3427

. . .

J$Z27

Relative Permeability Measurements Using Reservoir Fluids

NEC?AET-TIN M!J:<GA}{ c.c-I-Dm C( IU DrFf)vFt.?V QF<FA Ri_H lfti?[?~r~
rr-, mWL I--J. t ,.Lw . . .. . . . . . . . ..-. .-
MEMBER AIME CALGARY, ALTA., CANADA

ABSTRACT representative of the reservoir rock to characterize

the wetting equilibrium during the tests. Finally, a
Water-oil relative permeabilities measured using procedure was devised which, for the extracted
reservoir fluids and fresh, preserved cores are cores, yielded the original set of relative
shown to difler considerably from those obtained permeability curves.
routinely using refined fluids and extracted cores.
Upon saturating the extracted cores with the EXPERIMENTAL
reservoir jluias ana allowiiig :Liwi k3 ccme @
THE CORE
equilibrium, in this case for 6 days, the original
relative permeability curves were reestablished. The core was cut using lease crude oil in a
Pennsylvanian sandstone reservoir. Crude oil was
INTRODUCTION considered as the best coring fluid to preserve borh
reservoir nettability and the interstitial water. The
Ordinarily, relative permeabilities are measured
core was obtained from a pumping well that was to
using refined fluids and restored-state cores. On
be deepened 50 ft for improving the productivity
occasion, fresh core samples that had been flushed
index. The production string was 4%-in. casing and
with a refined oil, without any other cleaning or
had been cemented and perforated with the total
extraction, have been used. 1 To date, no relative
depth at 5,200 ft. Initially, a three-cone, hard-rock
permeability measurements have been reported
rotary bit was run on 2-3/8-in. drill pipe to drill out
using reservoir fluids and fresh preserved cores,
the cement plug and the casing flow shoe. Drilling
although a number of published studies have dealt
was continued for an additional 10 ft to cut new
with the influence of core handling l-s and other
formation and clean out the hole. For the coring
laboratory experimental factors 6-1 1 on results of
operation, the rotary bit was replaced by a diamond
displacement tests. This is not surprising. Special
core barrel having 3%-in. OD. De-gassed crude oil
procedures 3 have to be followed for obtaining,
containing no additives was used as the drilling
preserving, and handling native- state cores; and
fluid during both drilling and coring. This crude
companies are generally reluctant to permit any
had an API gravity of 35.5 (i.e., a specific gravity
procedures that may increase the expense or the
of 0.8473 gin/cc) and provided sufficient pressure
time required to complete a well. Consequently, againstthe formation. The intake pipe for the mud
suitable cores often are simply not available.
pump was positioned several feet above the bottom
Furthermore, only a very few of the petroleum
of a production-storage tank. This was done to
production res earth laboratories have the facilities
avoid picking up any sediments or asphalts that
for measuring interracial rension, contact angle and
may have accumulated at the tank bottom. The mud
relative permeabilities at the elevated temperatures
return line from the weH was diverted into a pit,
and pressures normally encountered in reservoirs. -.. -:4
and the return crude was nor recirculated to ZIVUKI
The following study provides, for the first time,
introduction of any oxygen into the well. The total
relative permeability data obtained with fresh,
quantity of the crude oil used was approximately
preserved cores and reservoir fluids at reservoir
400 bbl during the entire operation.
pressure and temperature. Measurements were also
When brought to the surface, the core was quickly
made routinely with refined fluids and extracted
canned in crude oil to minimize exposure to air. In
cores to afford comparisons. Advancing and receding
the laboratory, the core container was placed inside
contact angles were measured as a function of time
an airtight lucite box, which was fitted with sealed
with the actual reservoir fluids on a solid surface
gloves for sample manipulation from the outside. A
nitrogen atmosphere was maintained inside the box.
Original manuscript received in Society of Petroleum Engineers An approximately l-ft-long core piece was chosen
office May 8, 1971. Revised manuscript of SPE 3427 received
March 25, 1972. Q Copyright 1972 American Institute of Mining,
which, by visual examination, aPP=red to be
Metallurgical, and Petroleum Engineers, Inc, uniform. From each end, a l-in. piece was cut for
1Re ferences given at end of Paper.
rhe x-ray diffraction and mercury injection studies.
This paper will be printed in Transactions volume 253, which
The core used in the reIative permeability
.=i!; ~S.J=r 1572.

38 @fz7&z /f7z SOCIETY OF PETROLEUM ENGINEERS JOURNAL

measurements had a length of 10 in. and a diameter placed on the quartz surface and contact angles
of 2.06 in. Subsequent calculations gave a pore photographed using time-lapse photography until
volume of 65.5 cc and porosity of 12 percent. No no discernible changes took place in the contact
special efforts were made to keep the core at the angle. The contact angle that is measured in this
reservoir temperature of 138 F at all times; manner is called receding angle, OR, since the oil
however, the core was never below 70 F. is spreading over a previously water-covered
While still inside rhe lucite box, the core sample surface. To obtain the advancing contact angle,
was Inserted inside a. ~.-=-
-in. c. firriqu
------ 0 (~nside diameter 6A, a small voIume was withdrawn from the
of 2. I in. ) shrinkable Teflon FEP tubing. TO seemingly equilibrated crude oii drop. Photographs
prevent air from getting to the sample during the were taken as before.
sealing operation, the ends of the tubing were Contact angles were measured with precision
filled with surgical cotton, taking care that the goniometers on enlarged photographs of the drops,
cotton did not touch the core sample. The latter but were also compured by triangulations of the
was a necessary precaution to keep the cotton from drop images. The interracial tension was calculated
imbibing iiquids from the core. By rotating the by the sessile drop me thodl 2 from the shape of the
., . .
sample while an air-gun was moved lengthwise same drops used in the contact angle aetermliiatioii.
back and forth, the tubing was heated to
RELATIVE PERMEABILITY
apptoxlmately 220 F m a matter of a few minutes,
shrinking its diameter by about 24 percent and Relative permeabilities were measured at reservoir
forming a complete peripheral seal around the core. temperamre by the unsteady-state method using
The core itself is not heated appreciably during the constant volumetric rate. The superficial
operation, remaining nearly a t room temperature, displacement velocity, calculated as the volumetric
and there was no visible bleeding of any fluids injection rate divided by the tot al core
from it. This -is a simple, convenient method of cm ss-sectional area, was 1.16 ft/day giving
.. . --- L,w--r)o
core mounting and eliminates the need fV. =-rl..a ap~roximately 1 sq cm-cp/min. for the I-VP scaling
the core inside a nitrogen atmosphere during parameter. The following sequence of tests were
subsequent tests. For permeability measurements, made: (I) using reservoir fluids and the fresh,
the sealed core was held in a stainless-steel preserved core. After mounting the core in the
Hassler sleeve-type holder capable of withstanding Hassler holder, crude oil was flowed through it,
500 ~~i: This pressure, equivalent to twice the against a backpressure of 300 psi to dissolve any
saturation pressure of the crude oil at the reservoir free gas. -%. Lnls
. L- l.~---ea..a
P~cKpGsau4&
,
..~
=
nintained
~__.--. during
temperature, was ample to keep all gas in solution. permeability measurement to ensure that no gas
came out of solution. Porosity and initial
FLUIDS . . .
saturauons were calculate at die end of the test
Crude oil was obtained under anaerobic conditions from a mass balance on the dry and water saturated
from the flow line of a well in an undersaturat~d core, volumes of oil produced during the test, and
part of the reservoir and was recombined with its water recovered in boiling toluene extraction.
flowing solution gas. The viscosity of the Permeability at 100-percent water saturation was
reconstituted crude was 1.6 cp at reservoir measured to be 75 md. (2) using synthetic fluids
temperature. A high pressure trap was installed on and the extracted core. The core was extracted
the flow line to collect the small amount of water first with boiling benzene, then toluene, and was
being produced with the crude oil. The refined dried with a flow of warm, clean nitrogen. (3)
oil was a mixture of heptane and mineral oils to Finally, the core was resaturated with the reservoir
match the viscosity of the crude. Synthetic brine fluids, allowed to stand for 6 days to establish
having a chemical composition identicai to the contact angie
__. :l:k A..
eqtI11WL4Ulm,
=~~ ~~~ ~~i&3tiVe
produced water, was prepared in the laboratory and permeabilities remeasured using the reservoir
equilibrated with the crude oil before use.
fluids. Tests 2 and 3 were repeated to determine
CONTACT ANGLE AND lNTERFACIAL TENSION reproducibility.

Contact angles were measured on quartz crystal MERCURY INTRUSION AND X-RAY DIFFRACTION
surfaces which had been polished to approximately The mercury intrusion curve was obtained using
3,000 ~ flatness. Quartz represented the reservoir a slightly modified Aminco porosimeter, motor-driven
rock, ivhieii was e==-.. ----~ ~ii~ca.
.==.=n~;-llv The crystals withstanding 15,000 psia. The
...---
mdel , capable of
were boiled in 30 percent volumetric hydrogen porous rock, which had a bulk volume of 30 cc, was
peroxide solution and subsequently rinsed thoroughly out-gassed at iu micron vacuum. The tii~iCWy
in double-distilled water. They were stored in water level remained visible through a precision bore
inside quartz absorption cells until required for capillary and, therefore, intrusion volumes were
measurements. read directly from the mercury level.
To measure the contact angle, a quartz crystal X-ray diffraction studies were made following
was placed inside a titanium, high-pressure optical standatd powder diffraction techniques. Samples
cell capable of withstanding 2,000 lb. Measurements were flushed either with heptane or extracted with
were made at bottom-hole pressure of 1,200 psia boiling benzene and then dried prior to diffraction
and temperature of 138 F. A drop of crude oil was
measurements.

OCTOBER, 1972 S99

 RESULTS AND DISCUSSION used in the design. For the reservoir studied,
the predictions for future performance wouid have
Water-oil relative permeability ratios obtained
been overly optimistic if the relative permeabilities
with natural reservoir fluids in fresh, preserved
measured using refined fluids and extracted,
core, and with synthetic fluids in the extracted
restored state cores were used.
core, are shown in Fig. 1. lt ~afi be sem tk~t at
In an effort to expiain these differences, factors
all water saturations the relative permeability
that can affect the relative permeabilities were
ratio is higher in the former case. Although it is
studied. The mercury intrusion and the x-ray
generally agreed that the use of reservoir fiuids
diffraction curves for the natural and extracted
gives relative permeabilities that are more
cores were remarkably identical and within
representative of the reservoir than when refined,
experimental error, indicating that the cleaning
synthetic fluids and extracted cores are used, no
procedure had neither changed the pore size
results have been reported to date on the differences
distribution, nor modified the small quantity of
that may result. The relative permeability ratio,
kaolinite and illite that were present in the core.
krJkro, is directly proportional to the The interracial tension between the crude oil and
instantaneous water-oil ratio, Fwo. To obtain the
connate water was 28 dynes/cm, while between
cumulative water production during an incremental
the refined oil and the synthetic brine it was 32
oil production of ASO, one integrates numerically dynes/cm. This small difference is not expected
( Fwo x 8S.) over the saturation interval ASO using
to have a sensible effect on the recovery9 and,
small desaturation steps. Clearly, for the given hence, on the relative permeability measurements.
level of oil recovery, the predicted cumulative The interracial areas of several crude oil drops,
water production will be greater if the relative suspended in reservoir brine, were increased and
permeability ratio obtained with the natural reservoir decreased approximately 10 times. No rigid
fluids is used; and conversely, if it is planned to interracial films were formed; thus, the nature of
abandon the operations when a certain water-oil
the displacement was free of such effects. The
ratio has been reached, smaller oiI recoveries wiH
viscosities of the synthetic fluids had been matched
be predicted. Other considerations, such as the
to those of the reservoir fluids; all displacements
cumulative water to be injected, number of were carried out at the same constant flow rate.
injection wells, design of the injection system,
The connate water saturations were the same in
well lifting and field separation equipment, and
both tests, being about 18 percent PV. In the case
water disposal will be affected, depending on
of the extracted cores, a 300-cP refined oil was
which of therelative permeability ratio curves are
injected into the water saturated core at a high
ra~e, chosen by trial and error, to achieve the ii
?.000 t A percent saturation. The viscous oil was then
completely displaced out by the test oil. Other
experimental variables, such as temperature and
the backpressure were held as nearly identical as
possible. Therefore, the differences in nettability
and the consequent initial water distributions are
believed to have caused the change in the relative
permeability.
In Fig. 2 advancing and receding contact angles
for the natural reservoir fluids on a quartz surface
are shown. These results defined the manner in

NOTATION

0 . . ...0 vedcore.
pu:w~; resew,,

_ Cleaned core , pur, f,ed

flu,ds
Cleaned core, reser vow
flutds

o,~
20

wATER
30 40

SATURATION ,
50

PERCENT
60

PORE
70

VOLUME
80 90

FIG.
30

2
L/

TIUI ELAPSED
I
m
SS0.

INFLUENCE
MWW 1-

OF INTERFACE
I
m
CRIJMOIL-WATER

AGE ON
IMTEWU3
1
1.0.33

, MWUIES
4
fm300

FIG, 1 EFFECT OF FLUIDS AND LABORATORY ADVANCING AND RECEDING CONTACT ANGLES @
HANDLING ON RELATIVE PERMEABILITY RATIO. = 1,200 PSIA; T = 138F).

400 SOCIETY OF PETROLEUM ES GINEERS JOURNAL

 .. .. . :-.aa ----
.-A
which contact angle equlllmlum w-as atta...~ angle on relative permeability relationships of
ensured that the relative perrneabilities were Torpedo sandstone. They used a miici sodium
measured at equilibrium. The advancing contact chloride brine solution and a refined oil to which
angle reached a final value of 87 in approximately barium dinonylnaphthalene sulfonate had been
6 days from the time that water was made to added in varying amounts to control the contact
advance on a surface that previously had been angle. It is significant that, for this reservoir, the
covered and equilibrated with the crude oil. Water effect of using reservoir fluids in the relative
from rhe cell, made of titanium, was ariaiyzed for permeability measurements was similar to the
12 elements, including Fe, Mn, Cr, Ni, Mo, using adding of a strong surface active agent to refined
atomic adsorption. No contamination was detectable. laboratory fluids. Therefore, notwithstanding the
Also, a final contact angle of 85 was measured at additional expense and experimental difficulties,
ambient pressure and 138F using de-gassed crude reservoir fluids should be used in the measurements
oil in an all-silica and polytetrafluoroe thylene of relative permeabilities, particularly for formations
contact angle apparatus. Thus, it is felt that the that are suspected of not being strongly water-wet.
angles observed were free of metallic contamination The curves in Fig. 3 resemble those given by
effects. With the synthetic fluids the advancing Morgan and Gordon, 11 in their Fig. 6, for the
contact angle reached an equilibrium value of 33 relative pernieabilities of fine-grained and medium-
in a few minutes. These angles are marked on the grained cores. In other words, for this formation,
relative permeability curves ro which they apply. changing from reservoir to synthetic fluids had an
The receding contact angle for the natural reservoir effect on relative permeabilities similar to the
fluids was 74 indicating a hysteresis of about 13. differences observed between medium- and fine-
The individual oil and water relative permeabilities grained formations. On decreasing the contact
are shown in Fig. 3. At any water saturation the angle, the rock is behaving as if it were composed
relative oil permeability is smaller and the relative of finer grains. This is a change in the right
water permeability is greater for reservoir fluids. direction, because in strongly water-wer rocks,
Thes,e ~sults agree with the earlier work of Kyte water flows principally through the smaller of the
et tiL., in ~,hich ~he~ showed that the strongly pores. Thus, if no attention is paid to the use of
water-wet cores flooded more efficiently than reservoir fiuids, it is p~~~ibi~ to obtain relative
cores of intermediate wearability. The results also permeability curves with characteristics of an
agree with the recent work of Owens and Archer, 10 entirely different formation.

,\
who studied systematically the effect of contact Starting with the assumption that the relative

:\
permeability of the extracted core had been modified
because of nettability change, it was decided to
. ., test the possibility of reestablishing the original

r
relative permeability curves. The core was saturated
NOTAT ION
with refined oil and water, the latter occupying 18
09

:: \ c,. . . . . o ::u:y~rved core, reservow percent PV as before. The refined oil was then
_ Cleonad CWE , pur,fmd
displaced with crude oil and rhe core allowed to
: \
08 flu, ds stand for 6 days, the time required to attain an
;: \ m c,!~g.~ Co,e . ,eservolr
Ilunds
~quiiibrium contact angle. After this time period,
, \ the relative permeabilities were remeasured and are
07 T= 438 F
so :, \ shown by the continuous solid lines in Figs. 1 and
1 ~\
3. As can be seen, these duplicate the original
relative permeabilities. The cyc Ie was repeated
once again and within 1 percent agreement the
relative permeabilities of the extracted (OA = 33)
and ~Iig~nai cores (6A = 87) were reprodu~ed.
These limited result; point to the potentiai
possibility of ensuring that the relative permeability
characteristics of a porous rock in the laboratory
would resemble rhose of the fresh, preserved,
.i~~ .
reservoir rock. Mungan 4 and Schmla, USiiig
. . . ,
imblbiuon anti capiiiaiy pzessuEe tneasurements,
_ respectively, have reported the reestablishment of
u
a the original nettability of weathered cores. Since
representative reservoir fluids are more easily
obtainable than cores and only weathered cores are
available from a great many reservoirs, the
possibility of restoring unpreserved cores to
.-
0 10 20 30 40 50 60 70 reservoir conditions should not be overlooked in
wATER SATURATION , PERCENT PORE VOLUME laboratory measurements.
FIG. 3 EFFECT OF FLUIDS AND LABORATORY
HANDLiNG ON RELATIVE PERMEABILITIES.

OCTOBER, 1972 4al

 SUMMARY Cleaning on Water-Oil Relative Permeability, %ori
Monthly (1958) Vol. 22, No. 10, 26.
The present study with one reservoir has shown 6. Geffen, T. M., Owens, W. W., Parrish, D. R. and
that in measuring relative permeabilities one should Morse, R. A.: ({ ExPeriment~ Investigation of Factors
Affecting Laboratory Relative Permeability Measure-
use re~rvoir fluids and fresh, preserved reservoir
~ents,>~ Trans., AIME (1951) VO1. 192, 99-110.
cores. Using refined fluids and extracted cores can
7. Kyte, J. R., Naumann, V. O. and Mattax, C. C.:
yield wrong results and is not recommended. A $,Effect of Reservoir Environment on Water-Oil
possibility is suggested for ensuring that the Displacement, J, Pet. Tech (June, 1961) 579-582.
correct relative permeability curves are obtained 8. Colpitts, G. P. and Hunter, D. E.: Laboratory
when using dry and extracted cores. Displacement of Oil and Water Under Simulated
Reservoir conditions, j, Can. pet. Tech (1964)
REFERENCES Vol. 3, No. 2, 66.
9. Mungan, N.: %iterfacial Effects in Itnmiacible
1. Richardson, J. G., Perkins, F. M., Jr. and Osoba, Liquid-Liquid Displacement in Porous Media, Sot.
J. S.: Differences in Behavior of Fresh and Aged Pet. Eng. J. (Sept., 1966) 247-253.
East Texas Woodbine Cores, Trans., AIME (1955)
10. Owens, W. W. and Archer, D. L.: The Effect of Rock
VOL 204, 86-91. on Oil-Water Relative Permeability
Wettabilit y
2. Jennings, H. Y., Jr.: t<Surface Propetiies of Natural
Relationships, j. pet. Tech (~iiiY, 19?1) f)?~=8?8.
and Synthetic Porous Media, prod. Monthly (1957)
11. Morgan, J. T. and Gordon, D. T.: fnfluence of Pore
Vol. 21, No. 5, 20.
Geometry on Water-Oil Relative Permeability, J.
3. Bobek, J. E., Mattax, C. C. and Denekas, M. 0.: Pef. Tech. (Oct., 1970) 1199-1208.
t Reservoir Rock Nettability
Its Significance and
12. Lefebvre du Prey, E.: M6thode dInte~retation de la
Evaluation, Trans., AIME (1958) Vol. 213, 155-160.
Goutte Poa6e pour Mesurer la Tension Interfaciale et
4. Mungan, N.: [ Certain Nettability Effects in lAngle de Contact, Rev. inst. Franc. Petrole (1968)
Lab&atory Waterfioods, J. ~et. Tech, (Feb., 1966) Vol. 23, No. 3, 365.
247-252. 13. Schmid, C.: Nettability of Petroleum Reservoirs,
5. Jennings, H. Y., Jr.: #~Effect of Laboratory Core Erdol und Koble Erdgas Petrocbemie (1964) Vol.
17, No. 8, 605.
***

402 sOCIETY OF PETROLEUM ENGINEERS JOURNAL