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T.P.

3052

USE OF CENTRIFUGE FOR DETERMINING CONNATE


WATER, RESIDUAL OIL, AND CAPILLARY PRESSURE
CURVES OF SMALL CORE SAMPLES

R. L. SLOBOD, ADELE CHAMBERS, MEMBERS AIME, AND W. L. PREHN, JR., ATlANTIC REFINING CO., DAllAS, TEX.

ABSTRACT saturation may have equal value, (compared to use of discs)


but more work is required to establish this point." This work
The centrifuge has been found to be an extremely useful was followed in 1945 by a more detailed study' in which the
tool for determining capillary pressure curves and for estab- concepts of this experimental work were more clearly enun-
lishing connate water and residual oil in small core plugs. The ciated. A method for calculating saturation for any given
use of the centrifuge for determining the properties of small speed of rotation based on the observed volume of water dis-
core plugs has been discussed in the literature,'" but practi- placed was developed and a wider application of the method
cally no experimental evidence has been presented justifying was suggested.
the use of this method in preference to other methods (mainly The absence of any subsequent pertinent literature on this
disc method) now in use. Data have been accumulated and subject is interpreted as indicating that no additional work
are now presented demonstrating the advantages of the cen- has been completed to substantiate or deny the earlier claims
trifugal method, some of which are: (1) rapid establishment and suggestions of promise contained in the original papers
of equilibrium, (2) excellent precision yielding very repro- on this subject. One purpose of this report is to provide evi-
ducible results, (3) availability of high pressure differences dence designed to establish the practical value of centrifugal
between phases, (4) simple operational procedure, and (5) methods in determining core properties such as connate water
ability to establish connate water, residual oil, or to obtain and capillary pressure curves. It is also our purpose to suggest
complete capillary pressure curve in one day or less. A com- a broadening of the scope of this tool to include determina-
mercially available centrifuge capable of speeds up to 3,800 tions of residual oil by gas or water drives.
rpm, and a high speed attachment providing a maximum rate
of rotation of 18,000 rpm were used in this work in conjunction
with core holding tubes designed specifically for this applica-
tion. THEORY AND PRACTICE IN USE OF
In view of the outstanding advantages associated with the CENTRIFUGE
use of the centrifuge the conclusion has been drawn that this
method should be used in place of the more tedious, slower, Hassler and Brunner' have clearly presented the basic con-
and less reliable disc method for determining capillary pres- cepts involved in the use of the centrifuge by relating the per-
sure curves and for establishing connate water and residual formance of a small core in a field of high acceleration to the
oil in small core plugs.

INTRODUCTION
The need for accurate values of connate water, residual oil,
and capillary pressure curves in reservoir engineering has
been recognized for many years, and the extent of the effort
devoted toward solving these problems is reflected in the large
number of papers'-ll which have appeared in the literature
during the past decade. Most of the methods discussed in the
recent literature employ a porous disc as a semi-permeable
membrane to separate two immiscible phases and make pos-
sible the application of an explicit difference in pressure be-
tween two phases in the core. Thus, in the determination of
the capillary pressure curve the wetting phase (water) is
displaced by the non-wetting phase (air or oil).
Several investigators'2 have used centrifugal forces to de-
velop pressure differences between phases. As a result of the
first work' in this field the conclusion was reached that "the
more rapid centrifugal method for - measuring irreducible

1 References at end of paper.


Manuscript received in the office of the Petroleum Branch August 16,
1950. Paper presented at the Petroleum Branch Fall Meeting in New Or- FIG. 1 - CENTRIFUGE SHOWING COil, STROBOSCOPE, AND TWO
leans Oct. 4-6, 1950. TYPES OF CORE HOLDERS.

Vol. 192, 1951 PETROLEUM TRANSACTIONS. AIME 127


T.P. 3052 USE OF CENTRIFUGE FOR DETERMINING CONNATE WATER, RESIDUAL OIL, AND
CAPILLARY PRESSURE CURVES OF SMALL CORE SAMPLES
uation of critical gas saturation, may also be possible by
proper utilization of the centrifuge.

Trunnion Ring
Apparatus
A standard International Size 2 Centrifuge modified with a
Core cooling coil and compressor was used in this work, operating
at various speeds up to 3,800 rpm (Fig. 1). The refrigerated
model PR-1 Centrifuge might be preferable since slightly
higher speeds are possible with this model. The centrifuge
was mounted on a portable vibration less stand made by Inter-
Removable Core- national. For extremely high speeds (18,000 rpm with result-
Supporting Platform ing acceleration of 25,000 gravities at tip of centrifuge tube)
a multispeed attachment with four place conical head was
used. This attachment is belt driven and rotates 4.6 times the
~~-=-;:;;;;-:::?;T/--Oisplaced Fluids speed of the central driving shaft. For speed control a large
Variac was found to be superior to the variable resistance
generally supplied with the centrifuge. The tachometer sup-
plied with the centrifuge and a calibrated stroboscope (Type
FIG. 2 - CORE HOlDER WITH BOTTOM WELL FOR DISPLACED flUIDS
FOR USE IN NORMAL SPEED CENTRIFUGE. 631-B Strobotac - General Radio) were used to measure
rotation speeds.
A number of special tubes for supporting the core specimen
were designed with strength consistent with the large forces
known action of gravity drainage in a vertical column of uni- developed at the high speeds of rotation. The simplest holder
form composition. If long uniform cores were available from used in these studies consists of a straight cylindrical tube
all reservoirs, and allowing sufficient time for equilibrium, con- with a bed of sand to support the core. This system with water
nate water values and the capillary pressure curve itself could surrounding the core is ideally suited for establishing resid-
be obtained by analyzing sections of a core at various heights ual oil by water drive in a core saturated with oil and con-
above the free water level. The pressure difference between the nate water. Such a tube can be used in both the conventional
phases in this case can be calculated by the basic equation, trunnion rings for normal centrifugal speed, or in the special
=
!:::,.P (P, - P2) gh, where !:::,.P is the pressure difference between high speed attachment. Merely to establish connate water
the phase 1 and 2, at height h above the reference level, P, saturation in a core, or to establish residual oil by air drive,
and P2 the densities of the two fluids present in the porous the holder shown in Fig. 2 is used in the normal speed centri-
medium and g, the acceleration due to gravity. fuge. These tubes contain a well at the bottom where displaced
In the centrifuge, however, only a short core is used, but liquid is collected and kept out of contact with the core. The
large pressure differences between the phases are developed special holder shown in Fig. 3 is used in establishing connate
in spite of a small value of h because of the extremely high water in core samples that require the higher pressure differ-
acceleration which is developed at high rotational speeds. The ences between the phases attained by the higher rate of rota
relationship (developed below*) expressing the pressure dif tion in the high speed attachment. The special design is re-
ference between the phases in psi at any height h in the core quired because of the angle at which the tube is held in the
rotating at speed n (rpm) with a radius of rotation r is !:::,.P = high speed head. Finally, the holder shown in Fig. 4 is used
1.578 X 10-' (P, - P2) n'rh (p in g/ em", rand h in em). for obtaining the capillary pressure curve for the system air
If a core containing water is rotated at an appropriate speed displacing water, the displaced water being measured in the
in a tube containing oil or air around the core, the water can pipette contained in the lower end of the tube.
be displaced down to the connate water value while air or oil
replaces the displaced phase. If a capillary pressure curve is Aluminum Sfa fir
desired intermediate speeds of rotation are used, the speed
and volume of displaced water being measured for each equi-
librium state. Similarly, if a residual oil value is desired, the
core containing connate water and oil is placed in a tube
surrounded by air or water and rotated in the centrifuge.
When air is the displacing phase, the displaced oil accumu-
lates in a small chamber at the bottom of the tube. When
water is the displacing phase, the displaced oil accumulates
on top of the water layer. Other determinations, such as eval-

'If'
*The basic equation for acceleration in the centrifuge is a = -. If n
r
21T rn 47r2rn2
. - th n v - - - and a = - - . Dividing this equation by g
IS m rpm, e - 0' 3600
to et '. the ratio be~ween the acceleration.i~ the ct;:fltrifug~ and !hat of
gra;ityU gives g' == 0.0000111 n r. By comb~nlng thIS ~quatIon WIth .,the
2
equation for !'oP = (PI - P2) gh and convertmg th" umts from g/cm- to
psi by multiplying by 0.01422 we get !'oP = 1.578 X 10-' (Pl -p,)n'rh. The
only instance in which the value of 6,P need be known accurately is in t!:e
determination of the capillary pressure curve. In these cases a 0.8 ratio
between the radii from the center of the system to the .top of the core
and to the base of the core w~s always excee.ded. as specIfied !ay ~assler. FIG. 3 - CORE HOLDER WITH BOTTOM WElL FOR DISPLACED FLUIDS
In other cases. this equation gIves an approXImate answer whIch IS accu- FOR USE IN HIGH SPEED CENTRIFUGE.
rate enough for most purposes.
PETROLEUM TRANSACTIONS, AIME Vol. 192, 1951
128
R. l. SLOBOD, ADELE CHAMBERS AND W. l. PREHN; JR. T.P. 3052

HOLDER BODY WINDOW The storage space below the supporting plate has sufficient
volume to hold all of the displaced water without allowing
the collected water to contact the bottom of the core. At a
speed of 3,800 rpm a 6.P between phases of 14 psi is devel-
oped at the center of the core for the oil-water system and 50
psi for the air-water system. Generally, one hour is sufficient
time for the system to come to equilibrium. In some cases it
is desirable to mount the core in capillary contact with a disc
% in. to %, in. thick. In this way, the end effect is transferred
to the disc and a slightly greater net 6.P between the phases
TUBE BODY
operates to drive the core down to connate water more effec
FIG. 4 - CORE HOLDER FOR USE IN OBTAINING CAPillARY PRESSURE tively. No trouble with capillary contact is experienced here
CURVES. because of the extremely large force acting to push the core
Since the circuit driving the stroboscope did not operate into contact with the disc. Kleenex is also used here to im-
below 600 flashes per min, at rotatiooal speeds below 600 rpm prove the quality of contact.
a special contractor using a cam driven directly by the shaft To determine residual oil by air drive, the core plug con-
of the centrifuge was used to operate a microswitch. The open- taining connate water and oil is placed in the tube shown in
ing and closing of this switch was used to initiate the flashing Fig. 2. With air as the only other component present in the
of the light source. tube, the system is rotated at 3,800 rpm for approximately
one hour. The displaced oil is collected in the bottom of the
tube. The residual oil may be calculated from the weight of
Procedure
the core knowing the connate water value. Generally, a direct
A core plug, approximately 1 in. long and % in. in dian1- determination using the vacuum distillation technique is used
eter is used in all of the studies discussed. The core sample to measure directly the residual oil.
is always cleaned and then saturated with a sodium chloride Residual oil by water drive is determined by placing the
brine (approximately 5 per cent). From the dry weight and core containing connate water and oil in a bed of coarse sand
the saturated weight the porosity is determined. The saturated in the tube shown in Fig. 3. The core is then covered with
core is then subjected to one or more of the operations de- water, the tube closed, and then centrifuged for one hour
scribed below. Whenever possible, a material balance ap- in the high speed attachment at 18,000 rpm.
proach is used to evaluate each process, but in all cases where The capillary pressure curve for the system air displacing
accurate values are required, the final saturation of the core water is obtained using the special core holder shown in Fig.
plug is determined directly, either by weighing, which is 4. The fully water saturated core is placed in the holder, and
accurate when one of the two phases present is air, or by the unit then placed in the centrifuge. The system is rotated
direct analysis using vacuum distillation to remove the satu- at a number of different speeds selected to cover the range
rants and a liquid nitrogen trap to collect and measure the of pressure differences between phases required for the par-
liquid saturants from the core. Final dry weight is used to ticular core. At each speed setting, the rate of rotation is
check on loss of solid from the core. The temperature of the maintained constant until no additional water is observed to
0
centrifuge is maintained at approximately 75 F to eliminate collect in the pipette. In accordance with Hassler's recommend-
significant errors from evaporation. ation, the speed of the centrifuge should not be allowed to
The method used to establish connate water saturation in clecrea;:e at any time during the run. Pipettes are read to the
the cores depends upon the required pressure difference be- nearest 0.01 cu cm while rotating by use of light flashes from
tween the phases for the particular core and on the choice of a stroboscope. Generally, 30 to 45 minutes is sufficient time to
air or water as the displacing phase. For the tightest cores, establish equilibrium at each point. A complete curve with
the maximum pressure difference between phases should be 6 or 8 points may be obtained in one working day. In actual
used. To accomplish this the high speed head and the tube practice eight cores are run simultaneously. Subtracting the
shown in Fig. 3 to contain the core are used. The use of air volume of displaced water from the original water content
as the displacing phase will provide the maximum 6.P between
gives the average saturation, -;, in the core. The correct value
phases, but some difficulty in reproducibility has been experi-
of saturation to use in plotting the capillary pressure curve is
enced in this system. In most studies using the high speed head
determined by using the method suggested by Hassler' in
oil has been used as the displacing phase with excellent re-
sults. Generally, the water saturated core is placed in a bed 1.91r---.--,--,-..,-,"TTTr----r-,-,-,-;-n-r,---,-....---r-;-TTm
of 40-70 mesh sand (to prevent splitting of core from high CORE
COL
PERMEABILITY
1400md.
local pressure) which is confined with a fine monel screen and
supported by the shelf shown in Fig. 3. The displacing oil
1.8
H
COM
AVT
AVL
1140md.
2710 md.
2210 md.
phase is added, and the unit closed with a cap containing an
O-ring seal and a small vent hole. The pairs of tubes are bal-
~ 1~'L__1-tjJ~~~~~~~~~~~~~~~~
anced to within O.lg, inserted into the high speed head, and 5 V V
then rotated at 18,000 rpm (6.P between phases at midpoint ~ 1.6'1--~-i_Wc_1_.w.~-/---,4----jf--I--++I+i+----+-+-+-H++-H
of core is approximately 105 psi) until equilibrium is at- ~ /
tained. The time required for most cores is of the order of
one hour, although very tight cores may require several hours II 1.5t=ttttjjjt:::t~~W=~jjjjjjj
to approach equilibrium even closely. For looser cores which 1.41---l---1---1-+++++l--+---t--t++++++--+--+-++t+H-I
do not require excessively high pressure differences, the
simpler tube sho'Yn in Fig. 2 can be used in the normal speed
1.3!J.-.---L#~~-lz.!VJ'+;'. QYo-Y--L,QYd-c-ky.)-H
cji-!:'ylf----l..y-:d--lo/-d-ff:lobl
head centrifuging 4 or even 8 cores simultaneously using
,1-\.

TIME (HOURS)
standard equipment to hold the core tubes. In this normal
speed operation the core is placed on a monel platform which FIG. 5 - INTERSTITIAL WATER SATURATION IN CORE CENTRIFUGED AT
is supported on a shoulder cut into the wall of the monel tube. 2,300 RPM USING WATERAIR SYSTEM.

Vol. 192, 1951 PETROLEUM TRANSACTIONS, AIME 129


T,P. 3052 USE OF CENTRIFUGE FOR DETERMINING CONNATE WATER, RESIDUAL OIL, AND
CAPillARY PRESSURE CURVES OF SMAll CORE SAMPLES
50
rpm) apparatus to displace water by air have been discon
tinued. Results obtained were generally low and somewhat
z4 0
. m.
variable. Evaporation losses and trouble from other causes
o
~ such as cavitation may be the explanation. 'This system does
a: /
~3 0""--- provide the maximum .6.P between phases and may be useful
;a for extremely tight cores when all of the extraneous variables
a:
\oJ
AHU :: . md are properly controlled.
20

.i 10
The time required for establishing equilibrium when dis
placing water by oil in the high speed centrifuge (18,000 rpm)
is shown by the data in Table 1. These six cores represent five
different fields. The more permeable cores (several hundred
0 md) apparently attain equilibrium in one or two hours. Cores
" '
""TIME (HOURS)
-oY ~ ~ -9 of intermediate permeability (15 to 100 md) apparently are
FIG. 6 - STUDY OF TIME REQUIRED FOR RELATIVELY TIGHT CORES TO close to equilibrium after two hours of centrifuging, but the
COME TO EQUILIBRIUM IN HIGH SPEED WATEROIL SYSTEM. amount of data is insufficient to make a sweeping generaliza.

which the slope of the curve for Z; plotted against Z gives Table 1-- Water Content as a Function of Centrifuging
the value of saturation consistent with Z, where Z is the pres Time -- Water - Oil System at 18,000 rpm
sure difference between the phases at the top of the core Time in Centrifuge-Hours
(maximum .6.P in core). The value for Z is calculated assum-
Core K(md) 0.25 1.0 2.0 8.0 20.0
ing a constant value for acceleration from top to bottom of
core calculated on the basis of the radius of rotation meas- AJN 2.1 39.4 36.2 33.5 32.2 31.0
ured from the center of the centrifuge to the center of the core. AHD 2.7 33.5 30.1 27.8 27.3
APT 16 35.4 34.3
BVR 67 27.4 26.5
RESULTS
ED 458 26.4 26.4
Establishment of Connate Water: Air-Water AVX 885 13.0 12.0
and Oil-Water Systems
The time required for loose cores to come to equilibrium tion for this case. Extremely tight cores (2 md), however,
using air to displace water at 2,300 rpm (maximum .6.P be definitely are not at equilibrium after two hours of centrifug-
tween phases =
35 psi) was found to be approximately one ing. The above results on two tight cores are shown in Fig. 6.
From these curves it is evident that the cores are close to
hour. The rate of approach to equilibrium is shown in Fig. 5.
In the four cores studied with permeabilities ranging from equilibrium at 20 hours, and it is probable that a tenfold
1,140 md to 2,710 md, no change in fluid saturation was ob increase in centrifuging time would produce no more than one
served after one hour of centrifuging. These data were ob or two per cent decrease in water saturation. These data also
tained in the equipment used to obtain capillary pressure indicate that the more practical time of eight hours gives a
curves, the volume of expelled water being measured directly. reasonably close approach to the correct connate water value.
Other data, not presented, indicate that most cores of 200 md The reproducibility in connate water values obtainable using
permeability or higher will attain or closely approach equi. the centrifuge are shown in Table II. The reproducibility in
librium in less than two hours for the system air-water at most cases is within a few tenths of one per cent of the pore
speeds of 3,800 rpm. Studies using the high speed (18,000 space. This result is superior to any previous results observed
in this laboratory using the disc method or a flowing oil phase
100
100
,
80~----~------+------+--~~~----~
80 /.
/.
0:0
wo 0:0
I-:I:
I-
wo
I-:I:
~ w 60~-----+------1-----~~----~------~
~ .' ~ ~ 60
...J

1/.. .
~
...J

.
...J...J
~~ 5
t=:;) I-C)
~ ~ 40~------+-------~--~~-i--------r-------;
wO:
1-1-
~:;)

~ ~ 40
.
"1/ .. . .. . .
~~ 1-1-
~~
~o
20~-,~~------r------+------+-----~
a-! 20

20 40 60
-/0 INTERSTITIAL WATER
80 100
V" 20 40 60
INTERSTITIAL WATER
0/0
80 100
CAPILLARY PRESSURE METHOD CAPILLARY PRESSURE METHOD
FIG. 7-CORRELATION PLOT OF INTERSTITIAL WATER BY CENTRIFUGAL FIG. 8 - CORRElATION - INTERSTITIAL WATER BY CENTRIFUGE VS.
METHOD WITH INTERSTITIAL WATER BY CAPILLARY PRESSURE METHOD. CAPILLARY PRESSURE METHOD FOR TIGHT CORES.

130 PETROLEUM TRANSACTIONS, AIME Vol. 192, 1951


R. l. SLOBOD, ADElE CHAMBERS AND W. L. PREHN, JR. T.P. 3052

(dynamic method) to displace the water. The reproducibility 32


has been so good that small changes in the core which devel-
oped with use, such as changes in the wetting characteristics CORE No. AWA
Ka=494md . =22.5%
leading to changes in the connate water value, can be detected.
The checking values cited in Table II were generally obtained 28 ~- CENTRIFUGE DATA 1st RUN
on successive days. When results obtained over an interval of , 0- CENTRIFUGE DATA 2 nd RUN
several months with other operations performed on the core
X=DISK METHOD
were compared, differences of the order of several per cent of
the pore space were observed (Table III). These differences 24
are obviously significant in view of reproducibility to within
several tenths of one per cent for unchanged cores.
To obtain reliable connate water data the pressure difference CD
Q.
between the phases developed in the centrifuge must be suffi- ~,

"-'
cient to displace the water from the pore spaces. Consequently, I.&J
either the system which develops the maximum b,P between a::
phases must be used in all cases (not always desirable since :>
V)
this involves the use of the high speed head which holds only V)
I.&J
four cores at one time and requires more careful watching of a:: 16
the equipment) or the system used must, be selected on the Q..

basis of known core properties (permeability unless capillary >- ,


size distribution is known). The various systems used, listed in a::
ct
order of decreasing effectiveness in displacing water from the -.J 12
core are shown in Table IV. End butts act to transfer the zone -.J
of minimum l::,.P between phases from the lower end of the Q..
ct
core to the porous medium used for the end butt. Consequently, o
the zone of high water saturation, generally called the end
8
effect, is largely removed from the core and put into the end
butt. In addition, the height of the liquid column is increased
by the thickness of the butt leading to a slightly higher value
for b,P between the phases throughout the core. ~
The b,P between phases is 0 psi at the bottom of the core,
where 100 per cent water saturation is assumed to exist, and
4
,
it increases to a maximum at the top. The value of l::,.P at the X
X
0
o 0.2 0.4 0.6 0.8 1.0
Table II - Reproducibility of Connate Water Values:
BRINE SATURATION
Air - Water and Oil - Water Systems
Connate Water Values by Analysis
FIG. 9 - CAPILLARY PRESSURE CURVE SHOWING REPRODUCIBILITY.
Low Speed: Air-Water High Speed: Oil-Water
Core K(md) Test 1 Test 2 Test 1 Test 2
CPC 3100 9.0 9.1
11.2 11.3 ration losses, and other experimental difficulties may account
COS 2500
10.5 10.6 for the generally lower results obtained in this system.
COT 2100
CPA 1700 13.1 13.8 In order to evaluate further the reliability of the centrifuge
COF 1350 16.8 16.8 method lor establishing connate water in core plugs approxi-
AVX 885 14.4 14.1 13.9 14.6 mately 100 cores. on which capillary pressure studies using
COP 460 22.3 22.5 the disc method had been made, were selected. An interstitial*
EU 458 27.3 26.4 water determination with the normal speed air-water system
1188 453 8.5 8.4 was made on each of these cores. The results are shown in
BVR 67 26.5 27.4 Fig. 7.
APT 16 35.4 35.4 The data in Fig. 7 demonstrate a good correlation between
AHU 2.7 33.7 33.7 the centrifugal method and the capillary pressure system. The
AJN 2.1 36.8 36.2

top of a 1 in. core for typical systems is shown in Table IV. mental *Interstiti;~J ~ water denotes .. water ~aturation for some stated experi-
condItIon_ At a suffiCIently hIgh pressure difference between the
The maximum b,P is approximately 750 psi for the high speed phases, the interstitial water saturation will become equal to the connate
(irreducible) water saturation.
air-water systems.
Results of connate water determinations on a number of Ta b Ie III - Change in Connate Water Value Showing
cores using the six different systems are shown in Table V. Change in Core
These data show that for many of the more permeable cores Connate Water Value for Oil-Water
the normal speed air-water system or the air-water system with System: Using Higb Speed Head
end butt is as effective in de saturating the core as the high Core K (md) Orig. Value Later Value Difference
speed water-oil system (cores COY, COX, AVX, and 1189). COF 1350 14.5% 16.8% 2.3
The tighter cores (BVR, ATF, and AUE) show the real need EU 458 31.1 27.3 3.8
for the extremely high pressure differences between the phases BVR 67 25.0 26.5 1.5
produced in the high speed head. At this stage it is not clear APT 16 30.8 35.4 4.6
whether the results obtained using the high speed head for AHU 2.7 29.1 33.7 4.6
the air-water system are reliable. Cavitation,' possible evapo- _A_1N _______ 2_.1_____3_2_.2_ _ _ _..:3..:6.:..8=---_ _ _. .:4.:. :-6:.

Vol. 192, 1951 PETROLEUM TRANSACTIONS, AIME 131


T.P. 3052 USE OF-CENTRIFUGE FOR DETERMINING CONNATE WATER, RESIDUAL OIL, AND
CAPILLARY PRESSURE CURVES OF SMAll CORE SAMPLES
32 most all of the values are seen to lie well below the regression
line, indicating that the pressures used in the capillary pres-
CORE No. AVZ
K o "I030md. sure work were clearly inadequate.
+=24.9%
A-CENTRIFUGE DATA 1st RUN Capillary Pressure Curves: Air-Water System
28
.-CENTRIFUGE DATA 2 nd RUN Capillary pressure curves have been obtained on more than
X=DISK METHOD 30 cores by use of the centrifugal method described under
"Procedure." At least two determinations have been made on
-more than 16 different cores. Very good agreement between
24
check runs was generally observed. Typical results on three
cores are shown in Figs. 9 to n. Points on the capillary pres-
sure curve obtained in another laboratory by use of the disc
method are represented by x's in these plots to show the gen-
":20 eral agreement in value between the two methods_ The repro-
on
a. ducibility observed may be summarized quantitatively by
I&J
It: , stating that for all of the duplicate runs made the average
spread in saturation at 24 psi pressure difference between the
~16 phases was 2.7 per cent, and the average pressure spread at
(/)
I&J
It:
Q.
> Table IV - Pressure Difference Between Phases at Top
of Core I-in. Long
~12 System /';.P Max.
C( High Speed Centrifuge: Air-Water 750 psi
..J (18,000 rpm) Oil-Water 210 psi
..J
Ci: 4 Normal Speed Centrifuge (3,800 rpm) :
Air-Water with %-in. end butt 125 psi
~8 ,
Air-Water 100 psi
Oil-Water with %-in. end butt 35 psi
Oil-Water 28 psi
Constants:
4
~~
,.... .... Average Radius of Rotation for I-in Core-
Normal Speed 16.5 cm
Average Radius of Rotation for I-in Core-
High Speed 4.25 cm
"
0.2 0.4 0.6 0.8 1.0 Effective height of I-in. core when supported at slope
BRINE SATURATION
in high speed head =3.26 cm
Density of 50,000 ppm Chloride Brine = 1.053
fiG. 10 - CAPILLARY PRESSURE CURVE SHOWING REPRODUCIBIlITY. Density of Oil =0.758
Equation u~ed: /';.P =
1.578 x 10~' (P, - p,) n'rh;
cores in this study were divided into two groups. The cores /';.P =
psi; p = glcc; n = rpm;
of group I (shown in Table VI) had capillary pressure curves T =cm; h =cm
which were vectical in the higher pressure region (10 to 16
psi between phases for oil-water and up to 50 psi for air- Table V - Water Saturation Values Obtained to
water) indicating that the saturations at the completion of Demonstrate Relative Effectiveness of Various
the capillary pressure runs were at the connate water value. Centrifuge Methods
The connate water values on these cores obta~r.ed using the Normal Speed High Speed
air-water system in the centrifuge are in fairly close agreement Oil-Water System Air-Water System
No No
with the capillary pressure values. In most cases the centri- End End End End Oil- Air-
fugal method gave a slightly higher water saturation. In cases Core K(md) Butt Butt Butt Butt Water Water
such as this, true connate water was apparently attained in AVT 2710 7.7 6.7 5.7
the capillary pressure method, and the centrifuge value i5 AVL 2210 10.7 7.7 6.6
slightly in error because of the end effect previously dis- COY 1800 12.1 12.3
cussed. If greater precision is desired, this end effect can be COX 1600 14.5 14.8
eliminated by the use of butts. COF 1350 20.0 14.5
In Table VII are listed the second group of cores which had AVX 885 14.4 13.9
connate water value greater than 30 per cent or which did not COG 570 22.3 20.6 17.8 18.0
have vertical capillary pressure curves at the highest displac- 1189 470 18.1 9.8 10.8
ing pressures (16 psi) used. Lower values of interstitial water COP 460 22.3 20.5 19.5 18.3
saturation were observed on the majority of these cores by EU 458 36.2 31.1 21.5
centrifuging in the low speed air-water system as compared to 1188 453 8.9 8.5 5.4
the capillary pressure method_ Inadequate pressure, poor AEP 316 25.3 20.0 18.2
capillary contact, or failure to wait the extremely long time AEQ 203 24.7 22.8 19.9
necessary to establish true equilibrium in the capillary pres- AWB 138 26.8 22.0
sure system could explain these results_ A number of these BVO 84 30.7 27.2 26.4 25.2
cores were run in the high speed centrifuge (oil-water sys- BVR 67 40.1 29.4 27.2 26.5
tem) in order to obtain a better value for connate water. These ATF 5.4 49.1 29.0 24.4
results are given in Table VII and are shown in Fig. 8. AI- AUE 4.3 54.5 33.0

132 PETROLEUM TRANSACTIONS, AIME Vol. 192, 1951


R. l. SlOBOD, ADELE CHAMBERS AND W. l. PREHN, JR. T.P. 3052

95 per cent saturation was only 0.4 psi. These results were 32
obtained in cores from five different fields with permeabilities
ranging from 3.5 to 1,030 md. From the excellent reproduci- CORE No. BVL
bility observed in this study, the conclusion has been drawn K o=225 md. +=24.3%
that the centrifuge method is sufficiently reliable to replace 28
the disc method which is much less reliable and which is at &- CENTRIFUGE DATA 1st RUN
best only of comparable precision. -CENTRIFUGE DATA 2 nd RUN
a-CENTRIFUGE DATA 3 rd RUN
Residual Oil: Water Drive and Oil Drive 24 X=DISK METHOD

A small amount of data has been obtained showing that


reproducible residual oil values can be obtained either by
driving the core with water or with air. Some of the values
f1
for water drive are shown in Table VIII. In some cores the
agreement is excellent (within several tenths of 1 per cent of
the pore space). In others the variation is greater than 1 per IIJ
cent of the pore space. Unfortunately, as a result of the mate-
a:
:::>
rials and methods used in this laboratory, the wetting charac- (/)1 6
(/)
teristics of cores apparently change with use, resulting in IIJ X
changes in the observed value for residual oil. This difficulty a:
Q..

Table VI - Comparison of Interstitial Water Values ~I 2 ~


Obtained by Centrifugal Method (Low Speed Water-

\-
C(
Air System) and by Capillary Pressure Method ..J
..J
Core K(md) Cap. Pres.* Centrifuge Q..
C(
CPC 3100 4.5 9.0 (,) 8 \:
AVT 2710 5.2 6.7 ~
COS 2500 10_6 11.2
CPD
AVN
A VS
2400
2318
2230
6.8
5.8
5.7
10.6
6.0
7_2 4 ~
AVL
COT
COY
2210
2100
1800
5.3
9.6
9.6
7.7
10.5
12.1
~ -... iIII&L

CPA 1700 10.3 13.1 0 ~


COX 1600 10.7 14.5 o 0.2 0.4 0.6 0.8 1.0
COR 1540 14.8 16.0 BRINE SATURATION
COL 1400 13.8 14.7 FIG. 11 - CAPILLARY PRESSURE CURVE SHOWING REPRODUCIBILITY.
COF 1350 13.0 20.0
COz 1300 11.0 13.3 is expected to be overcome by modifications in procedure and
COM 1140 14.0 16.1 materials used so that results reproducible to a fractioI). of
AVZ 1030 11.2 11.6 1 per cent of the pore space can be attained.
COR 975 17.0 18.9 As a result of considerable experience with the centrifuge
AVV 954 11.0 ILl in establishing connate water and residual oil in core samples
AVW 926 10.9 11.4 for use in subsequent experimental work, particularly in the
AVX 885 13.5 14.1 laboratory determination of relative permeability, the versa-
COl 680 20.6 24.7 tility, reliability, and convenience of this method have been
COO 680 18.0 19.1 amply demonstrated. Moreover, this tool can be used to facili-
A VY 679 13.2 15.2 tate relative permeability determinations by rapidly establish
COG 570 11.0 20.6 ing residual oil saturation after the point has been reached
COl 525 19.7 23.0 where the oil saturation changes slowly with time in the rela-
CON 500 19.1 19.8 tive permeability apparatus. After residual oil is established,
A WA 494 16.3 16.6 the relative permeability of air (or water) may be determined
1189 470 9.8 9.8 in the relative permeability equipment. The use of the centri-
COP 460 21.2 22.3 fuge as outlined above, in which cores are provided with de-
1188 453 9.0 8.9 sired saturants present, has proved to be extremely valuable,
AES 351 20.9 21.5 and in future applications this use may possibly exceed in
AEP 316 19.0 20.0 importance the determination of core properties merely for
COQ 315 25.1 28.9 their own sake.
APL 237 13.8 15.1 Other applications such as the determination of critical gas
APK 227 12.6 15.3 saturation and studies at simulated reservoir conditions pos-
AWC 204 26.4 23.0 sibly may be carried out in the centrifuge.
AEQ 203 20.9 22.8
AWB 138 26.0 26.8 CONCLUSIONS
APR 89 18.7 21.8
ATF 5.4 17.4 49.1 1. In the evaluation of the property of core plugs the cen-
'All Cores Apparently at Connate Water from Capillary Pressure Curve. trifuge can be used to establish connate water saturation,
Vol. 192, 1951 PETROLEUM TRANSACTIONS, AIME 133
T.P. 3052 USE OF CENTRIFUGE FOR DETERMINING CONNATE WATER, RESIDUAL OIL, AND
CAPILLARY PRESSURE CURVES OF SMALL CORE SAMPLES
residual oil by air or water drive, and can be used to obtain Table VIII - Reproducibility in Residual Oil D'eter.
capillary pressure curves. minations Using Water to Displace Oil from Cores
2. The use of the centrifuge for connate water, residual oil, Containing Connate Water
and capillary pressure studies has many advantages, particu- Residual Oil Values - % of Pore Volume
larly with respect to the disc method now in common use.
Core K(md) Run 1 Run 2 Run 3 Run 4 Avg.
These are:
a. Little devel.opment cost is involved as most of the parts COP 460 21.3 21.3 21.3
are commercially available. 1447 283 14.4 10.2 11.4 10.2 10.8
AWB 138 21.7 19.6 20.7
Table VII - Comparison of Interstitial Water Satura- API 16 34.3 34.3 34.3
tions Attained by Centrifugal Methods with Those 1443 7.5 29.2 31.8 30.6 28.8 30.1
Obtained by Capillary Pressure Methods 1437 4.8 24.0 24.0 26.4 23.6 24.6
Cores with vertical capillary pressure curves and with residual 1439 0.86 30.8 28.7 30.1 32.2 30.4
(water) values above 30%: b. The initial cost is low.
Low Speed High Speed
c. Apparatus is a simple, compact system requiring little
Core K(md) Cap. Pres. Water-Air Water-Oil
manipulation, which makes it nearly foolproof and re-
EU 458 32.1 36.2 31.1 sults in very little lost data.
COY 360 26.1 28.6 d. System reaches equilibrium rapidly, making results avail-
XY 345 37.8 36.1 able more quickly. The time loss usually experienced as
BVL 225 34.8 23.6 a natural result of equipment failure and experimental
COK 140 30.2 32.0 difficulties in long drawn out experiments is not present.
BVO 84 44.5 27.2 25.2 More accurate data are also obtained because equilibrium
BVN 84 43.3 31.9 is really attained instead of just approached.
BVR 67 40.0 29.4 25.0 e. Results are more accurate because sources of error such
API 46 32.8 31.6 as poor capillary contact and failure to attain equilib-
APQ 38 37.8 34.5 rium are absent and because higher pressure differences
BVM 27 51.0 40.0 35.4 between phases necessary for many cores are available.
APU 22 54.5 52.3 34.1 f. Results are reproducible with greater precision than in
APT 16 35.3 43.5 30.8 other known methods.
AHF 3.1 40.3 48.0 27.3 g. The theoretical basis of the work appears to be sound
AHU 2.7 71.1 52.0 29.1 since the principle of drainage which is involved in the
AHG 2.2 61.5 50.5 25.6 centrifuge is closely related to that in the reservoir.
YZ 0.6 50.0 53.5 41.3 3. The centrifuge is particularly applicable to establishing
Cores of which the capillary pressure curve was not vertical: connate water in cores either for determining that value or for
CBW 12.4 92.6 82.9 experimental work in which cores containing connate water
ZH 4.4 73.6 58.0 are needed.
BAG 3.8 78.5 56.4
CGI 3.6 81.7 79.8
AHA 3.5 88.3 49.0 29.8 ACKNOWLEDGMENT
AAC 2.7 65.8 67.3 The authors wish to acknowledge with gratitude the cooper.
CGP 2.7 72.2 81.2 67.5 ation of Dean W. Lee Hart and the personnel of Southwestern
ANG 2.7 48.6 46.1 27.4 Medical College of the University of Texas in making avail-
CGV 2.4 78.4 48.0 33.6 able their equipment for preliminary investigation.
CHH 2.3 97.5 87.4
ANB 2.2 50.8 48.6 29.6
AOR 2.1 80.0 79.6 57.1 REFERENCES
AXV 2.1 72.8 57.0 29.1 1. McCullough, J. J., Albaugh, F. W., and Jones, P. H.: APi
CGN 2.0 76.5 83.2 67.1 Drill. and Prod. Prac., (1944), 180-188.
CGK 1.9 98.0 83.6 2. Hassler, G. L., and Brunner, E.: Trans. AIME, (1945),
ATX 1.8 82.1 83.3 160, 114-123.
CHD 1.4 72.4 67.8 3. Amyx, J. W., and Yuster, S. T.: Producers Monthly, (Dec.
AHB 1.3 57.5 66.5 40.0 1946),11, No.2, 10-13.
A YB 1.0 75.4 80.5 47.0 4. Bruce, W. A., and Welge, H. J.: Oil and Gas lour., (July,
BAF 1.0 78.5 73.0 1947), 156, No. 21, 223-238.
BL W 1.0 69.0 69.5 5. Calhoun, J. c., Jr., Lewis, Maurice, Jr., and Newman,
CGH 0.9 89.9 88.3 R. C.: Trans. AIME, (1949), 186, 189196.
AZU 0.8 79.6 66.6 6. Hassler, G. L., Brunner, E., and Deahl, T. J.: Trans.
CGJ 0.7 73.2 88.9 AIME, (1944), 155-174.
AKO 0.6 97.0 77.8 7. Leverett, M. C.: Trans. AIME, (1941), 142,152-169.
AZW 0.5 88.1 67.5 8. Rose, Walter, and Bruce, W. A.: Trans. AIME, (1949),
AZX 0.5 71.4 64.7 186, 127-142.
CGG 0.4 91.1 83.5 9. Stahl, C. D., and Nielsen, R. F.: Producers Monthly, (Jan.,
CGL 0.3 95.5 94.5 1950), 14, No.3, 19-22.
CHG 0.3 91.0 93.4 76.3 10. Thornton, O. F., and Marshall, D. L.: Trans. AIME,
AZI 0.2 75.7 77.3 41.0 (1947),170,69-80.
AZM 0.2 78.9 70.4 11. Yuster, S. T., and Stahl, C. D.: Producers Monthly, (Dec.,
AZN 0.2 76.5 62.1 1948), 13, No.2, 24-29. ***
134 PETROLEUM TRANSACTIONS, AIME Vol. 192, 1951

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