SPE 151856

A CT 6can $ided &ore-flood 6tudy of the /eak-off 3rocess in 2il-based

'rilling )luids 1,* 1 1,2 3
Andrea S. van Overveldt, SPE, Hua Guo , SPE, Gerard de Blok , SPE, Pavel Bedrikovetsky , SPE, Pacelli L.J.
1
Zitha
1
Delft University of Technology, Department of Geotechnology, Stevinweg 1, 2628CN Delft, The Netherlands
2
Shell China E & P Co. Ltd, PetroChina, 26/F, Yanlord LandMark Office Building No.1, Section 2 Renmin South
Road, Chengdu 610016, Sichuan, P.R. China
3
University of Adelaide, Australian School of Petroleum, SA 5005, Australia
*Currently with Maersk Oil.

Copyright 2012, Society of Petroleum Engineers

This paper was prepared for presentation at the SPE International Symposium and Exhibition on Formation Damage Control held in Lafayette, Louisiana, USA, 15–17 February 2012.

This paper was selected for presentation by an SPE program committee following review of information contained in an abstract submitted by the author(s). Contents of the paper have not been
reviewed by the Society of Petroleum Engineers and are subject to correction by the author(s). The material does not necessar ily reflect any position of the Society of Petroleum Engineers, its
officers, or members. Electronic reproduction, distribution, or storage of any part of this paper without the written consent of the Society of Petroleum Engineers is prohi bited. Permission to
reproduce in print is restricted to an abstract of not more than 300 words; illustrations may not be copied. The abstract must contain conspicuous acknowledgment of SPE copyright.

Abstract
The leak-off of oil-based mud (OBM) into sandstone cores was studied both theoretically and experimentally. Simple models
were used to describe the build-up of the external filter cake and the internal filtration of small particles. Then systematic
static leak-off experiments were done using an innovative method where CT scans taken at time intervals were used to
visualize and accurately quantify infiltration of fluids into sandstone cores. This method allowed the monitoring of the leak-
off process in a way that could not be done by the traditional API filter paper press test. The composition of oil based drilling
fluids was varied, to investigate the influence of various particles on the leak-off process. Scanning electron microscopy
(SEM) was used to characterize the external filter cake and internal filtration. The core flow experiments were matched to the
theory for linear static filtration. The results lead to new insights concerning the build of external filter cake and internal
filtration. This work creates a basis for future improvement of oil-based mud, by providing a better understanding of
mechanisms involved in leak-off process and its control.

1. Introduction
The drilling of oil and gas wells requires careful formulation of the drilling fluids. Since the exploration and production of
hydrocarbons has been moving to greater depths (e.g. Jellison et al. 2008), there is an increasing demand of oil-based drilling
mud (OBM) that are stable at the high pressures and temperatures (HPHT) encountered at those depths. Besides being stable
at HPHT conditions, OBMs have superior lubricating characteristics, great effectiveness against corrosion and ensure
adequate cooling of the drill string and the drill bit (Aston et al. 2002; Bland et al. 2002; Bourgoyne et al. 1991).
A typical OBM consists of water-in-oil emulsions stabilized by a surfactant, to which other components are added to
accomplish specific tasks (Bourgoyne et al. 1991). Lime Ca(OH) 2 ensures the alkalinity of the water phase. A second
surfactant dissolved in the oil phase modifies the wettability of drilled formations and of dispersed minerals from water-wet
to oil-wet: this prevents adhesion of water droplets on mineral surfaces enhancing thus the stability of the OBM. Colloidal
solids (e.g. Bentonite) dispersed in the oil increase the yield stress and the viscosity of the OBM, helping thereby the
transport of the cuttings to the surface. Barite or calcium carbonate particles also dispersed in the oil increase the overall
density of the drilling fluid, enabling good pressure control, wellbore stability and sealing the formation.
Another equally important role of the solid particles dispersed in the OBM is to form a filter-cake for minimizing the leak-off
of the OBM into the matrix of the formations being drilled (Al Ubaidan et al. 2000; Romero et al. 2006). Often the build-up
of the filter cake is insufficient to prevent leak-off. Therefore, chemical additives are used for reducing the permeability of
2 SPE 151856

the filter-cake (Longeron et al. 1998; Aston et al., 2002; Hua et al., 2011). In the 1940s fluid loss control was mostly achieved
by using bentonie (Nelson 1990). In the 1950s the introduction of carboxymethyl-hydroxyethylcellulose (CMHEC) hailed the
beginning of the use of polymers as leak-off control agents (Mueller, 1992). In the last three decades, additives such as
Gilsonite, which are soluble or partially-soluble in oil, have been widely used as leak-off control agents (Aston, 2002; Davis,
1988).
The leak-off process is reminiscent of the filtration of particles during Produced Water Re-Injection (PWRI), for which a
large body of literature exists (Iwasaki 1937; Herzig et al. 1970; Bedrikovetsky, 1993; Elimelech et al., 1993; Sharma et al.,
1997; Sharma and Yortsos 1987). Much progress was made in the understanding of filtration in the last two decades owing
chiefly to new theoretical developments (Bedrikovetsky 2001; 2002; 2003; 2004; Rousseau et al., 2008; Sharma et al., 1997),
more systematic use of CT scanning techniques in core floods (Al-Abduwani 2005; Ali et al. 2005, Saraf et al 2008; Obeta et
al. 2010) and advances in post-mortem analyses with scanning electron microscopy (SEM), x-ray fluorescence (XRF) and
nuclear magnetic resonance (Bailey et al. 2002). Nevertheless, many questions persist about the mechanisms underlying the
leak-off and ways to mitigate it when drilling with OBM.
The purpose of this study was to determine the role of the most relevant components of the OBM of the leak-off process and
to examine in detail the relation between filter-cake build-up and the internal filtration. A theoretical analysis of the leak-off
process accounting for both the filter-cake build-up and the internal filtration and systematic leak-off experiments through
natural porous sample was undertaken. CT scans done at different times were used to visualize and quantify simultaneously
the external filter-cake build-up and the internal filtration. This approach provides more detailed picture of the filtration
process than the standard API filter paper method traditionally used for testing drilling fluids. The microstructure of the filter
cake and penetration of particles into the core were further examined by Scanning Electron Microscopy (SEM) analyses at
the end of each experiment. The paper proceeds with the theoretical model (Section 2). This is followed by the experimental
details are presented (Section 3). Next the results are presented and discussed (Section 4). Then the main conclusions of this
study are drawn (Section 5).

2. Theoretical Model

2.1. Physical model

Fig. 1 depicts the arrangement for the filtration of an oil-based mud (OBM) with viscosity  through a porous medium with
length L and cross-sectional area S , and porosity  and permeability k. The solid particles suspended in the OBM are
characterized by the dual size distribution shown in Fig. 2. It is assumed that the particles have average diameters d1 and d2
such that, if d3 denotes the diameter of the pores in the porous medium, then d1 < d3 < d2. Correspondingly, we denote the
concentrations of the particles (number of particles per unit volume) c 1 and c 2 . The leak-off process is initiated upon applying
a constant pressure drop  p across the OBM, leading simultaneously to the build-up of a filter cake with porosity  c ,
permeability k c and thickness l c and the infiltration of the porous medium by oil fluid with volume V(t). The governing
equations for this process presented in the next sections, were derived from mass conservation arguments and the Darcy’s
law under the following basic assumptions: (1) the carrier oil fluid and particles are incompressible, (2) the flow is laminar
and isothermal at the given pressure and flow rate, (3) only the largest particles contribute to the formation of the external
filter cake, (4) the smallest particles will be retained in both the porous medium and the external filter cake and (5) the
emulsified water droplets do not have any significant contribution to the formation of the filter-cake.

lc,kc,c

k,

S
Fig. 1: Schematic arrangement of the leak-off process.
SPE 151856
3

S m a ll L a rg e
P a rt ic le s P o re s P a r tic le s

Frequ enc y

D i a m e te r
Fig. 2: Large and small particle size distribution and the pore size distribution. It is assumed that the large
particles do not penetrate the pores and the small particles penetrate both the filter cake and the pores.

2. 2. Governing equations
To formulate the governing equations, we assumed further that the largest particles in the OBM do not penetrate the porous
medium; their size is much larger than the pore sizes of the porous sample (d2>>d3). Therefore at any time t, the smaller
particles will flow through a medium composed of both the external filter cake and the core sample. For simplicity, we
assume further that the smaller particles are also much smaller than pore sizes in the external filter cake (d1 << d2/a, a= 6-
10). Therefore, in principle, the smallest particles can be retained in both the external filter-cake and the porous medium.
However, the analysis below is restricted to the case where the interaction of the small and large particles is repulsive such
that the retention of the smaller particles in the external filter-cake is negligible. For this case, we only need to consider the
internal filtration in the porous medium, which greatly simplifies the analysis as it enables the separation of the build-up of
external filter-cake and the internal filtration. A more detailed analysis, accounting also for the internal filtration of the small
particles in the external filter-cake, is presented in the Appendix.

2.2.1. External filter-cake build-up

The formation of the external filter cake was described in detail elsewhere (Hua et al., 2011). Here, only the key equations
will be presented. The filtrate volume V(t) obeys the following ordinary differential equation (ODE):

dV t 
Q 0 =  F0 V  t  + 1  , (1)
 
dt

with,

k ΔP k c2
Q0 = S , F0 = . (2)
η L kc  1 - c  1 - c2  LS

where we have assumed the permeability of the medium to be constant. Assuming that F0 is constant, the ODE can readily be
solved with the generic initial condition V(ts) = Vs, where Vs and ts are, respectively, the spurt loss and spurt time. This gives

 Q 0 t, t < t s


V t  =   F V + 1 2 + 2F Q t - t  -1 (3)
0 s 0 0 s
 , t > ts

 F 0

when Vs = 0, ts = 0 ; the above expression reduces to:

1 + 2 F0 Q 0 t - 1
V t  = (4)
F0
4 SPE 151856

If in addition the condition 2F0Q0t >> 1, which is always a reasonable assumption for long times, the expression for the fluid
loss Eq. 4 can be further simplified to:

2Q0
V (t ) = t
F0
(5)

This equation shows that the filtrate volume grows proportionally to square root of time (taking the spurt loss time as the
reference time) in agreement with the Carter’s equation for leak-off during fracture propagation (van der Hoek, 2002).

2.2.2 Internal filtration

As already mentioned (see Section 1), the internal filtration can be satisfactorily described using the classical deep filtration
theory. The starting point of the theory consists of the mass conservation, particle retention kinetics, and the Darcy’s
equations. Assuming porosity to be constant, the particle diffusion and dispersion coefficient, to be very small and the
deposition coefficient is constant    0 the governing equations can be written:

  t c  u  x c  (1   )  t 
(6)
 t   0 u c
(7)
u    k    xP
(8)

Here c is the concentration of suspended particles,  is concentration of deposited particles,  the effective porosity of the
sandstone core and u is the velocity. The equations are to be solved with the following initial conditions and boundary
conditions:

c ( x , 0 )  0 , ( x , 0 )  0 , x  0 , c (0 , t )  c 1 ,  (0 , t )  0 , t  0 .

The solution c  x , t  and   x ,t  can be expressed:

 c 1 e x p (  K x ), x  vt
c (x ,t )   , (9)
0, x  vt

   0 c 1  v t  x  e x p (  K x ), x  vt
 (x ,t )   . (10)
0, x  vt

The total concentration of particles C (x ,t ) in the porous medium is the sum of the suspended particles and deposited particles
and can be expressed as

C ( x , t )   c ( x , t )  (1   ) ( x , t ) . (11)

Substituting c(x,t) and  (x,t) by their expressions yields the following expression:


 c1 1   λ 0  v t - x   e x p (  K x ), x  vt
C (x ,t )    , (12)

0, x  vt

It follows from this expression that the concentration of particles at any position x should increase linearly with time. In
particular, for x  0 we have

C 0 (t )  c 2  1  λ0 u t  (13)
SPE 151856
5

3. Experimental

3.1 Preparation of the OBM

Table 1 gives the main characteristics of the components of the OBM used in this study. For the preparation of the OBM, the
primary emulsifier OmniMul was dissolved in the base oil, while stirring the mixture using an IKA overhead stirrer. The
rotation speed of the stirrer was increased gradually till it reached 5000 rpm and, after adding the required amount of
surfactant, stirring was continued for another 5 min. Lime Ca(OH)2 was dissolved in water in a separate beaker and intensely
mixed using a magnetic stirrer. The brine was then added while stirring the oil phase: stirring continued for an additional 5
min. The Bentonite, secondary emulsifier OmniChem and the fluid loss control additive were added consecutively while the
emulsion phase was being stirred. Finally, barite was added and the drilling fluid was stirred with IKA stirrer at a rate of 3000
rpm for 10 min.

Table 1: Characteristics drilling fluid components

Component Function Specific Gravity
Sipdrill 2/0 Base oil 0.81
Water Dispersed phase 1.00
Lime= Ca(OH)2 Reduce pH of water 2.24
Bentonite Viscosity control 2.40
Barite Density control 4.20

Gilsonite Fluid loss control 1.00

OmniChem Wettability control 1.00
OmniMul Emulsifier 0.95

3.2 Experimental setup

The setup used to conduct the experiments is shown schematically in Fig. 3. The core holder was made of PEEK, a plastic
material which is transparent to X-rays and has good mechanical properties. The core-holder is vertically placed in the CT
scanner, such that the scans are taken parallel to axis of the core. Two flow lines are connected to the top-end of the core
holder. One flow line is connected to the gas source (bottle and pressure regulator) used to pressurize the core-holder and the
other is connected to the syringe used to inject the drilling fluid. The experimental setup has an outlet valve, to ensure that the
drilling fluid does not penetrate into the core during injection.
Bentheimer sandstone cores with properties given in Table 2 were used to do the experiments. The cores are cast in Araldite
self-hardening glue and then dried in an oven for 48 hours at a temperature of 60 0C. From the CT scans it was estimated that
the glue penetrates a maximum 2 mm into the core which is negligible. After hardening of the glue, the core is machined so
that it fits precisely in the core-holder and to a length that is one third of the total core-holder.

Fig. 3: Schematic of the set-up used to investigate the leak-off of an OBM with the aid of CT scans.
6 SPE 151856

Table 2: Characteristics sandstone cores

Material Bentheimer
Porosity (%) 20±1
Permeability (D) 1.3±0.2
Diameter (cm) 3.8 ± 0.1
Length (cm) 5.8 ± 0.1
Pore volume( cm3) 13± 0.5
Pore Size Average (m) 17±5

3.3 CT scanning of the samples

The CT scan images were obtained using a third generation SAMATOM Plus4 Volume Zoom Quad slice scanner from
Siemens, using the scan settings given in Table 3. More details about the CT scanner can be found elsewhere (for instance Al
Abduwani et al., 2005). The images represent maps of the X-ray attenuation coefficients of the subject examined
reconstructed from multidirectional X-ray transmission data obtained by rotating X-ray source and detector around the
subject. The X-ray attenuation coefficient  of a pure substance can be expressed as

   NA Z M a  b Z 
3 .8 3 .2
E (14)

where  [kg/m3] is the density of the material, NA [1/mole] the number of Avogadro, Z the atomic number, M [kg/mole] the
molecular weight and E[J] the X-ray photon energy; a [m2] is the Klein-Nishina cross-section and b constant (a = 9.8×10-28
m2/electron for E in keV). The first and second terms in equation (14) account for Compton scattering and photoelectric
absorption, predominant respectively at high and low energies (E >> 100 keV and E << 100 keV). In the range investigate
(80-140 keV) both contributions are significant. Due to losses, the actual energy of the X-ray beam is nearly 25% lower than
the nominal value. Eq. (15) holds for compounds by replacing , Z and M by effective quantities. The effective atomic
1 / 3 .8
 
Z   
3 .8
number Z is given then by giZi  , where gi and Zi are respectively the electron faction and atomic number of the
 i 
i-th atomic species. The attenuation coefficients are conveniently normalized with respect to the attenuation coefficient of
pure water  w and expressed in Hounsfield Units (HU), according to the following equation

  w  1
3
H  10 (15)

Clearly, vacuum has attenuation -1000 HU and pure water has attenuation 0 HU. The attenuation coefficient for air at
atmospheric pressures is nearly equal to that of vacuum.

Table 3: CT scanning settings used in this study

Description Conditions
Voltage 140 kV
Current 250 mA
Voxel size 0.3×0.3×1.0 mm
Scan Mode Sequential

3.4 Experimental procedure

The set of leak-off experiments performed in this study is shown in Table 4. The composition of the drilling fluid was varied
systematically, starting with a base oil-based mud (OBM) to which barite and Gilsonite particles were added as indicated in
the table. Although great care was taken when preparing the OBM and in conducting the leak-off experiments, slight
differences in the OBM formulation and core characteristics may lead to variability in the leak-off process. For this reason,
for each OBM formulation, the leak-off experiment was done twice to appreciate the reproducibility of the measured leak-off
volumes.
Each experiment started by placing a dry core in the core-holder and then a (dry core) CT scan image was taken, to determine
precisely the position of the core holder in the scanner and to collect reference CT scan data. The CT images were shot at
planes containing the axis of the core. Next the OBM was carefully injected during 1.0 min using a syringe, while keeping
SPE 151856
7

the outlet valve is closed. Hereafter a CT scan image was made before overburden pressure was applied. Then a pressure of
7.0 bar was applied by turning the pressure regulator on. Immediately after the outlet valve was opened to start the leak-off
experiment. During the leak-off experiment CT scan images were taken at time intervals, over a period of 30 minutes. In the
first 5 min, 3 or 4 images were taken in an attempt to record the spurt-loss behavior accurately. At the end of each experiment
the core and the external filter cake were carefully sawn and then carefully characterized using a Philips XL30 environment
scanning electron microscope (ESEM).

Table 4: Overview of the four types of experiments done during this study. Each experiment was
done twice, as noted by the letters A and B, to check the reproducibility. Exp. 1 (A,B) was done
with the base OBM, without barite or Gilsonite particles. In Exp. 3-4 these components were added
as indicated in the table.
Experiment 1(A,B) 2(A,B) 3(A,B) 2(A,B)
Base OBM +Barite +Gilsonite +Barite+Gilsonite
Component Concentration
(Weight%)
Sipdrill 2/0 (Base Oil) 69 29.5 68.2 29.4
Water (Dispersed phase 3 1.3 21.0 9.1
OmniMul (Emulsifier 1) 21 9.10 3.7 1.5
Bentonite (Viscosifier) 4 1.6 2.9 1.3
OmniChem (Emulsifier 2) 1 0.4 0.8 0.4
Lime 2 0.9 2.2 0.9
Barite - 57.2 - 56.9
Gilsonite - - 1.2 0.5

Table 5: Chemical formulae of the OBM constituents contributing to

the external filter cake and the intrenal particle deposition. The marker
elements were used for the interpretation of the SEM.
Compound Chemical Formula or Markers Element Analysis
Elemental Composition
Bentonite Al2O34SiO2H2O Si, Al
Lime Ca(OH)2 Ca
Barite BaSO4 Ba
Gilsonite C, H, N, S, O N

4. Results and discussion

The results discussed below correspond to the experiments shown in Table 4. As already mentioned the reference experiment
was done an OBM without barite or Gilsonite. For this experiment, first we present the CT scan images and then derive the
CT scan profiles from which we determine filtrate volume of fluid infiltrating the porous medium. Then we discuss the
micrographs obtained at the end of the experiment. For the experiments 3-4, we only discuss the filtration volumes and the
SEM images to highlight any differences with the base case.

4.1 Base Oil-Based Mud

4.1.1. CT images and attenuation profiles

Fig. 5 shows four CT images obtained at different times during the leak-off experiment with the base OBM (Exp. 1 in Table
4). In this experiment a total of 17 CT scan images were obtained over the duration of the test (30 minutes) but only four
images were selected to illustrate the leak-off behavior. In fact for each time, a set of 4 parallel images with a spacing of 0.5
mm from each other were actually obtained: these images were averaged to obtain the image shown in the figure. The upper
dark blue, intermediate light blue and lower yellow parts correspond, respectively, to air, OBM and the sandstone core. The
red dots on the corners near the OBM/porous medium transition represent the O-rings. It can be clearly seen from the image
that the level of the OBM in the sample holder diminishes as a function of time. At the same time change in color (from
yellow to orange) in the bottom part (core sample) reveals the penetration of the core by the fluid. The external filter-cake is
not clearly visible in the images because of the low attenuation of its main constituents (Bentonite, water droplets, etc.).
8 SPE 151856

3500

3000

2500

2000

1500

1000

500

Start 33 Seconds ± 15 Minutes ± 30 Minutes 0

Fig. 5: CT images for leak-off experiment done with the base OBM (Exp. 1A)

To visualize the filtration volume and the external filter cake more clearly, the CT images are subtracted from the start image,
resulting in the images shown in Fig. 6. The upper light blue strip is a measure of the sum of the volume of fluid that
penetrate the core and the volume of the particles in the filter cake. The lower light blue strip corresponds to the external filter
cake formed on the core sample. While the external filter-cake was clearly visible, measuring its thickness precisely proved
to be rather difficult as it was too small for the settings of the CT scanner. However, we could establish that the upper bound
of the thickness should be around 1.0 mm.

3500

3000

2500

2000

1500

1000

500
7 Seconds ± 15 Minutes ± 30 Minutes
0
Fig. 6: Subtracted CT images showing the evolution of the OBM for leak-off experiment done with the
base OBM (Exp. 1A)

For further quantitative analysis of the experiments, the data in Fig. 5 were averaged over the cross-sections of the core,
resulting in the CT scans attenuation coefficients vs. distance plotted in Fig. 7. The zero of the x-axis is taken at the top of the
inner part of the core-holder. The CT-image in the inset corresponds to 7.0 s from the start of the experiment. The variation
of the CT values along the axis of the core-holder (see Fig. 7a) represents respectively air, OBM and sandstone core with the
impinging fluid and particles. The vertical lines represent the air/OBM and OBM/porous medium interfaces. The region
surrounded by the red rectangle was magnified (see Fig. 7b) to visualize better the movement of air/OBM interface.
Although it is not possible to make a quantitative comparison of the model predictions and the experimental data due to lack
some insight about the consistency of the experiments was by making a qualitative comparison. From the analysis of the
build-up of the external filter cake and equation (12) for the internal filtration the expected CT attenuation profiles is as
sketched in Fig. 8. Clearly all the features of the predicted by this curve are visible in the measured CT attenuation profiles
(Fig. 7a).
SPE 151856
9

3000 3500

3000
2500

2500

Attenuation coefficient
2000 0 sec.
7 sec.
19 sec.
33 sec. 2000
47 sec.
1500 71 sec.
142 sec.
171 sec. 1500
231 sec.
1000 291 sec.
351 sec.
1000
470 sec.
589 sec.
890 sec.
500
1188 sec.
500
1486 sec.
1784 sec.

0
0 20 40 60 80 100 120 140 160 0
Position Core [mm]

a)

1000

800
Attenuation coefficient

0 sec.
7 sec.
19 sec.
33 sec.
600 47 sec.
71 sec.
142 sec.
171 sec.
400 231 sec.
291 sec.
351 sec.
470 sec.
589 sec.
200 890 sec.
1188 sec.
1486 sec.
1784 sec.
0
56 57 58 59 60 61 62 63 64 65 66
Position Core [mm]

b)
Fig. 7: (a) CT attenuation profiles for leak-off experiment with the base OBM (Exp. 1A). The inset image
corresponds to 7.0 s. (b) Magnification of the air/OBM interface reveals the evolution of the filtration
volume over time.

C(x,t)
Filter Cake 9
x 10
6

6 Porous Medium
5
C(x,t)

Drilling Fluid 4

0
0
0 1 2 3 4 5 6 7 8
Position (x)

x
Fig. 8: Concentration profiles predict from the combination of the external filter cake build-up and the
internal filtration. The off-set of the internal filtration is due to the attenuation of the sandstone.
10 SPE 151856

4.1.2. Filtration volume

Fig. 9 shows that the filtration volume increases linearly as a function of the square root of time, after the spurt time. The
linear dependent of V on t1/2 agrees with the proposed model (see Eqs. 6-8). The equations were fitted to the experimental
data using the Levenberg-Markarg least-squares method (Nocedal and Wright, 1999; Kanzow et al., 2004). The spurt loss
volumes for the experiments 1A and 1B, respectively, 4.00±0.1 and 3.08±0.1 ml are rather different due probably to
differences in the start time of the experiments. Our model for the static filtration contains the parameter for the flow rate
during the spurt loss Q0. Following the usage in the literature (Bourgoyne et al., 1991), the spurt loss volumes are determined
by extrapolation and using the intersection of the linear fit at zero time. This was done considering that V (t )  Q 0 t for t<ts, i.e.
the leak-off volume is quadratic with the square root of time. However, the spurt time determined by this method is not very
accurate due scarcity of points for t<ts: to improve the prediction of the spurt loss more scans should be made in the first 5
seconds of the experiments.
To allow this, the experimental set-up was slightly modified before conducting experiments 2-4. New flow lines were
installed to allow the control of the pressurization and the outlet valve from outside the CT scanner room. This reduced the
time needed to take the first CT scans after applying and opening the outlet valve could be reduced form 11 s to 3-4 s. It is
possible that the spurt time is even smaller than 3-4 seconds. This indicates that process of internal filtration and buildup of
filter cake, under the experimental conditions of this study, were very fast. Furthermore, the largest amount of leak-off
occurred during the spurt.

V(t)=0.27 t1/2+4.00
5 R2=0.95
Filtration Volume (ml)

4
V(t)=0.30t1/2 +3.08
R2=0.97
3

Experiment5
1 Linear Fit Exp 5
Experiment 16
Linear Fit Exp16

0
0 1 2 3 4 5 6
t1/2 [min]

Fig. 9: Filtration volume as function of the square root of time for leak-off experiments with the base OBM
(Exps. 1A and 1B).

4.1.3 Characterization of the external and internal filter cakes

The external filter cake and the top part of the core were examined using SEM (Figs. 10 and 11). The contrast in the images
is determined by the atomic number of the elements. In addition an elemental analysis of the constituents of the OBM was
also used for the interpretation of the filtration tests. The particles are smaller than the beam size and, therefore, the spectrum
shows the collective compositions at the interested area.
The thickness of the external filter-cake was found to be 0.60+0.05 mm. The dark and grey particles represent bentonite and
lime respectively. Traces of white barite particles are also present. Large and small pores are visible throughout the external
filter cake. The tiny pores are probably due to the emulsified water droplets that evaporate upon drying the filter cake.
Fig. 12 gives an overview of the elements present in the internal pore space and elements in the external filter cake. Using the
elemental composition given in Table 5 it was possible to get an impression of the contribution of the different particles to
the external filter cake and to the internal filtration. The elemental analysis revealed that the external filter-cake is a
combination of bentonite and lime particles. Fig. 12 shows that Al and Si, the markers of Bentonite, are present in both the
external and the internal filter cake. The ratio Al/Si for the external cake is totally different than that for the internal cake.
This is because Si is the main component of sandstone rock. For a quantitative analysis of the internal filtration of Bentonite
in all experiment series an element analysis of a pure sandstone core would have been useful. However, it was not available
at the time of the experiments.
In the theoretical model it was assumed that particles will pass through the external filter cake and penetrate into the core if
they are smaller than the pore size and that particles larger than the pore size will not penetrate the core. A more complex
SPE 151856
11

picture emerges from the above results. Small particles not only penetrate the porous medium, but also they are part of the
external filter cake, filling up gaps between larger particles. The large particles initiate the formation of the external filter
cake and small particles plug the pore space in the cake, causing leak-off to slow down considerably.

External Filtercake

Sandstone

Glue

Fig. 10: Top core after drying

External Cake Thickness:599m External Filtration

Internal Filtration Internal Filtration

Fig. 11: SEM micrographs for the leak-off experiment with the base OBM (1A). The dark grey particles (A)
are lime and the light grey particles B are bentonite. The dense white particles are most probably traces
of barite.
12 SPE 151856

45

40

35

30
External Cake
Internal Filtration
25

Wt%
20

15

10

0
O Na Mg Al Si S K Ca Fe
Elements

Fig. 12: Elemental composition (wt%) of the external filter-cake and internal filtration for experiment 1A.

4.2 Effect of Barite

4.2.1. Filtration volume

The CT scans obtained in the second set of experiment with added barite (see Exp 2A,B in Table 4) were much noisier that
those for the base OBM. However, by an astute subtraction of the images we could visualize the variation of the OBM
volume due to leak-off and the filtration volumes vs. time shown in Fig 13.
The measured spurt loss volumes for experiment 2A and 2B, respectively, 0.89±0.1 ml and 1.21±0.1 ml (Fig. 13) are much
closer than in the first experiment, which proves that the modification of the set-up has improved the accuracy of the
measurements as desired. However, the difference is unfortunately not negligible and more work will be needed to improve
the measurements further. In this experiment the spurt loss volumes of 0.87 and 1.21 cm 3 are significantly smaller than the
spurt loss volume of 4.00 and 3.08 cm3 for the previous experiment, indicating a good leak-off control.
The linear dependence of the leak-off volume on the square root of time after spurt time is also observed in this case. The
slopes have values of 0.13±0.01 and 0.14±0.01 cm3/s2. The presence of barite improvises the leak-off control compared to the
experiment series with the base OBM. It should be noted that traditionally barite is added mainly for weight control, thus
making the particle density of the drilling fluid significantly higher than that of the drilling fluid used in the experiments with
the base OBM. Here we show that barite also contributes significantly to fluid loss control.

4
Filtration Volume [ml]

2 V(t)=0.14 t1/2+1.21
R2=0.96

Experiment 2A
1 Linear Fit Exp 2A
1/2 Experiment 2B
V(t)=0.13 t +0.89 Linear Fit Exp 2B
R2=0.99
0
0 1 2 3 4 5 6
t1/2 [min]

Fig. 13: Filtration volume as function of the square root of time for leak-off experiments with the base
OBM with added barite (Exps. 2A and 2B).
SPE 151856
13

4.2.2. Filter cake and internal filtration

The thickness of the external filter cake was estimated using a ruler (Fig. 14) and measured more precisely using SEM
images (Fig. 15). It was found to be 2.00 ± 0.05 mm. This value is much larger than that of the previous experiment (about
0.6 mm). The SEM micrographs show also that the external filter cake consists of combination of larger and smaller particles
of barite (bright white particles), bentonite and lime particles. The particles are densely packed in contrast with the previous
experiment. Several larger and tiny pores are equally visible in the external filter cake.
The SEM micrographs show further that the pores near the OBM/porous medium interface are plugged mainly by the smaller
barite particles. These particles seem to have formed agglomerates which filled up the pores. This suggests that the deposition
into the core took mostly place in the first few seconds and occurred at shallow depth into the core of 1.0±0.1 mm.
The elemental analysis (see Fig. 16) supports the idea that barite is the main component in the pore space as well as in the
external filter cake in good agreement with the SEM analyses. This supports the idea that adding barite to the base OBM
favored both the formation of an external filter cake and the internal filtration (plugging of the pores). The efficiency of barite
as leak-off control agent is probably due to the fact that barite is characterized by a wide particle size distribution. The
combination of smaller and larger particles probably led to external filter-cake with a lower permeability and to clogging of
the porous medium by internal filtration.
The above observations indicated that the external filter-cake build-up and internal filtration occur simultaneously in good
qualitative agreement with the proposed theoretical analysis (see Section 2). However, the fact that in the experiment we are
dealing with a wide distribution of particles sizes rather than a dual particle size distribution as assume in the model precludes
any quantitative comparison.
Our finding that barite is in fact an efficient leak-off control agent seems to contradict the argument of others (e.g. Aston et
al. 2002) who suggested that barite does not play a significant role in leak-off control.

External Filtercake

Sandstone

Glue

Fig. 14: Top core after drying for the leakoff experiment with the base OBM with added barite.
14 SPE 151856

B A

External Cake Thickness:2000m External Filtration

Internal Filtration Internal Filtration

Fig. 15: SEM micrographs experiment 2A. The dark grey particles A indicate lime, the light grey particles
B indicate bentonite and the white particles C is barite

50

45 External Cake
Internal Filtration

40

35

30
Wt%

25

20

15

10

0
C O Na Al Si S Ca Ba Fe
Elements

Fig. 16: Elemental analysis for the experiment 2A, showing the weight percentage of elements in the
external filter cake and internal filtration.
SPE 151856
15

4.3 Effect of adding Gilsonite

4.3.1. Filtration volume

In the third experiment Gilsonite was added to the base OBM (see Exps. 3A,B, Table 5). The spurt loss volumes for
experiment 3A and 3B are respectively 0.95 ±0.1 ml and 1.87 ±0.1 ml (Fig. 17). These values are smaller than those for the
base OBM (see Subsection 4.1). However, they are larger than the case of the base OBM with added barite.
The difference in spurt loss and filtration volume for the repeated experiments 3A and 3B is much higher than in the other
experiments: the spurt loss in the experiment 3B is twice that of experiment 3A.
The slope of V(t) vs. t1/2 in experiment 3B (0.24) is approximately 30% larger than in experiment 3B (0.16). Other
experiments, in contrast, show spurt loss variations in the order of 20-30% and much smaller differences in the slope of V(t)
vs. t1/2. The reason for this differences is not completely clear. We suspect that it is due to variations in the properties of the
Gilsonite and perhaps also on its interaction with the oil and other constituents of the base OBM. Gilsonite consists of
lyophilic solid materials which might swell and become softer over time. This would lead to a poorer leak-off control as since
the softer particles can be deformed more easily making it harder to build-up a filter cake.
Despite the above limitations in the reproducibility of the experiments the data confirm that Gilsonite can be effective in
preventing leak-off. However, the data also shows that if not properly designed using Gilsonite as leak-off control agent by
adding it to the base OBM when losses occur might not give the desired results.

5
Experiment 3A
Linear Exp 3A
Experiment 3B
Linear Fit Exp 3B
4
Filtration Volume [ml]

V(t)=0.24 t1/2+2.16
3 R2=0.98

V(t)=0.16 t1/2+
1 1.14
R2=0.94

0
0 1 2 3 4 5 6
t1/2 [min]

Fig. 17: Filtration volume as function of the square root of time for the leak-off experiment with base OBM
and added Gilsonite (Exps. 3A and 3B).

4.3.2 Characterization external filter cake and internal filtration

The thickness of the external filter cake measured from the SEM is approximately 0.84 ±0.05 mm (Figs. 18 and 19). The
external filter cake contains lime, bentonite, and Gilsonite particles. Bentonite and Gilsonite have also penetrated the pore
space. The external filter cake shows large holes, similar to the external filter cake in the experiment for the base case drilling
fluid. The elemental analysis (Fig. 20) indicates that the composition of the external cake and particles retained in the core are
similar to that of the base case except for the addition of the carbon and nitrogen, the markers of Gilsonite. The latter is
present in the external and internal cake.
16 SPE 151856

External Filtercake

Sandstone

Glue

Fig. 18: Top of core experiment 3A, after drying. Scale in cm

External Cake Thickness:836m External and Internal Filtration

Internal Filtration Internal Filtration

Fig. 19: Images of external filter cake and internal filtration for experiment 3A using SEM
SPE 151856
17

40

35 External Cake
Internal Filtration

30

25
Wt%

20

15

10

0
C N O Na Mg Al Si S Cl K Ca Ba Fe
Elements

Fig. 20: Element analysis for experiment 3A, displayed is the weight percentage of elements in external
filter cake and internal filtration.

4.4 Base OBM with barite and Gilsonite

4.4.1. Filtration volume

In this fourth and last set of experiments both barite and Gilsonite were added to the base OBM (see Exps. 4A,B). The spurt
loss volumes for experiment 4A and 4B were, respectively 0.58±0.1 ml and 0.79±0.1 ml and the slopes of V(t) vs. t1/2 in both
experiments, 0.18 and 0.17 respectively, were nearly equal. The reproducibility of the experiments is excellent. The spurt loss
and total filtration volume are the lowest of all the experiments reported. This suggests that for the experiments performed a
combination of particles in the form of bentonite, lime, barite, and Gilsonite is most efficient in leak-off control. This also
supports the idea that a good leak off control requires a combination of external filter cake build-up, internal filtration and an
agent that reduces the permeability of the external filter-cake and the clogged part of the core. The experiments did not
provide concrete clues as to how this lowering of the permeability is achieved with Gilsonie. This question should be subject
of future studies.

4
Filtration Volume [ml]

2 V(t)=0.17 t1/2+0.79
R2=0.69

1 Experiment 4A
V(t)=0.18 t1/2 +0.58 Linear Fit Exp 4A
Experiment 4B
R2=0.79 Linear Fit Exp 4B
0
0 1 2 3 4 5 6
t1/2 [min]

Fig. 21: Filtration volume as function of the square root of time for experiment 4A and 4B
18 SPE 151856

4.4.2 External filter cake and internal filtration

The measured thickness of the external filter cake with SEM (Fig. 22 and 23) was approximately 2.76 ±0.05 mm. This OBM
mixture seems to have wide range of particle sizes, which causes build-up of a compact external filter cake. The particles
deposited in the external filter cake are mostly barite, but lime, bentonite, and Gilsonite are also present. Compared to the
experiment where barite was added to the base OBM (Exp. 3, Table 5), the porous medium contains less barite particles, but
contains a mix of different components. The pore space is also not filled up densely by particles in comparison to the
experiment where barite was added and Gilsonite was not present (see also Fig. 24). This indicates that Gilsonite induces the
formation of a densely packed external filter cake, which limits the penetration of individual particles into the core.
A densely packed filter cake blocking drilling fluid to penetrate into the core is desirable. From the experiments without
barite it was possible to visualize the external filter cake on the CT images. The external filter cake seems to already take
substantial form during the spurt. It is expected that the initial build-up of the external filter cake is due to particles larger
than the pores not penetrating into the core; simultaneously internal filtration takes places of particles smaller than the pore
penetrating into the core. However these smaller particles are also necessary to build-up an impermeable filter cake.
Instantaneous formation of an impermeable external filter is not possible but internal filtration should be limited to an
absolute minimum. A possible option to obtain faster an impermeable filter cake is to have a continuous gel like phase in the
drilling fluid which quickly forms an impermeable layer on the core surface.

External Filtercake

Sandstone

Glue

Fig. 22: Top core after drying

External Cake Thickness:2761m External and Internal Filtration

Internal Filtration Internal Filtration

Fig. 23: SEM micrographs of external filter cake and internal filtration for experiment 4A where barite and
Gilsonite were added to the base OBM.
SPE 151856
19

50

45 External Cake
Internal Filtration

40

35

30
Wt%

25

20

15

10

0
C N O Na Mg Al Si S Cl K Ca Ba Fe
Element

Fig. 24: Elemental analysis for experiment 4A, displayed is the weight percentage of elements in external
filter cake and internal filtration.

5. Conclusions
 The combination of the CT scanner core flow experiments and the characterization of the external filter cake and
internal filtration proved to be an efficient tool to quantify filtration and explain the mechanisms involved.
 An external filter cake was visualized over time on the CT images in experiments where no barite is present in the
drilling fluid. During spurt the external filter cake had already formed substantially. When barite was present in the
drilling the noise of barite was too strong for a proper visualization of the formation of an external filter cake. The
buildup of filter cake is very fast and the thickness is too small to be accurately measured with the current settings of
the CT scanner.
 The spurt loss seems to take place in a rather short time frame of a few seconds. The spurt loss volume is the
determining factor in the total amount of filtration volume. Future research into controlling leak-off should focus on
lowering the spurt loss volume.
 The theory for the linear square root behavior seems to match with our experimental results in all the experiments
series. The experiments show that the mechanisms involved with deep filtration are more complicated than the
theory proposed for linear deep bed filtration in the theory section. Small particles not only penetrate into the core
but also contribute to build-up of an impermeable external filter cake.
 Adding Gilsonite improves leak-off using the base case drilling fluid as reference, addition of barite is however
more efficient than addition of Gilsonite. Addition of barite particles to the base case drilling fluid, results in a pore
space filled up with barite agglomerates. The addition of both barite and Gilsonite to the base case drilling fluid is
most efficient in controlling fluid leak-off, and builds up the most densely packed filter cake. However, in addition
of barite, the density of particles dramatically increases in the mud; the gravity might play a role in the filtration
process. If Gilsonite is present in the drilling fluid, the internal pore space is not completely filled up with particles.
The role of Gilsonite is not yet fully understood.
 Build up of external filter cake take place simultaneously with internal filtration. The pore space does not have to be
completely filled with particles to establish leak-off control

Acknowledgements
We are grateful to Prof. P.K. Currie for input and ideas. We are gratefull to Arjan Thijssen for his assistance with the SEM
images. We thank Ellen Meijvogel-de Koning for her help with the CT scans and Marc Friebel for technical support.
20 SPE 151856

Nomenclature
K = consistency index
n = flow index
0 = yield stress
 = shear stress
Rp = plug radius
R = radius drill pipe
P0 = pressure start drill pipe
PL = pressure bottom drill pipe
l = length of well
V(t) = filtration volume
ts = spurt time
k c, k f = permeability of filter cake and filter paper
Δp = total pressure drop
η = viscosity of mud
S = area of filter paper
c = porosity of filter cake
V(t) = volume of filtrate
cp = concentration of particles in the mud
D = dispersion coefficient
x = distance along the core in the direction of flow
c = concentration of suspended particles
C = total concentration of particles
c1 = concentration particles in external filter cake
c2 = concentration particles internal filtrate
 = concentration of deposited particles
 = effective porosity of the sandstone core
u = the velocity
 = the deposition coefficient,
lc = thickness filter cake
L = core length
rc = radius center well to filter cake
rf = radius center well to penetration depth internal filtrate

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SPE 151856
23

Appendix: Analysis for the external filter-cake build-up and deep bed filtration for a dual particle injection.

Consider the general case of the injection of suspension with two-size particles as described in Section 2. The large particles
are larger than any pore. They cannot enter the porous medium and form external filter cake from the very beginning of
injection. The small particles first filtrate through the cake and then filtrate through the rock. The system of equations (6) and
(7) describes the deep bed filtration. Introduction of dimensionless variables and parameters

x Ut c 1    
x  ,t  ,C  ,S  ,    0 1    L (A-1)
L c
0 0
L c1

into (6) and (7) yields the following dimensionless system

 C  S  C S
  0,  C , (A-2)
t x t

where  is the dimensionless filtration coefficient for the rock; that for the filter cake is denoted c. The injected
concentration of small particles is c10, L is the core length,  is the core permeability, U is Darcy’s velocity.
The analytical model presented below generalizes solution (9). The analytical solution reveals the following scenario. The
concentration front of small particles propagates with the unity fluid velocity along the core from the beginning of injection
along the trajectory x=t. In zone 0 ahead of this front, x>t, both suspended and retained concentrations are zero, C=S=0.
Concentrations are non-zero in zone I behind the concentration front x=t until the transition time ttr, where the retention
concentration reaches its critical value α (α is the critical porosity coefficient), i.e. Scr=(1-)α/c10. After the critical porosity
value is reached at the core inlet x=0, particles cannot penetrate in the rock anymore, i.e. the suspended concentration in zone
II behind the front x=t-ttr equals zero. The suspension concentration in zone I ahead of this front is not zero as it corresponds
to deep bed filtration in the core.
Zone III corresponds to external filter cake built of the large particles. Its speed D1 is obtained from the mass balance of
injected large particles: D1=c20/(1-1), where 1 is the porosity of the cake. The cake (zone III) expands ahead of the front x=-
D1t. At the moment ttr, the internal cake of small particles starts forming inside the large particles cake. The front of the
internal cake is denoted as z(t). Zone IV of the internal cake expands between the front z(t) and the core inlet x=0. After the
intersection of the fronts of external and internal cakes in point (x3,t3), a new cake is formed of two size particles (overall
injected suspension). The velocity D3 is obtained from the mass balance of injected large and small particles: D3=( c10+ c20)
/(1-3). Here 3 is the porosity of the cake formed of two size particles (overall injected suspension). The front of this cake
propagates along the line x=x3-D3(t-t3). Zone IV of the internal cake is ahead of fronts z(t) and x=x3-D3(t-t3) until the core
inlet x=0.
Below we describe the analytical solution.
Zone III. The characteristic line passing via point (x,t) crosses the external cake front in point (-D1t2, t2), so

t  x
D 1t 2  x  t  t 2 , t 2  (A-3)
D1  1

According to solution (9),

 D t  x
C ( x , t )  e x p    c  D 1 t 2  x    e x p    c 1  (A-4)
 D1  1 

The retained concentration S(x,t) is found from (A-4) using (A-2), i.e. by integration of (A-4) in t from –x/D1 to t.
Core inlet. The suspended concentration at the core inlet, as it follows from (A-4), is:

 D 1t 
C (0, t)  exp   c  (A-5)
 D1  1 

Substituting (A-5) into second eq. (A-2), we obtain the equation for retained concentration at the core inlet:
24 SPE 151856

dS  0, t   D 1t 
  exp  c  (A-6)
dt  D1  1 

The retained concentration at the core inlet is:

D1  1    D 1t  
S  0, t    1  e x p    c  (A-7)
 c D 1   D1  1  


It allows calculating the transient time ttr:

1  1   D1  1    D 1 t tr  

  1  e x p c  (A-8)
 c D 1  D1  1  
0
c1  

The suspension concentration at the core inlet after the transition time is zero, retained concentration remains constant.
Zone I. Characteristic line crossing point (x,t) intersects the external cake front at the moment t1:

t  x
D 1 t1  t  x  t1 , t1  (A-9)
D1  1
Characteristic line covers the distance D1t1 inside the external cake and distance x in the core. As it follows from solution (9)

 t  x 
C  x,t  e x p    c D t1  e x p    x   e x p    c D  exp    x  (A-10)
 D1  1 

Retained concentration S(x,t) is found from (A-10) using second eq. (A-2), i.e. by integration of (A-10) in t from x to t. Note
that this equation reduces to solution (9) when c=0, meaning no filtration of small particles in the external filter-cake.
Zone IV. Suspension concentration behind the front of internal cake, which propagates inside the external cake x=z(t), as it
follows from (A-4), is

 D 1t  z  t  
C ( z t  , t)  exp  c  (A-11)
 D1  1 

The velocity of the internal cake is obtained from the mass balance of injected small particles:

dz C  z,t 
 (A-12)
dt 1  2

where 2 is the porosity of the external cake plugged by small particles. Combining Eqs. (A-11) and (A-12) results in the
ordinary differential equation for the internal front position z(t)

dz 1  D t  z
 exp  c 1  (A-13)
dt 1  2  D1  1 

Introducing new variable in (A-13)

D 1t  z
y  c (A-14)
D1  1

results in
SPE 151856
25

D1  1 dy 1
  D1  exp  y  (A-15)
c dt 1  2

which is solved by separation of variables. The time t3 at which the internal cake front reaches the front of the external cake is
calculated from the intersection of front trajectories:

z  t 3    D 1t 3 (A-16)