10%SF 1.11 0.94 50 1.01 1.75 87%
C+10%SF+0.1CF 1.08 0.96 50 0.96 1.84 91%
C+10%SF+0.2CF 1.08 0.98 50 1.00 1.79 82%
Cement (C) 1.33 1.06 40 1.13 4.30 306%
W/C=0.44
C+0.1%CF 1.30 1.20 40 1.26 2.66 121%
C+0.2%CF 1.32 1.04 70 1.23 2.26 118%
C+2.5%Bent 1.26 1.13 190 1.16 2.48 120%
C+2.5%Bent+
1.29 1.00 90 1.02 3.14 214%
0.1%CF
C+4%Barite 1.97 1.91 40 1.95 4.03 111%
C+4%Barite+
1.32 1.24 40 1.28 2.77 124%
W/C=0.38 0.1%CF
C+4%Barite+
1.37 1.28 50 1.30 2.70 112%
0.2%CF
C+5%FA 0.83 0.83 30 1.07 2.96 255%
C+5%FA+0.1%CF 0.89 0.82 30 0.83 1.93 135%
C+5%FA+0.2%CF 1.02 0.95 30 0.99 2.17 128%
(ii) Hydration of Cement

A high-performance semi-adiabatic calorimeter (P-CAL 1000, Calmetrix Inc.) was used to
record the temperature change during the hydration (7 days) of a Class H oil well cement with
different additives. The volume of the specimen tested was 1.64 L. As shown in Fig 12 and
summarize in Table 7, 0.075% carbon fiber with and without 0.075% Fe/Ni nanoparticles
reduced the peak temperature of the cement. Further addition of 1% biosurfactant reduced the
peak temperature by 21.5 ºF, and it also delayed the time to reach the peak temperature by 0.7 h.

Calorimeter
Figure 12. Hydration Temperature with Time for a Class H Oil Well Cement with
Different Additives Recorded using P-CAL 1000 Calorimeter
(Int: Internal temperature or hydration temperature; Ext: External temperature or room

temperature; CF: Carbon fiber; NP: Nanoparticle).
Table 7. Peak Temperature and Corresponding Time for a Class H Oil Well Cement
Hydration with Different Additives Recorded by P-CAL 100 Calorimeter
Peak Temperature
Additives (ºF) Peak Time (h)
With no Additive 171.7 20.5
With 0.075% Carbon Fiber 169.8 20.7
With 0.075% Carbon Fiber + 0.075%
Fe/Ni Nanoparticles 168.7 20.6
With 0.075% Carbon Fiber + 0.075%
Fe/Ni Nanoparticles + 1% Biosurfactant 150.2 21.2
Note: Water to Cement Ratio = 0.4. The weight percentage of carbon fiber, Fe/Ni nanoparticles
and biosurfactant was determined according to the weight of cement powder.
Based on Vicat needle test at room condition the initial setting time was determined to be after 6
hours and the final setting time was about 8 hours. As shown in Fig. 12 the cement continues to
hydrate beyond the experimentally determined setting time based on the Vicat needle test
(determined by hardness).
(i) Fibers
Carbon Fibers: Addition of 0.075% of carbon fibers to the cement with a w/c ratio of 0.4
reduced the peak temperature by about 2oF degrees and increased the time to peak reach the peak

temperature by 0.2 hr. Hence adding 0.075% carbon fiber (amount used in the piezo-resistive
studies) had minimal effect on the hydration process of the cement. This was also reflected in the
resistivity and changes in resistivity during the initial 24 hours of curing.
(ii) Nanoparticle
Fe/Ni Nanoparticle: Addition of 0.075% of Fe/Ni nanoparticles with 0.075% of carbon fibers
reduced the peak temperature by 3oF and the time by 0.1 hr. Hence addition of 0.075%
nanoparticles had minimal effect on the hydration of cement.
(iii) Surfactant
Biosurfactant: Addition of 1% of biosurfactant to the cement with o.o75% of Fe/Ni
Nanoparticles and 0.075% carbon fibers reduced the hydration temperature by 21.5oF degrees
and increased the time to reach the peak temperature by 0.7 hours. Hence addin the biosurfactant
affected the hydration of the cement.
(iii) Temperature Effect
All the materials were mixed at room temperature and cured at different temperatures with and
without capping the mold (Table 8). In this study, 10% of silica fume was added to the modified
oil well cement (0.1% carbon fibers). The specimens were placed in molds and cured at different
temperatures (room temperature and 60o C) and the electrical resistance was measured
continuously up to 6 hours.
Table 8. Testing Conditions for the Four Specimens
Specimen No. Testing Condition Remarks

1 Room temp (23oC) with cap Minimum moisture loss
2 Room temp (23oC) without cap Moisture loss at room
temperature
3 In the oven (60oC) with cap Effect of curing
temperature with
minimum moisture loss
4 In the oven (60oC) without cap Maximum moisture loss.
It was observed that specimens at higher temperature hardened after about 3 hours, compared to
specimens at room temperature which hardened after 6 hours. In Fig. 13, the time taken to reach
the minimum resistance are compared (represents the minimum resistivity as indicated in Fig.
11). The specimens cured at 60oC required almost half the time to reach the minimum resistivity
as compared to the room temperature cured specimens. Capped specimen at room condition took
more time as compared to 60oC, to reach the minimum resistance. Figure 14 shows the changes
in relative electrical resistivity ratio (R/Ro) after 6 hours. The change in resistivity ratio was
about four times higher for specimens cured at 60oC compared to the room temperature cured
specimens. Hence the electrical resistivity was sensitive to the changes in the curing temperature
of the modified oil well cement (with 0.1% carbon fibers).

Figure 13. Time to research minimum Figure 14. Change in electrical resistance
resistance for different conditions ratio after 6 hours
(c) Solid Behavior

Piezo-Resistive Behavior
(i) Fibers
Carbon Fiber: After 7 days of air curing, the specimen (w/c = 0.4) with 0.075% carbon content
(total weight of cement mix) was tested under compression loading. Typical change in resistivity
with compressive stress is shown in Fig. 15. The change in resistivity in the bulk material was
much higher than the strain response. For example, the change in bulk resistivity was 45% as
compared to a strain of 0.05%, at a compressive stress of 5 MPa. This shows the magnification
of the resistivity response of the modified cement with 0.075% of carbon fibers. The axial
compressive strain was about 0.2% at failure for the fiber modified cement and the resistivity
change was 80%. The resistivity change was about 400 times higher than the change in strain.
For 0.125% carbon fiber content specimen, the resistivity change response was different
where the resistivity initially reduced with applied compressive stress (Fig. 16). Once the crack
formed, may be due to cracking of the matrix between carbon fibers the change in resistivity
increased considerably. The specimen was tested after 7 days of specimen made. The percentage
change in resistivity at failure was around 150%, nearly double the amount observed with
0.075% fibers.
Carbon Fiber and Foam: Cement specimen with 5% of foam (based on cement content) and
0.075% of carbon fiber was tested under compressive loading after 28 days of curing at room
condition to quantify the piezoresistive behavior of the modified cement (Fig. 17). At a
compressive stress of 5 MPa the change in resistivity was about 8% while the axial strain was
about 0.06%. After formation of crack in the specimen, larger change in resistivity was observed.
As shown in the Fig. 17, percentage change in resistivity at the failure stress of 35 MPa was
around 60% as compared to the failure axial strain of 0.25%. Hence the carbon fiber
modification was also effective with the addition of foam.

Crack
CF - 0.075%
W/C - 0.4
Curing time - 7 days
Figure 15. Piezo-resistivity Behavior of Oil Well Cement with 0.075% CF
Crack
CF - 0.125%
W/C - 0.4
Figure 16. Piezo-resistivity Behavior of Oil Well Cement with 0.125% CF

Crack
CF - 0.075%
W/C - 0.4
Foam- 5%
Figure 17. Piezo-resistivity Behavior of Oil Well Cement with 0.075% CF & 5% Foam
(ii) Nanomaterials
Metal: Addition of Fe, Ni and Fe+Ni metal nanopatricles and multi-walled nanocarbon tubes
were studied. Addition of 0.075% of Ni nanoparticle also showed the piezoresistive response for
3 days cured cement (Fig. 18). Addition of Ni nano particles didn’t affect the compressive
strength of cement. At 1000 psi compressive stress, the change in resistivity was about 30%,
higher than what was observed with 0.075% carbon fibers (20%). Near failure stress the change
in resistivity was about 50% as compared to 80% for the carbon fiber modified cement (Fig. 18).
Multi-walled Nanotubes (MWNT): Addition of 0.075% of MWNT also showed the

piezoresistive response for 3 days cured cement (Fig. 19). Addition of MWNT did affect the
compressive strength of cement. At 1000 psi compressive stress, before failure, the change in
resistivity was about 11%, much lower than what was observed with 0.075% carbon fibers.

Strain
Figure 18. Piezo-resistivity Behavior of Oil Well Cement with 0.075% CF & 0.075% Ni
Nanoparticles
Figure 19. Piezo-resistivity Behavior of Oil Well Cement with 0.075% CF & 0.075%
MWNT

Temperature Effect
As shown in Fig 20, the compressive stress response of modified OWC with 0.075% CF added
and cured at room temperature and 200 ºF for 3 days curing time are compared. It was observed
that under 200 ºF, the compressive strength of the cement decreased while the change in the
resistivity with applied stress increased. At 1000 psi compressive stress the change in resistivity
were 20% and 80% at room temperature and 200oF respectively. Hence the carbon fiber
modification was effective at higher temperature. The failure resistivity of room temperature
cured specimen was about 80%.
Figure 20. Effect Temperature on the Piezo-resistivity Behavior of Oil Well Cement with
0.075% CF
(d) Fluid Loss
(i) Filers
The effect of bentonite and barite on the in fluid loss of a oil well cement was investigated at
various pressures. The bentonite and barite contents were varied up to 2.5% and 4% respectively.
Test results showed that increasing the pressure reduced the blowout time and increased the rate
of fluid loss (Table 9). Increased bentonite addition (or contamination) increased the blow out
time and decreased the fluid loss. Addition of 2.5% bentonite reduced the fluid loss rate by 76%
at 300 and 400 psi, 81% at 200 psi and 86% at 100 psi. Addition of 2.5% bentonite also
increased the blow out time by about 200% at all pressures. As shown in Fig. 21 o.5% bentonite
addition reduced the fluid loss rate by 69% to 48% when the pressure was increased from 100 to
400 psi. The 4% barite addition was comparable to the 0.5% bentonite addition as related to the
fluid loss but the blowout time was much lower (Fig. 22).

Figure 21. Total Fluid Loss with Varying Amounts of Bentonite and Barite with Pressure
Figure 22. Blowout Time with Varying Amounts of Bentonite and Barite with Pressure

Table 9. Effect of bentonite and barite on fluid loss properties of class H oil well cement,
w/c ratio 0.38.
Filtrate
Total Filtrate Blow out
Additive Pressure Rate Remarks
(mL) time (sec)
(mL/s)
Fluid loss varied
100 96 200 0.48
from 96 to 124
200 127 234 0.54 mL based on the
No Additives pressure
300 119 140 0.85
400 124 100 1.24
100 81 560 0.14
Fluid loss was
0.5% 200 89 260 0.34 reduced
Bentonite 300 105 210 0.50
400 103 160 0.64
100 68 1261 0.05
Lowest fluid
2.5% 200 76 711 0.11
loss. Longest
Bentonite 300 83 398 0.21 blowout time
400 87 300 0.29
100 89 255 0.35 Fluid loss similar
to 0.5%
4% Barite bentonite. Blow
400 103 80 1.29 out time was
much less
Varied Varied Bentonite was
Fluid loss more effective in
Pressure effect from 80 from 0.05
Remarks varied from reducing the fluid
on fluid loss to 1261 to 1.24
68 to 124 mL loss
sec. mL/s
5.2 Smart Drilling Muds/Fluids
The drilling mud and drilling fluids, with and without modifications, were characterized
base on the resistivity, rheological properties and fluid loss.
(i) Water Based

(a) Resistivity:
As shown in Fig. 23 and summarized in Table 10 the resistivity of the drilling mud
changed with bentonite content. Increase in the bentonite content decreased the resistivity. The
resistivity of 1% bentonite drilling mud was 10.4 Ω.m, which was 10 times (1000%) higher than
the initial resistivity of cement with w/c ratio of 0.38. This difference will help in the monitoring
of drilling mud displacement and cement injection during the installation of the casing in the oil
well.

Figure 23. Variation of Resistivity with Bentonite Content in the Water based Drilling Mud
Table 10. Resistivity Change with Bentonite Content in the Drilling Mud
Resistivity
Bentonite% (Ω.m) Remarks
0.25 15.1 Resistivity decreased
0.5 13.7 with increase in
1 10.4 bentonite content.
When the bentonite
1.5 9.1
content was increased
2 8.1 from 1% to 6% the
3 6.0 resistivity decreased by
4 5.5 about 60%
6 4.8
8 3.1
2% Bentonite: The resistivity was 8.1 Ω.m. Hence it was over 8 times (800%) higher than the
initial resistivity of cement with w/c ratio of 0.38.
4% Bentonite: The resistivity was 5.5 Ω.m. Hence it was over 5.5 times (550%) higher than the

6% Bentonite: The resistivity was 4.8 Ω.m. Hence it was over 4.8 times (480%) higher than the
(b) Rheological Properties

The shear stress versus shear strain rate ( 40 sec-1) was invesigated for 2, 4 and 6%
bentonite drilling muds. The shear strain rate was much lower than what is used in the FANN
viscometer (512 and 1024 sec-1).
2% bentonite: This is a shear thining drilling mud. When the shear strain rate was varied from 0
to 40 sec-1, the shear stress developed varied from about 3 to 9 pa and the relationship was
nonlinear (Fig. 24).
to 40 sec-1, the shear stress developed varied from about 9.5 to 18 pa and the relationship was
to 40 sec-1, the shear stress developed varied from about 15 to 45 pa and the relationship was
Figure 24. Shear Stress – Shear Strain Rate Relationship for 2% Bentonite Drilling Mud


(c) Modeling
The four conditions that need to be satisfied for as shear thinning drilling mud is as follows:
Condition 1:    o When   0. …………………………………………. (3)

d
Condition 2:  0 ………………………………………………………… (4)
d
d 2
Condition 3:  0 ……………………………………………………….. (5)
d 2
Condition 4:    ,    * ……………………………………………… (6)
The rheological models that were used to represent the drilling mud behavior are as follows:
(i) Herschel-Buckley Model (Modified Power Law)

The Bingham plastic model assumes a linear relationship between shear stress and shear strain
rate. However, a better representation for the shear thinning behavior of a drilling mud is to
consider the modified Power law relationship which is represented as follows:
    o  k1 ( ) n .......................................................................(7)
Hence verifying the conditions that needs to be satisfied.
d
 k1n *  ( n1)  0  kn  0 ………………………………. (8)
d
d 2
 k1[n(n  1)] *  ( n2)  k1n(n  1)  0
d 2
…………………… (9)
 (n  1)  0  n  1
This Model doesn’t satisfy Condition 4 (since when    *   ).

Where:
o: yield point (pa).
k1: is the consistency index (pa*secn).
n: is flow behavior index.
: is shear rate (sec-1).

* is the ultimate shear strength of the drilling mud (pa)
. The shear stress-strain rate predictions for 2%, 4% and 6% bentonite muds are compared in
Figs. 24, 25 and 26 respectively.
(ii) Casson Model

This model was originally developed for ink pigments but has been shown to give a good match
for some oil-based fluid systems (Ayeni 2003).
1 1 1 1
   o  k2 *  ……………………………………………….. (10)
2 2 2 2
1 1
1  2 d 1 1 
  k2 2 * *  2  0  k2  0
2 d 2
…………………………… (11)
d
2
1 1 1
  k2 2 3  0
d 2
2 2

This Model doesn’t satisfy Condition 4 (since when    *   ).
Where:
k2: model constant (
yield Stress (pa).
: shear Rate (sec-1).

1/ 2
A plot of versus gives an intercept of and a slope of k 2 . The parameters of this
model were obtained using non-linear regression analyses. This model combines a yield stress
with greater shear thinning behavior than the Bingham plastic model.
The shear stress-strain rate predictions for 2%, 4% and 6% bentonite muds are compared in Figs.
24, 25 and 26 respectively.

(iii) Hyperbolic Model (New Model Proposed)
The new hyperbolic model proposed is as follows:

  o  ……………………………………….. (12)
A  B *
d ( A  B )  B A
   A0
d ( A  B ) 2
( A  B ) 2
……………..(13)
d 2  AB
 B0
d 2
( A  B ) 2
   ,    * = o + 1/B ……………………………...(14)
Where:
o: yield stress.
A and B: are model parameters.
: is the shear rate (sec-1)
* is the ultimate shear strength of the drilling mud (pa)
The shear stress-strain rate predictions for 2%, 4% and 6% bentonite muds are compared in Figs.
24, 25 and 26 respectively.
(ii) Salt Contamination Effect
Rheological
Plastic viscosity, yield point, gel strength (10 second and 10 minutes), for a 6% (w/w) bentonite
mud with different percentage (0 to 0.3% w/w) of salt (NaCl) content was determined using the
FANN viscometer (Strain rates of 512 and 1024 sec-1). Results (Fig. 27) show the effect of salt
which reduced the plastic viscosity, yield point and gel strength of bentonite drilling mud. The
plastic viscosity was reduced by about 10%, yield point was reduced by about 35%, and gel
strength was reduced by about 22% with an addition of 0.1% salt.

(a)
(b)

(c)
Figure 27. Effect of salt on 6% Bentonite Mud (a) Plastic viscosity, (b) Yield point and (c)
Gel strength
(ii) Salt on the resistivity: The variation of resistivity with salt content is shown in Fig. 28 for
6% bentonite drilling mud. The electrical resistivity was sensitive to the salt content and an
addition of 0.1% (w/w) salt (also represent contamination) reduced the resistivity by 40%. Hence
resistivity will be a good sensing property to evaluate level of salt contamination in the drilling
mud.
(iii) Relationship between resistivity and plastic viscosity

A relationship between the resistivity and the plastic viscosity was determined from the
experimental data and shown in Fig. 29. Based on the limited data, a linear relationship is
proposed as follows:
μ = Aρ + B …………………………………………………(15)
Where, μ = Plastic viscosity (cP),

ρ = Resistivity (Ohm-m),
A and B are constants.
From this investigation, A was 3.74 (cP/Ohm-m) and B was 8.76 cP with the coefficient of
determination R2 = 0.97

Figure 28. Effect of salt on the Resistivity of 6% Bentonite Mud
30
Plastic Viscosity (cP)
25
20
15
2 2.5 3 3.5 4 4.5 5 5.5
Resistivity (Ohm-m)
Figure 29. Relationship between the Resistivity and the Plastic Viscosity 6% Bentonite
Mud

(b) Fluid Loss Behavior
Filter press testws performed with several additive but results with two additives xanthan
gum and corn starch are presenated. The results are shown. The amounts of additives used were
0.1%, 0.3% and 0.5% based on the amount of bentonite. The results presented are for 4%
bentonite drilling mud.
(i) Xanthan gum (C35H49O29)

The filter loss was measured every 2.5 minutes and the results are shown in Fig. 30 and
summarized in Table 11. The xanthan gum was very effective in reducing the fluid loss.
Addition of 0.5% Xanthan gum reduced the fluid loss from 180 mL to 24 mL about 80 %
reduction.
Figure 30. Fluid Loss with Time for 4% Bentonite Drilling Mud with Varying Amount of
Xanthan Gum (C35H49O29)
(ii) Corn Starch(C27H48O20)

The results are shown in Fig. 31 and summarized in Table 11. The corn starch was very
effective in reducing the fluid loss. Addition of 0.5% corn starch reduced the fluid loss from 180
mL to 22 mL about 80 % reduction.

Figure 31. Fluid Loss with Time for 4% Bentonite Drilling Mud with Varying Amount of
Corn Starch (C27H48O20)
(b) Resistivity
Xanthan Gum: The variation of resistivity with the addition of Xanthan gum in water is
compared in Fig. 32. With the addition of 0.1% and 0.50% Xanthan gum the resistivity reduced
by 18% and 50% respectively. Hence resistivity is good measure to determine the Xanthan gum
content in water.
Corn Starch: The variation of resistivity with the addition of corn starch in drilling mud is
compared in Fig. 33. With the addition of corn starch the resistivity reduced and was measurable.

Figure 32. Variation of Resistivity with the Addition of Xanthan Gum to Water
(Blue column (left column) stands for resistivity from conductivity meter
and brown column (right column) stands for resistivity by API machine)
Figure 33. Variation of Resistivity with the Addition of Corn Starch to 4%

Bentonite Drilling Mud (Blue column (right column) stands for resistivity
from conductivity meter and brown column (left column) stands for
resistivity by soil resistivity machine using four probe case)

Table 11. Fluid Loss with Xanthan and Corn Starch Additives in 4% Bentonite Drilling
Mud
Additive Filter Loss (mL) Remarks
Total Total
Pressure
Xanthan gum Bentonite Filtrate at Filtrate at End Time
(psi)
30 min the End
Filter loss was over in
No additive 4% 32 180 100
1 day
0.1% of Filter loss was over in
4% 21.25 31.5 100
Bentonite 100 min
4% 18 26.5 100
Bentonite 90 min
4% 17.5 24 100
Bentonite 50 min
Additive Filter Loss (mL) Remarks
Total Total
Pressure
Corn starch Bentonite Filtrate at Filtrate at End Time
(psi)
30 min the End
Filter loss was over in 1
No additive 4% 32 180 100
day
4% 22 100 100
Bentonite 2.5 hours
4% 20 25 100
Bentonite 85 min
4% 19.5 22 100
Bentonite 40 min
(ii) Oil Based Mud (OBM)
In this study, both mineral oil and vegetable oil were used in preparing the oil based drilling mud
with 4% bentonite (by wt.%). The ratio of Oil to water was varied from 4:1 (300mL:75mL) to
1:1.
(a) Resistivity
The resistivity of OBM with varying compositions and 0.1 % CF are shown in Fig. 34 and
summarized in Table 12. Reducing the oil content from 4:1 mix to 1:1 mix reduced the resistivity

100 times. The resistivity of 1:1 OBM was over 100 times higher than the initial resistivity of
cement with w/c ratio of 0.38.
Carbon Fiber: The resistivity of OBM (4:1) was 14,100 Ω-m and was reduced to 11,300 with
0.1 % CF addition.
Surfactant: Adding 1% of sodium dodecyl sulfate to the OBM (4:1) with 0.1% CF reduced the
resistivity to 6.3 Ω-m.
Figure 34. Variation of resistivity with Different Composition of OBM
Table 12. Resistivity of Various Composition of OBM with 0.1% CF

Composition Resistivity (Ω-m) Remarks
Oil: Water 4:1 11,300 Reducing the oil: water ratio

substantially reduced the resistivity.
Oil: Water 7:3 5,200
Oil: Water 5:5 113

Figure 35. Variation of Resistivity of OBM with O.1% Carbon Fiber and 1% Surfactant
Table 13. Resistivity of OBM with O.1% Carbon Fiber and 1% Surfactant
Composition Resistivity (Ω-m) Remarks
Oil: Water 4:1 14,100 Very high resistivity
Oil: Water 4:1 + 0.1% CF 11,300 Carbon Fiber reduced the resistivity
Oil: Water 4:1 + 0.1% CF + 6.3 Very large reduction in the resistivity with
1% SDS Surfactant the addition of a anionic surfactant
(b) Fluid Loss

Addition of salt reduced the fluid loss in OBM (Fig. 36). The ratio of mineral oil to water is 4:1
(300mL:75mL). Samples were mixing with 5% and 10% of NaCl. Increasing the salt content
from 5 to 10% reduced the fluid loss 300 mL to 150 mL, a 50% reduction in the fluid loss.
.

Figure 36. Fluid Loss of 4% Bentonite Oil Based Drilling Mud with Varying NaCl Contents
(iii) Synthetic Based Mud (SBM)
(a) Base Material
In this study, fatty acid methyl esters (FAME) were produced from by reacting alkali-catalyzed
vegetable oil (fats or fatty acids) with methanol.
(a) Resistivity
The resistivity of the SBM wa affected by the ester content. With increase in ester content
the resistivity increased (Fig. 37 and Table 14). The resistivity of SBM with 35% ester and 65%
water was about 25 Ω-m, 25 times higher than initial resistivity of cement with w/c ratio of 0.38.
Carbon Fiber: Addition of carbon fiber reduced the resistivity of SBM as shown in Fig. 37 and
summarized in Table 14. Addition of 0.1 to 0.2% CF reduced the resistivity by 10%.
(b) Rheological Properties
Viscosity ws measured using Baroid FANN Viscometer subjected to 300 rpm and 600 rpm.
Biosurfactant: The plastic viscosity was increased and the yield point was decreased with the
addition of surfactant to the SBM with 70% ester and 30% water (Fig. 38). A reduction in the
yield point helps in reducing the pressure required to bring the drilling fluid back into motion

from static condition which is a highly desirable property. Also increasing the biosurfactant
content decreased the YP/PV ratio.
Figure 37. Variation of Resistivity with Ester Content With and Without Carbon Fibers
Table 14. Variation of Resistivity with Ester Content With and Without Carbon Fibers
Ester/Water %CF Resistivity without Resistivity with Remarks

ratio CF (Ω-m) CF (Ω-m)
0/100 0.2 23.8 21.8 Resistivity
5/95 0.18 24.1 22.0 reduced about
11/88 0.17 24.6 21.9 8% with the
21/79 0.15 25.4 22.7 addition of up to
30/70 0.13 26.2 22.7 0.2% carbon
35/65 0.12 26.6 24.6 fiber.
Remarks Varied the CF Increased with Addition reduced Addition of
addition from increase in ester the resistivity Carbon Fibers
0.12 to 0.2% content reduced the
resistivity
Salt: As shown in Fig. 39, the ration of YP/PV of SBM (70:30) increased with increase in salt
content. When 1% biosurfactant was used it was effective in reducing the YP/PV ratio up to 5%
salt content. At higher salt content it increased the YP/PV ratio.

Figure 38. Variation of PV and YP with Biosurfactant Content in SBM
Figure 39. Variation of YP/PV ratio with Biosurfactant Content in SBM

6. CONCLUSIONS
Based on the experimental study in characterizing the modified smart cement and drilling
mud/fluid following conclusions are advanced.
(1) Material resistivity will be the sensing property selected to represent both cement slurry and
drilling mud/fluids. This selection will unify the real time monitoring, using the same
instruments, for both oil well cement and drilling mud.
(2) Resistivity was sensitive to the types and amount of additives used in the oil well cement and
drilling mud/fluid.
(3) Several resistivity parameters have been identify to characterize the curing of the oil well
cement. Changing the water-to-cement ratio from 0.38 to 0.44 increased the resistivity by
30% and reduced the time to reach the minimum resistivity by 30 minutes. During the curing
of the cement, initial resistivity reduced by about 10% to reach a minimum resistance and
maximum change in resistance within the first 24 hours of curing varied from 50 to 300%
(4) Addition of 0.1 % carbon fiber to the cement reduced the initial resistivity and made the
material piezoresistive. The resistivity change due to applied stresses was 30 to 80 times
higher than the change in the strain in the material, making the cement material smart and
sensing. Also the addition of 0.1% carbon fiber did not affect the rheological properties of
the cement. For the carbon fiber modified smart cement, the resistivity change at peak stress
was about 400 times higher than the change in the strain. Hence carbon fiber modified
cement will be used in Task 6 and Task 7 of this study.
(5) Addition of 0.1% of carbon fiber made the cement with other additives such as nanoparticle
and silica fume more piezoresistive.
(6) Contamination of the cement by bentonite can be detected based on the change in resistivity.
Bentonite reduced the fluid loss in cement.
(7) Resistivity changed with bentonite content in the water based drilling mud. When the
bentonite content in the drilling mud was changed from 2% to 6% the resistivity reduced by
40%. Salt contamination of the water based drilling mud can be determined based on the
reduction of resistivity. Xanthan gum and corn starch can be used to control the fluid loss in
the drilling mud.
(8) Since the resistivity of water based 6% bentonite drilling mud is over 400% higher than the
initial resistivity of cement slurry, movement of the drilling mud and cement can be
identified during the installation of the oil well.
(9) Resistivity changed substantially with the oil–to-water ratio in the oil based drilling mud.
Adding surfactant substantially reduced the resistivity of OBM.
(10) Resistivity changed with ester-to-water ratio and with the carbon fiber addition in the
synthetic based drilling mud.

7. BIBLIOGRAPHY
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Cements Exploration and Production Department, 22nd Edition.
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3. Caenn, R., Darley, H. C. H. and Gray, G. (2011) Composition and Properties of Drilling
and Completion Fluids, Gulf Publishing Company, Houston.
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5. Durand, C., T. Forsans, et al. (1995). "Influence of Clays on Borehole Stability - A
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Maintaining Hydrocarbon Flow, Journal of Petroleum Technology, pp. 28-30.
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14. Labibzadeh, M., Zhhabizadeh, B. and Khajehdezfuly, A., (2010) "Early Age
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Drilled Shafts Socketed in Clay Shale and Limestone, Journal of Geotechnical and
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Ash Grouts," Construction and Building Materials, Vol. 16, pp.353-363.
17. Ozgurel, G., Gonzalez, H. A. and Vipulanandan, C., (2005) "Two dimensional Model
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Proceedings, Pipelines 2005, ASCE, pp. 631-642.
18. Park, J., Vipulanandan, C., Kim, J. and Oh, M. H. (2006) "Effect of Surfactants and
Electrolyte Solutions on the Properties of Soils," Journal of Environmental Geology, Vol.
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19. Ravi, K. et al. (2007) "Comparative Study of mechanical Properties of Density-reduced
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Ridge, New Jersey, 628 pp.
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Nonlinear Models for Gelling and Maximum Curing Temperature Rise in Polymer
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25. Vipulanandan, C. and Nam, E. (2009), “Drilled Shaft Socketed in Uncemented Clay
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Penetrometer” Proceedings, Contemporary Topics in In Situ Testing, Analysis, and
Reliability of Foundations, Foundation Congress 2009, ASCE, GSP 186, pp. 119-126.
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Clayey Soils,” Proceedings, GeoCongress 2008, Geotechnics of Waste Management and
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Cement Mortar", Proceedings, Engineering, Construction and Operations in Challenging
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Piezoresistive Smart Structural Materials", Proceedings, Engineering, Construction and
Operations in Challenging Environments, Earth & Space 2004, ASCE Aerospace
Division, League City, TX, pp. 656-663.
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Cementing Drilling Muds Monitoring Deepwater Wellbore

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Cementing Drilling Muds Monitoring Deepwater Wellbore

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Smart Cementing Materials and Drilling Muds

for Real Time Monitoring of Deepwater

RPSEA Ultra-Deepwater Program

Final Report – PHASE 1

Project No. 10121-4501-01

C. Vipulanandan and R. Krishnamoorti

Project 10121-4501-01 / UH-CIGMAT 1 Final Report PHASE 1

3. Theory and Concept……...................................................................................................... 10

4. Materials and Methods..….................................................................................................... 11

4.1 Oil Well Cement……………………………………………………………………. 11

4.2 Drilling Muds………………………………………………………………………. 14

5. Results and Discussion..….................................................................................................... 16

5.1 Smart Cement……………………………………………………………………. 17

5.2 Smart Drilling Muds………………………………………………………………… 32

Project 10121-4501-01 / UH-CIGMAT 2 Final Report PHASE 1

Project 10121-4501-01 / UH-CIGMAT 3 Final Report PHASE 1

1.1 OIL WELL CEMENT

Project 10121-4501-01 / UH-CIGMAT 4 Final Report PHASE 1

Class H 52-64 16-24 0.6-3 11-15 1.8 220-300

Class G 56-58 18-19 1-2 11-15 -- 270-350

C3S – Tricalcium silicate; C2S – dicalcium silicate; C4AF –Tetracalcium aluminoferrite

1.1.2 PIEZORESISTIVE BEHAVIOR

Project 10121-4501-01 / UH-CIGMAT 6 Final Report PHASE 1

1.2 DRILLING MUDS

Project 10121-4501-01 / UH-CIGMAT 7 Final Report PHASE 1

Project 10121-4501-01 / UH-CIGMAT 8 Final Report PHASE 1

d. Viscosity modifiers: Sodium carboxymethyl cellulose (CMC) is used to increase

f. High temperature stabilizer: Lignite/Leonardite is used as a mild dispersant and thinner

g. Control biological activities: Bactericide is added to prevent bio-degradation of natural

Project 10121-4501-01 / UH-CIGMAT 9 Final Report PHASE 1

3. THEORY AND CONCEPTS

Where R = electrical resistance

/ = R/R ……………………………………………………………... (2)

In TASK 5 (PHASE 1) the sensitivity of the materials () to changes (composition,

Project 10121-4501-01 / UH-CIGMAT 10 Final Report PHASE 1

(a) Sample Preparation

Project 10121-4501-01 / UH-CIGMAT 11 Final Report PHASE 1

(a) (b) (c)

Project 10121-4501-01 / UH-CIGMAT 12 Final Report PHASE 1

(d) Setting Time

(e) Curing Conditions

Project 10121-4501-01 / UH-CIGMAT 13 Final Report PHASE 1

(g) Fluid Loss

4.2 Drilling Mud

(i) Bentonite Content

Figure 5. Histogram of bentonite used in drilling mud

Project 10121-4501-01 / UH-CIGMAT 14 Final Report PHASE 1

Project 10121-4501-01 / UH-CIGMAT 15 Final Report PHASE 1

5. RESULTS AND DISCUSSIONS

Project 10121-4501-01 / UH-CIGMAT 16 Final Report PHASE 1

*Percentage of foam/silicate based on the weight of cement

(a) Rheological Properties

Project 10121-4501-01 / UH-CIGMAT 17 Final Report PHASE 1

Plastic Yield Point YP/PV Remarks

Project 10121-4501-01 / UH-CIGMAT 18 Final Report PHASE 1

Project 10121-4501-01 / UH-CIGMAT 19 Final Report PHASE 1

Project 10121-4501-01 / UH-CIGMAT 20 Final Report PHASE 1

(b) Setting Behavior

Project 10121-4501-01 / UH-CIGMAT 21 Final Report PHASE 1

Project 10121-4501-01 / UH-CIGMAT 22 Final Report PHASE 1

Initial Minimum 1Hour 24Hour

Cement (C) 0.98 0.86 70 0.87 1.43 67%

(ii) Hydration of Cement