“Enhanced Wellbore Stabilization and Reservoir Pro-

ductivity with Aphron Drilling Fluid Technology”

Topical Report: Task 4.1 Correlation of Capillary Suc-

tion Time with Leak-Off Behavior

by

Tatiana Hoff
&
Fred Growcock

Issued December 17, 2004

DOE Award Number DE-FC26-03NT42000

MASI Technologies LLC
8275 El Rio St. suite 130
Houston, Texas 77054
 DISCLAIMER

This report was prepared as an account of work sponsored by an agency of the United
States Government. Neither the United States Government nor any agency thereof, nor
any of their employees, makes any warranty, express or implied, or assumes any legal
liability or responsibility for the accuracy, completeness, or usefulness of any informa-
tion, apparatus, product, or process disclosed, or represents that its use would not infringe
privately owned rights. Reference herein to any specific commercial product, process, or
service by trade name, trademark, manufacturer, or otherwise does not necessarily consti-
tute or imply its endorsement, recommendation, or favoring by the United States Gov-
ernment or any agency thereof. The views and opinions of authors expressed herein do
not necessarily state or reflect those of the United States Government or any agency
thereof.

2
Introduction
Core Leak-off tests are commonly used to ascertain the ability of a drilling fluid to seal
permeable rock under downhole conditions. Unfortunately, these tests are expensive and
require a long time to set up. To monitor fluid invasion trends and to evaluate potential
treatments for reducing fluid invasion on location, a simpler screening test is highly de-
sirable.
The Capillary Suction Time (CST) Test has been used since the 1970's as a fast, yet reli-
able, method for characterizing fluid filterability and the condition of colloidal materials
in water treatment facilities and drilling fluids. For the latter, it has usually been applied
to determine the state of flocculation of clay-bearing fluids and to screen potential shale
inhibitors
In this work, the CST method was evaluated as a screening tool for predicting relative
invasion rates of drilling fluids in permeable cores. However, the drilling fluids exam-
ined -- DRILPLEX, FLOPRO, and APHRON ICS – are all designed to generate low fluid loss
and give CST values that are so high that fluid invasion comes to be dominated by ex-
perimental artifacts, such as fluid evaporation. As described in this work, the CST pro-
cedure was modified so as to minimize such artifacts and permit differentiation of the flu-
ids under investigation.

Objectives
Evaluate the potential for Capillary Suction Time to predict rates of invasion of APHRON
ICS and other drilling fluid systems into permeable formations.

Project Description
The Capillary Suction Time (CST) Test, a rapid and cost-effective technique, is com-
monly used to ascertain the state of flocculation of a fluid and its ability to control filtra-
tion through permeable media. The standard CST method breaks down, however, for
highly dispersed low-filtration-rate fluids.
In this study, a Modified CST procedure was developed that eliminates this problem and
is shown to provide results that correlate well with conventional static Core Leak-Off test
results for drilling fluids. This procedure calls for measurement of the travel distance of
the fluid front, or CSD, in a specified amount of time.
For drilling fluids that seal via similar mechanisms, the Modified CST Test can be used
to predict the trend in the rate of fluid invasion into permeable formations. Fluids which
seal via different mechanisms yield different CSD vs. Leak-Off correlations, most likely
because of differences in spurt loss behavior.

Conclusions
Using a Modified CST procedure that generates a measurement of CSD (the distance that
the fluid front travels in 60 min), it has been demonstrated that CSD for low-fluid-loss
drilling fluids correlates with Core Leak-Off test results and obeys standard static filtra-

3
tion theory. The Modified CST procedure has promise as an on-site tool to monitor fluid
invasion trends and evaluate potential treatments for reducing fluid invasion.
Aerated Enhanced APHRON ICS and DRILPLEX drilling fluids generate lower CSD and
Core Leak-Off than solids-free APHRON ICS and FLOPRO drilling fluids. Because the
sealing mechanism varies with type of drilling fluid, different CSD vs Core Leak-Off cor-
relation curves must be used for each fluid system. System-to-system variability of the
CSD vs Core Leak-Off correlation is likely due to the greater impact that spurt loss has
on Core Leak-Off than on CSD.
For a given drilling fluid system, CSD and Core Leak-Off correlate inversely with LSRV,
i.e. CSD and Leak-Off ∞ (LSRV)-1. In addition, additives such as CaCO3 (and air in the
Enhanced APHRON ICS Drilling Fluid) decrease Core Leak-Off and, to a lesser extent,
CSD.

Experimental Approach
The Modified CST and Core Leak-Off test methods utilized in this project are described
in Appendices A and B at the end of this report. In all cases, the fluid samples were
blended with a Prince Castle mixer and hot-rolled for 16 hours at 150°F. Initial tests
were performed using the standard CST method.1 Various mud types were evaluated,
and the results are given in Figure 1.

Figure 1. CST Results - Standard CST Procedure

Capillary Suction Tests - Aphron ICS v. Other Muds
Tests Terminated
100000
21,000 21,000 21,000
8,000
10000 4,900
2,200 1,800
Log Scale

1000
Seconds

420

100 37

10

1
Pre-hydrated bentonite in water
Pre-hydrated bentonite in water + 4.6 ppb 25% CaCl2
FloPro NT
DrilPlex
Standard Aphron ICS Mud(DOE Group base mud+1 ppb Blue Streak) 0% Air
Standard Aphron ICS Mud(DOE Group base mud+1 ppb Blue Streak)~20% Air
Super Enhanced Aphron ICS (w/ 2 ppb Blue Streak), 0% Air
Super Enhanced Aphron ICS (w/ 2 ppb Blue Streak), 56% Air
Super Enhanced Aphron ICS (w/ 2 ppb Blue Streak), 49% Air

The fluids with very long CST values cannot be very clearly differentiated, and artifacts
such as evaporation of water from the blotting paper control the rate of advance of the

4
filtrate. It was determined that CST values higher than a few thousand seconds are
fraught with unacceptably high error. For these fluids, the Modified CST test appears to
provide a much more precise and accurate way to monitor relative filtration rates. As de-
scribed in Appendix A, the Modified CST test involves measuring CSD, the distance in
mm traveled by the fluid in a given time period. Results for the APHRON ICS Drilling
Fluid (with and without entrained air) appear in Table 1 in Appendix A.
Four samples of each system were blended, and the concentration of viscosifier specific
to each system was varied. The systems utilized were: Standard APHRON ICS, Super En-
hanced APHRON ICS (SE APHRON ICS), FLOPRO, and a DRILPLEX. The Standard APHRON
ICS system is converted to the SE APHRON ICS via addition of small quantities of three
products: Aphronizer A, Aphronizer B and Plasticizer. All of the drilling fluids were run
as “solids free” systems, but some tests were also run with samples containing 30 ppb of
CaCO3 with a nominal particle diameter of 40 µm. The corresponding Low-Shear-Rate
Viscosity (LSRV), Leak off, and CSD were measured for each one of these samples. All
of the tests were run at room temperature. LSRV was measured with a Brookfield LV-
II+ Viscometer at 0.06 sec-1 using a L3 spindle. The Core Leak-Off tests were run with
1,000 psi confining pressure, 500 psi inlet pressure and no back pressure, using 2-in long
Aloxite cores of about 5 darcy air permeability. In all cases, the CSD values used for the
correlations were those measured at 60 min (half of the total testing time). The CSD vs
Leak-Off correlations obtained with the 30-min CSD data were similar to these, but the
CSD data appeared to be somewhat less precise. The correlations obtained with the 90-
min and 120-min data were also similar to those obtained with the 60-min data and did
not appear to provide any greater precision. Consequently, the 60-min CSD values were
used for all of the correlations.

Results
Filtration in the Modified CST (CSD) Test
“Static filtration takes place when the mud is not circulated, and the filter cake grows un-
disturbed”.2
If a unit volume of a stable suspension of solids is filtered against a permeable substrate
(paper or core in our case), and x volumes of filtrate are expressed at time t, then 1 – x
volumes of cake will be deposited on the substrate. As a simplifying approximation, the
rate of growth of the filter cake is assumed to be proportional to the rate of growth of fil-
trate. Therefore, if Qc be the volume of the cake, and Qw the volume of the filtrate:
Qc = 1 – x = R (1)
Qw x
Where R is a constant. Now, the area of the filter cake, A, is constant in linear static
filtration, such as API Fluid Loss and Core Leak-Off tests. It is also constant in a CSD
test, though the filtrate itself expands radially along the plane of the paper. Qf is given
by the product of A and the thickness of the filter cake:

Qf = Ah

5
Thus, h = R Qw / A (2)

Now, Darcy’s law states

dq = k ∆P A (3)
dt µh
Where k = permeability of the filter cake (darcy), ∆P = differential pressure across the
cake (atm), µ = viscosity of the filtrate (cP), h = thickness (cm), q = volume of filtrate
(cm3), and t = time (sec).
Therefore,
dq = k ∆P A2
dt µ R Qw
Integrating,
Qw2 = 2k ∆P A2 t / µR (4)
Unifying the constant terms results in
Qw2 = K t (5)
or,
Qw = K’ t1/2 (6)
Where K and K’ are proportionality constants. Equation (6) governs filtration under
static conditions.2
In the Modified CST method (CSD), the distance that the fluid travels, d, is proportional
to Qw. Thus,
d = K’’ t1/2 (7)
Some results for two types of APHRON ICS Drilling Fluids are plotted in this fashion in
Figure 2.
The results in Figure 2 for the two samples of Deaerated APHRON ICS Drilling Fluids
demonstrate the high reproducibility of the Modified CST test.
The linearity of the t1/2 plots shows that CSD follows static filtration theory. It does not
necessarily follow, however, that CSD will correlate with core Leak-Off behavior. Key
differences between core Leak-Off and Modified CST tests include saturation of the pore
network (wet vs. dry), the nature of the filter medium (core vs. paper), differential pres-
sure (elevated inlet pressure vs. ambient pressure), and possibly temperature.
The effect of saturation of the pore network with the base fluid is manifested as a dis-
placement in the apparent “spurt loss.” Spurt loss is generally defined as the loss of
whole mud that occurs initially during fluid invasion, i.e. prior to formation of a fully es-
tablished filter cake. This is given approximately by the y-axis intercept on the t1/2 plot. In
the mathematical treatment of static filtration given above, spurt loss is assumed to be

6
negligible. However, spurt loss is known to be significant in permeable rocks. Further-
more, “a low fluid loss and a dry cell with high hold up volume will cause a negative y-
axis intercept”.3 To prove this, two CSD tests were run, one using dry filter paper and
one using wet filter paper. The system used was Deaerated SE APHRON ICS Drilling
Fluid with 5 ppb viscosifier. The results are shown in the Figure 3.

Figure 2 - CSD vs. Square Root of Time

Travel Distance vs Square Root of Time

12

10
d=distance travel (mm)

8
Standard AphronICS
R2 = 0.9658
6

Super Enhanced
4 AphronICS R2 = 0.99
Super Enhanced AphronICS
2 previous run R2 = 0.9987

0
0 2 4 6 8 10 12
1/2
t

Figure 3 - CSD for Wet vs. Dry Filter paper - Deaerated SE APHRON ICS

Spurt Loss Comparison Wet vs. Dry Filter Paper

9
8
wet filter paper
d=distance travel (mm)

7
6
dry filter paper
5
4
3
2
1
0
0.00 2.00 4.00 6.00 8.00 10.00 12.00
1/2
t

7
It is evident from Figure 3 that, when the paper is saturated with water at the start of the
test, the straight line plot for the dry filter paper is displaced upwards about one unit. The
spurt loss changes from negative to approximately zero, thus confirming the role played
by the interstitial fluid in the paper.
The effects of the nature of the filter medium and differential pressure are more complex.
Once a filter cake is well established, the filtration rate is not expected to be affected very
much by the nature of the filter medium (paper vs. core), since fluid flow is controlled
entirely by the permeability of the cake. Conversely, spurt loss is dominated by Darcy
flow, Equation (3), where k and h are now the permeability and thickness of the filter
medium, respectively, and µ is the viscosity of the whole mud. Each mud system has a
different viscosity profile, which will in turn produce a different rate of spurt loss. In ad-
dition, different concentrations and size distributions of particulate matter in the mud will
affect the spurt loss period (the length of time of the spurt loss phase). Thus, total spurt
loss, as given by the product of the spurt loss rate and spurt loss period, will vary from
mud to mud. The higher the permeability of the filter medium, the greater will be the
spurt loss and the variability in spurt loss from mud to mud. Thus, the effects of the na-
ture of the filter medium and pressure differential are expected to be manifested in a
higher spurt loss for the Core Leak-Off tests vs. the CSD tests. This will undoubtedly
lead to different correlations of Core Leak-Off vs. CSD for each mud system,4,5 as dem-
onstrated later in the present report.
The results for all of the Modified CST (CSD) and core Leak-Off tests are shown in Ta-
ble 1.
Table 1 - Summary of LSRV, CSD and Core Leak-Off Test Results

LSRV CSD @ 60 Leak-Off

Drilling Fluid System
(cP) min (mm) (mL)

FLOPRO

Sample 1: 2.25 ppb Viscosifier 82,382 9.5 101.8

Sample 2: 2.60 ppb Viscosifier 113,200 8.5 92.2

Sample 3: 2.85 ppb Viscosifier 168,400 7.0 69.3

Sample 4: 3.15 ppb Viscosifier 180,000 6.5 63.1

DRILPLEX

Sample 1: 0.18 ppb Polymer 6,400 12.0 20.3

Sample 2: 0.40 ppb Polymer 9,200 11.0 11.8

Sample 3: 0.80 ppb Polymer 12,400 10.5 11.0

Sample 4: 1.20 ppb Polymer 43,200 10.0 7.9

8
 Aerated SE APHRON ICS

Sample 1: 2.50 ppb Viscosifier 46,800 6.5 24.5

Sample 2: 3.50 ppb Viscosifier 89,600 3.5 14.9

Sample 3: 5.00 ppb Viscosifier 176,000 3.0 12.4

FLOPRO + 30 ppb 40-µm CaCO3

Sample 1: 2.25 ppb Viscosifier 62,387 6.0 2.9

Sample 2: 2.60 ppb Viscosifier 168,800 6.0 4.4

Sample 3: 3.50 ppb Viscosifier 206,400 6.0 4.1

Aerated APHRON ICS + 30 ppb

40-µm CaCO3

Sample 1: 5.0 ppb Viscosifier 169,000 2.0 1.2

Deaerated SE APHRON ICS

Sample 1: 2.5 ppb Viscosifier 17,996 7.8 156.8

Sample 2: 3.5 ppb Viscosifier 63,586 6.2 79.5

Sample 3: 4.2 ppb Viscosifier 105,000 5.0 61.0

Sample 4: 5.0 ppb Viscosifier 153,000 4.0 28.8

Deaerated APHRON ICS

Sample 1: 2.5 ppb Viscosifier 47,590 9.0 210.8

Sample 2: 3.5 ppb Viscosifier 76,784 7.0 39.6

Sample 3: 4.2 ppb Viscosifier 127,000 6.5 33.9

Sample 4: 5.0 ppb Viscosifier 166,000 6.5 24.6

Correlations of CSD and Core Leak-Off vs. LSRV

The effect of LSRV on CSD (see Table 1) is shown in Figure 4.

9
 Figure 4. CSD vs. LSRV for All the Systems

LSRV vs. CSD - Solids Free Systems

DRILPLEX R2 = 0.7986
12

10
R2 = 0.8426
CSD, 60 min (mm)

Standard Aphrons - 0% air FLOPRO (solids free)

8
R2 = 0.981
R2 = 0.9222
Super Enhanced Aphron -
6 0% air

R2 = 0.8854
2
Super Enhanced Aphron
15% air
0
0 20000 40000 60000 80000 100000 120000 140000 160000 180000

LSRV (cP)

All of the curves in Figure 4 follow power law trends fairly well, though it appears that
the curves cannot be unified into a single model, i.e. each fluid system appears to follow
a different power law expression. The APHRON ICS systems gives lower CSD values than
the DRILPLEX and FLOPRO systems. Aerating the SE APHRON ICS lowers the CSD even
more. The air in the APHRON ICS systems is present in the form of pressure-resistant
bubbles called aphrons, which have been shown to function as an invasion control agent.6
Figure 5 shows the correlation of Core Leak-Off vs. LSRV for all the data.
As was the case for the CSD correlations, Core Leak-Off appears to follow a power law
trend with respect to LSRV. Again, it does not seem possible to be able to unify the
curves; indeed, the curves appear to be considerably more scattered than were the CSD vs
LSRV curves. As discussed in the previous section, this is likely the result of spurt loss
being more variable for invasion into a core than for invasion into blotter paper. This is
especially evident for the DRILPLEX system, which exhibits the lowest Core Leak-Off,
yet the highest CSD. The sealing mechanism of this fluid involves a special polymer-clay
network that is thought to be particularly effective at reducing spurt loss.7

Core Leak-Off vs. CSD

Figure 6 shows the correlation of Core Leak-Off vs. CSD for all the systems.

10
 Figure 5. Core Leak-Off vs LSRV

Core Leak-Off vs LSRV - Solids Free Systems

220
R2 = 0.8267
200
Super Enhanced Aphron - Standard Aphrons - 0% air
0% air
180
R2 = 0.9031
160
Core Leak-Off (ml)

140

120
R2 = 0.9587
100
FLOPRO (solids free)
80

60
Super Enhanced Aphron
R2 = 0.7895 15% air
40
DRILPLEX R2 = 0.9283
20

0
0 20000 40000 60000 80000 100000 120000 140000 160000 180000

LSRV (Cp)

Figure 6. Core Leak-Off vs CSD

Core Leak-Off vs. CSD - All the Systems

220
Standard Aphrons - 0% air
200
R2 = 0.9767
180

160
Core Leak-Off (ml)

140

120
Super Enhanced Aphron -
0% air FLOPRO (solids free)
100
R2 = 0.9744 R2 = 0.9928

80

60
R2 = 0.9945
40
Super Enhanced Aphron R2 = 0.97
15% air DRILPLEX
20
FLOPRO + 30 ppb
Safecarb 40
0
0 1 2 3 4 5 6 7 8 9 10 11 12
SEA 15% air + 30 ppb
CSD, 60 min (mm)
Safecarb 40

11
As expected from previous discussions and borne out by Figure 6, there is a fair correla-
tion between CSD and Core Leak for individual fluid systems, but there is no unifying
correlation curve for all of them.
Addition of CaCO3 to the FLOPRO and the Enhanced APHRON ICS systems reduces both
Leak-Off and CSD. Likewise for addition of air to the Enhanced APHRON ICS.
From the results shown in Figure 6, it appears that CSD and Core Leak-Off for any given
fluid system correlate well enough to approximate the value of the Leak-Off of a particu-
lar system based on its CSD value.
Thus, the value of CSD measurements is expected to lie in monitoring of fluid invasion
trends and evaluation of potential additive treatments.

Nomenclature
BHT = Bottom-Hole Temperature
CSD = capillary suction displacement (distance traveled by the fluid front)
CST = capillary suction time
LSRV = low-shear-rate viscosity at 0.06 sec-1

References
1. Fann Instrument Co.: Capillary Suction Timer Instruction Sheet, Part No.
E10280001EA, Rev. C, Houston, TX, 1995.
2. Darley, H. C. H. and Gray, G. R.: Composition and Properties of Drilling and
Completion Fluids, Fifth Edition. Gulf Professional Publishing, 1988.
3. “MI Drilling Fluids Engineering manual,” Revision No: A-0, Chapter 7 - Filtration
Control.
4. Lee, D. J.: “A Dynamic Model of Capillary Suction Apparatus,” J. Chem. Eng.
Japan, Vol. 27, No. 2, pp 216-221(1994).
5. Guan, J., Amal, R. and Waite, T. D.: “Effect of Floc Size and Structure on Biosol-
ids Capillary Suction Time,” Water Sci Technology, Vol. 47, No. 12, pp. 255-60
(2003).
6. Growcock, F. B., Khan, A. M. and Simon, G. A.: “Application of Water-Based
and Oil-Based Aphrons in Drilling Fluids,” SPE 80208, SPE Internat. Sympos. Oil-
field Chem., Houston, Texas, Feb. 5-8, 2003.
7. Fraser, L. J., Reid, P. I., Williamson, L. D. and Enriquez, F. P., Jr.: “Formation-
Damaging Characteristics of Mixed Metal Hydroxide Drill-In Fluids and a Com-
parison with Polymer-Base Fluids,” SPE 57714, SPE Drilling & Completion, p.
178 ff, Sept. 1999.

12
 APPENDIX A
Modified CST (CSD) Procedure

For fluids with very long CST’s – typically more than a few minutes for the fluid to
travel between the two conducting rings – the distance traveled from the sample cup
within an arbitrary time period (30, 60, 90 and 120 min was used in this work) provides
an accurate relative assessment of the permeability of the filter cake:
• Two 2-cm (20 mm) rules are attached to the top of the transparent cover (see Figure 7).
• The 1.8 cm opening of the test cylinder is placed against the filter paper.
• Five mL of the test mud is placed into the cylinder using a 5 mL syringe.
• The migration of the mud fluid is recorded every 30 minutes for 2 hours.
• The results are expressed in distance (mm), or CSD, versus time (min). At least two
readings from different points around the cylinder are taken at each time and averaged.

Figure 7. Modified CST (CSD) Apparatus

Results obtained with a deaerated APHRON ICS and an aerated APHRON ICS are shown in
Table 2. Sometimes the filtrate did not migrate uniformly in all directions, as noted by
the ranges in CSD.
Table 2. Some Results of Modified CST Test

Migration Distance CSD

Fluid 30 min 60 min 90 min 120 min

Deaerated APHRON ICS 2-3 5 - 5.5 6 - 7.5 7.5 - 8.5

Aerated APHRON ICS 2 3 3 -5 3-6

13
 APPENDIX B
Leak-Off Test Procedure

The apparatus is shown in Figure 8. The test procedure employs a constant Inlet Pressure
of 500 psig and no back-pressure (Outlet Pressure of 0 psig) and is carried out at the same
temperature as the CSD tests, i.e. ambient temperature:
• Heat oven to appropriate BHT.
• Apply 500 psig to the piston port.
• Close off piston port (where 500 psig will still be active).
• Open confining port and apply 500 psig.
• Open piston port (both ports will be open at this point).
• Continue to apply pressure until it reaches 500 psig above hydrostatic pressure.
• Apply appropriate reservoir pressure (Back Pressure).
• Open computer program and begin to collect data.
• Apply appropriate mud pressure via accumulator while valve to seal tester is shut.
• Open mud pressure valve to seal tester to start test.
• Collect for 30 min.
• Release pressures in reverse order of application.
• Results are reported as leak-of (in grams) of fluid on a digital balance. This is con-
verted to volume (mL) from the density of the leak-off fluid, the dead volume (wa-
ter between core and mud sample) is subtracted, and the result is reported as the
Net Leak-Off.
• The degree of invasion can also be calculated as

% Invasion = [ (Pore Vol. - Net Leak-Off)/ Pore Vol.] X 100%

14
Figure 8. Core Leak-Off Test Apparatus

15