4-1

Petroleum Fluid Properties

CHAPTER 4.
LABORATORY PVT MEASUREMENTS
4-1

INTRODUCTION

In the previous chapters we have discussed the compositions, phase behaviour and
physical properties of petroleum fluids as well as setting about defining the various
parameters of interest to Engineers. In this chapter the experiments through which these
parameters are determined in the laboratory will be described.
It is assumed that a valid fluid sample is available for the tests, either through i) obtaining
a single phase sample in the field, or ii) through recombination of separator gas and liquid
in the laboratory. Validation of field samples and recombination are integral parts of
Reporting PVT data and are treated in the chapter dealing with PVT Reports, together with
Quality Checks applied to the laboratory measurements.
The majority of PVT measurements are derived from a relatively straightforward suite of
experiments depending upon fluid type. Several of the tests are applied to all types of
fluid, employing the same principles in different equipment. However, a typical
arrangement of apparatus for volumetric work is shown schematically in Figure 1. The
cell shown in the figure is of the 'long-windowed' type suitable for relative phase volume
measurements (e.g. in volatile oil studies), but it is common to use other specialised
designs such as 'inclined-window' cells and 'blind' cells, (i.e. no windows) for black oils and
other studies. Nevertheless the principles of operation remain the same for all
configurations and specific details and/or limitations will be highlighted as the individual
measurements are discussed.

4-2

CONSTANT MASS EXPANSION (CME) EXPERIMENT

The Constant Mass or 'Constant Composition Expansion' (CCE) experiment is carried out in
virtually all PVT studies irrespective of fluid type. It is used to measure the total fluid
volume and compressibility over a wide range of pressures extending beyond initial
reservoir pressure to pressures below the anticipated separator pressures. For black oils
and many volatile oils it is also used to determine the saturation pressure at reservoir
conditions. A schematic representation of a CME experiment is shown in Figure 2.
For both oils and gases the (recombined) fluid sample is transferred into the PVT cell and
brought to reservoir temperature and a pressure above the reported initial reservoir
pressure. The total volume of the fluid is then measured upon pressure reduction. The
various types of Relative Volume (or PV) curves obtained from this experiment are shown
in Figure 3.
For a black oil or volatile oil, the transition from single to a two-phase
system is apparent in the plot. For gas condensates the separation of the liquid phase is
not readily apparent from the experimental volumetric data and it must be determined
visually (see below).

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Petroleum Fluid Properties

CELL

MERCURY
PUMP
THERMOSTAT

Figure 1: Schematic Representation of PVT Apparatus for Volumetric Measurement

The number of pressure reduction steps and the total pressure range covered is generally
determined by consultation between the Engineer who commissions the study and the
laboratory personnel. The CME experiment may also be carried out at other temperatures
in addition to the reservoir temperature to help model the producing conditions for
subsequent process calculations.
For oil samples, the differential volume expansion below the bubble point pressure is
significantly higher than that above the bubble point pressure. This allows the bubble
point to be determined from a graphical plot of the total fluid volume as a function of
pressure. The point at which the slope of this point changes is the bubble point of the fluid
sample. The change in differential volume expansion is due to the presence of the vapour
phase, which has a much greater compressibility than the corresponding liquid phase.
For oil samples - where the relative volumes of oil and gas are not usually determined the CME experiment is often carried out in a "blind" cell to improve the volumetric
accuracy of the experiment.
As mentioned above, for gas condensate fluids the plot of total fluid volume as a function
of pressure does not have a "sharp" change of slope at the saturation pressure unless the
system has appreciable liquid dropout when crossing the dewpoint pressure. This
behaviour can be observed in simple (synthetic) mixtures with 2 to 5 components, but is
rarely discernible in real systems.

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Petroleum Fluid Properties

Gas

Reservoir
Fluid

Hg

P > Psat

Reservoir
Fluid

Gas

Oil

Gas

Gas

Oil
Oil

Hg

Hg

P1 < Psa t

P = Psat

Hg

P2 < P1

Oil

Hg

Hg

P3 < P2

P4 < P3

Figure 2: Schematic Representation of Constant Mass Expansion Experiment

Black Oil

Pressure

Pressure

Volatile Oil

Psat (= Pb)

P sat (= Pb)

Volume

Volume

Psat (= P d)

Dry Gas

Pressure

Pressure

Gas Condensate

Volume

Volume

Figure 3: Variation in p,V Behaviour for Various Fluids

It is recommended for the measurement of dewpoint pressures that the system be studied
in either a 'long-windowed' (Figure 1) or a 'Sloane-type' Gas Condensate cell where visual
observation of the retrograde liquid volume may be made. The dewpoint is then
determined by plotting the volume of retrograde liquid Vliq as a function of pressure.
Extrapolation as Vliq -> 0 yields the dewpoint pressure for the system.
In the single phase region the relative volume curves are also used to calculate: i) the
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Petroleum Fluid Properties

variation of density with pressure, ii) the isothermal compressibility and iii) the thermal
expansivity if the volume of sample is recorded at more than one temperature.

4-3

DEPLETION EXPERIMENTS
4-3-1

DIFFERENTIAL LIBERATION (DLB)

The differential liberation experiment is the classical depletion experiment for reservoir
oils. The experiment is carried out at reservoir temperature to simulate the volumetric and
compositional changes in the reservoir during production (depletion).
Initially an 'inclined-window' PVT cell is charged with the reservoir oil sample and the cell
taken to reservoir temperature. A series of stepwise pressure reductions is carried out
with the system left after each pressure reduction to separate and for equilibrium to be
established.
o

V(Gas, P, 60 F)
1

Reser voir
Fluid
Hg

P > Psat

Gas
Oil

Oil

Oil
Hg

P = Psa t

Hg

P1 < Psat

Hg

Gas
Oil

V (Gas, P, 60 F)
2

Oil

Hg

Repeat
n
Times

Oil

Oil

Hg

Hg

Hg

P1

P2

P2

(P, T r es)

(P, 60 F)

Figure 4: Schematic Representation of Differential Separation Experiment

Once equilibrium has been reached, the liberated gas phase is removed from the cell and
analysed (this may be via a simple separator system) and the volume of the liquid phase
and gas phase are determined. The pressure of the liquid phase remaining in the cell is
then reduced again and the procedure repeated until the final pressure (usually
atmospheric) is reached. The process is shown schematically in Figure 4.
Use of an inclined window allows the outlet of the top valve in the PVT cell to be clearly
seen. This allows the operator to control visually the displacement of the gas phase right
to the oil meniscus. The oil remaining in the cell at Tres, 0 psig is termed 'Residual Oil'.
When the Residual Oil has cooled to ambient temperature, its properties (volume at 60 oF,
density, composition) are also measured. Note that the volume of Residual Oil necessarily
shrinks due to thermal contraction while cooling. This 'shrinkage' is measured by
recording the volume of oil at both Tres and 60 oF and is an important part of completing
the material balance checks described in the following Chapter. The gas and oil
volumetrics for a DLB experiment are shown in Figure 5.

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Petroleum Fluid Properties

Vob @
(Tres, P b)

Sample
Volume
Vg3

Vo3

Vg1

Vg2

Vo2

Vo1

Vro (Tres)
o

Vro(60 F)
P3

P2

P1

Psat

Pressure
Figure 5: Gas and Oil Volumetrics During Differential Liberation
The quantities determined from DLB experiments are the relative oil and gas volumes, the
oil and gas density at stage pressures, the Solution GOR (Rs), and the gas deviation factor
(Z) as a function of pressure, and the gas expansion factor.
In modelling reservoir depletion, the DLB experiment makes the assumption that all gas
liberated in the reservoir is produced and leaves behind the remaining oil to liberate fresh
gas. This is not always a valid assumption, particularly for volatile oils, and a Constant
Volume Depletion (CVD) experiment is usually recommended.

4-3-2

CONSTANT VOLUME DEPLETION (CVD) EXPERIMENT

The constant volume depletion (CVD) experiment is generally carried out for volatile oil
and gas condensate reservoir fluids. Again, this experiment is a laboratory model of
reservoir fluid depletion during production. It differs from the DLB experiment in that not
all the equilibrium gas is removed at each pressure stage. In this respect it models a
reservoir formation of Constant Volume which is producing rich gas, but retaining the
equilibrium liquid phase. This experiment is carried out for volatile oils because of the
relatively large volumes of gas liberated under reservoir conditions when the reservoir
pressure falls below the bubble point pressure and the high shrinkage of the liquid phase
with pressure reduction. The CVD experiment is shown in Figure 6.

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Petroleum Fluid Properties

Gas

Gas

Cond.

Gas

C ond.

} Wellstream

Cond.

Res.
Fl uid

Res.
Fluid

Res.
Fl uid

Hg

Hg

Hg

Hg

Hg

Hg

Hg

Hg

P > Pdew

P = Pres

P 1= Pdew

P 2< Pdew

P2

P3

P3

V = V

dew

Repeat
n
Times

V = V

dew

V = V

dew

Condensate

Figure 6: Schematic Representation of a Constant Volume Depletion

Again, the experiment starts with a single-phase reservoir fluid sample of known volume
at reservoir temperature and pressure. As before, the pressure is reduced stepwise
resulting in an expanded volume for the fluid at each stage. After equilibration, sample is
displaced from the top of the cell to return the fluid volume to the original value. At some
point during pressure reduction, the fluid passes through the saturation pressure - either
a dewpoint (Pd - gas condensate) or a bubble point (Pb - volatile oil). It is, therefore, part of
the upper (gas) phase which is displaced from the cell to re-establish constant volume.
The fluid removed at each stage is flashed to near standard conditions and analysed to
determine the composition and C7+ molecular weight. Generally, between 5 and 10
pressure reduction steps are completed down to atmospheric. After the final stage, the
liquid remaining in the cell is analysed.
The data that is determined from CVD experiments are the volume of gas and liquid at
pressure and temperature, the cumulative amount of produced (wet) gas, the gas Z-factor
and the composition of the produced wellstream. All of the reported volumetric data is
reported relative to the volume of fluid at the dew point, for gas condensate or bubble
point, for volatile oils. The determination of the correct saturation pressure (and sample
volume) is of paramount importance with small changes in pressure leading to very large
shifts in relative volumes. This can be misleading if the high compressibility of such fluids
is not taken into account in reviewing the volumetrics.
Finally, it should be noted that the compositional changes determined during a laboratory
CVD experiment may be quite different to those for a reservoir under water drive.

4-4

SEPARATOR TESTS

Separator tests (sometimes termed multistage separations) on reservoir fluids are carried
out to simulate potential Production Separator Stages and provide volumetrics and other
information on the Stock Tank Oil and liberated gas streams. These days, compositional
information obtained from these tests is often used to tune computer models (essentially
Equations-of-State) to allow determination of optimum separator conditions for production
of the reservoir.
Separator tests are carried out along similar lines to the depletion tests described above,
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Petroleum Fluid Properties

except that the temperature is also reduced at each stage and there are only a few
pressure steps (often just one between Pres and Patm). The procedure is set out below.
A known amount of single phase reservoir fluid is charged to a pressure vessel and the
pressure and temperature are adjusted to the conditions of the first stage separator. The
system is then brought to equilibrium and the liberated gas removed from the cell. Again,
the amount of gas is measured (at both separator and standard conditions) as well as its
composition.
The pressure and temperature of the liquid remaining in the pressure
vessel is then changed to those of the second stage separator and the above process
repeated. Once the cell is reduced to stock tank conditions, the amount, gravity and
composition of the remaining liquid (stock tank liquid) can be determined. Any number of
stages can be simulated in this manner in the laboratory. Often several separator tests
are requested by engineers to simulate several potential production situations. The
methodology is shown in schematically in Figure 7.
Separator tests are rarely performed on gas condensate systems because there is often the
practical difficulty of obtaining enough reservoir fluid to produce enough sufficient liquids
for the experiments.
o

V(Gas,
P, 60 F)
1

Gas

Oil

Oil
Hg
Hg

V(Gas,
P, 60 F)
2

Gas
Oil

Oil

Oil

Hg

Hg

Hg
o

(P, 60 F)

(P,
T )
1 1

(P,2 T 2)

Figure 7: Schematic of a Separator Test Series

4-5

VISCOSITY MEASUREMENTS

In the petroleum industry there are various techniques available to physically determine
the reservoir fluid viscosity. CoreLab currently uses two methods 1) Rolling Ball
Viscometer (RBV) and 2) Falling Sinker Viscometer (FSV). The RBV is widely used for oils
and liquid phases but is inappropriate and too inaccurate for gases. The FSV has been
developed by CoreLab to replace the RB technique and can be used for all types of
reservoir fluids from dry gas systems to heavy bio-degraded oils. The techniques of each
method are briefly discussed below.

4-5-1

THE ROLLING BALL VISCOMETER (RBV)

The RBV has become something of an industry standard method, although it has a
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Petroleum Fluid Properties

4-8

number of severe limitations in practice. The technique is only suitable for use with
liquids and it suffers from a lack of fully developed theory. In this context, it is necessary
to calibrate the instrument with known viscosity standards similar to the fluids to be
measured. Calibration aside, however, the principle of operation is straightforward:
The RBV consists of a highly polished stainless steel barrel (typically 1/4" (6 mm)
diameter) which can be closed at the top by means of a plunger. A steel ball rolls within
the barrel, its diameter necessarily being slightly smaller than the bore, but dependant
upon the viscosity range to be measured. During measurements, the barrel must be filled
completely with the fluid to be studied. The barrel is inclined at a known angle and the
ball rolls along it under gravity for a measured distance. The roll time is determined by a
suitable timing mechanism. When operating correctly, the roll time interval is a measure
of the viscosity. The instrument is shown schematically in Figure 8.
If the clearance between the bore of the barrel and the ball diameter is too small, then the
flow of fluid past the ball will be turbulent. Under these conditions the RBV does not
measure viscosity correctly since the theory (such as it is) assumes laminar flow. To
control the rolling time, measurements can be made at different angles or the stainless
steel ball and/or the barrel may be replaced with a different diameter. The working
equation is as follows:
oil = (( t x (? ball - ? oil) - a )) x b
Where:

t
= rolling time in seconds,
(? ball - ? oil)
= difference in density between ball and oil,
a&b
= constants of the system which are determined from
calibration with oils of known viscosity.

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Petroleum Fluid Properties

Detectors

Figure 8: Principle of rolling ball Viscometer.

Oil viscosities are usually measured at reservoir temperature over a range of pressures
both above and below the saturation pressure extending down to near atmospheric
pressure.
Measurements below saturation pressure are made under differential
conditions, ie: matched as closely as possible to the stage pressures used for the
differential liberation. RBVs are constructed in such a way as to allow a pseudodifferential liberation of gas to be conducted within them, leaving the oil to fill the
measuring chamber. In this way, the viscosity of the oil in the reservoir can be measured
as gas is depleted from it. The change in viscosity with release of gas is usually very large.
Unfortunately, the RBV is susceptible to a number of errors in addition to the limitations
outlined above. In particular, the ball can bounce and/or slide during its roll time
resulting in scattered and poorly reproducible results. Great care is needed by the
laboratory in order to produce self-consistent, smooth data.

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Petroleum Fluid Properties

4-5-2

FALLING SINKER VISCOMETER

The theory of the FSV has a similar principle to the RBV in that it measures the time for a
solid body to move through a fluid, but the FSV is based on sound physical principles.
Therefore the equations that govern the motion of the body are derived from the
fundamental laws of fluid dynamics.
The principle of the FSV is that a self-centring bullet shaped sinker falls under gravity
inside a precision bore tube. The sinker initially free falls, eventually accelerating to a
terminal velocity and the fall time between two detection coils at this terminal velocity is
determined. An inductive core in the sinker induces the timing signals. The instrument is
shown schematically in Figure 9 and Figure 10. The equation of motion at terminal
velocity yields the viscosity as follows :oil = t x (sinker - fluid) / A x sinker
Where:t

= fall time in seconds,

(sinker - oil) = difference in density between sinker and fluid,
A = constant of the system determined from calibration.

In theory the constant A can be determined from first principles by direct measurement of
the tube and sinker dimensions. Such a calculation would then only require the fall time
and the buoyancy correction for the sinker. However in practice it is found that accurate
measurement of the dimensions is very difficult and an error of +/- 1/1000 mm in
measuring the radius of the tube or sinker will produce an error in A of over 5% .
Therefore the FSV is also calibrated using known viscosity standards to determine
constant A. This value is then checked against the theoretical value for consistency and is
normally found to be within 2-3 % . Unlike the RBV where the barrels interchange for
various viscosity ranges, here the sinkers, of varying diameters are interchanged. It
should be noted that as with the RBV, the viscosity measurements are preferably carried
out where calibration data exists for that range. However, as long as measurements are of
the same order of magnitude or higher than the calibration data the viscosity data should
be accurate.

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Petroleum Fluid Properties

Mounting
Frame
End Plug

Rotating
Cradle

Shr ink age

Chamber
Homogeniser
Sample
Valve

Isolation
Valve

Pressure
Vessel

Viscometer
Assembly
Electrical
Leadthrough

End Plug
Cleaning
Plug

Sinker Plug

Figure 9 : Schematic of Falling Sinker Viscometer

In freefall, at terminal velocity,

Equations of Motion yield:

PRECISION BORE
TITANIUM TUBE
INDUCTIVE CORE

TITANIUM SINKER

DETECTOR COILS

RESERVOIR FLUID

Figure 10: Principles of Falling Sinker Viscometer

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Petroleum Fluid Properties

4-5-3

CAPILLARY TUBE VISCOMETER

The Capillary Tube Viscometer is employed in many laboratories to determine the

viscosities of effluent fluids from core floods and slim tube studies as well as through
direct application in PVT experiments by connection to a cell (Figure 11). Measurement of
the viscosity is determined by measuring the pressure drop ? P across a capillary at
constant fluid flowrate by applying Poiseuille's equation:

32. .v.l
d2

P =

where l and d are length and internal diameters of the capillary respectively and v is the
average fluid velocity. Fluid velocity is normally derived from a volumetric flowrate on a
high pressure pump in which case the equation becomes:

128.Q.l.
.d 4

P =

where Q is the volumetric flowrate. It is immediately apparent that the diameter of the
capillary is critical to the measurement and high pressure capillary viscometers are
usually calibrated to avoid severe measurement errors in d. Nevertheless, long capillaries
rarely if ever have a uniform internal diameter and the differential pressure ? P is easily
dominated by 'end effects' due to burring in cutting the tubing. Capillary viscometry is a
more difficult laboratory experiment than it at first appears and results from it should be
reviewed carefully where important calculations (eg: mobility ratio) are involved.

DPT
PRESSU RE
GAUGE

FS

BPR
CAP.
COIL

CELL

CONSTANT
FLOWRATE
PUMP

THERMOSTAT
Figure 11: Operation of a Capillary Tube Viscometer

4-6

SPECIAL MEASUREMENT REQUIREMENTS

4-6-1

PVT CELL DESIGN

Gas condensate reservoir fluids generally require special attention. For these fluids we are
trying to measure small liquid phase volumes in equilibrium with a very large volume of
vapour phase. However, these small volumes of liquid are important because they may
impact substantially on the economics of a reservoir development.
A schematic of a PVT cell optimised for gas condensate fluids is shown in Figure 12
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Petroleum Fluid Properties

Figure 13. The hour glass shape maximises the height of condensate liquid in the
"capillary" section of the cell. This cell design is sometimes referred to as a 'Sloane' cell.
These cells are typically vary in internal volume from 1 to 4 litres, which will provide a
good surface area to volume ratio and thus reduce any surface hold-up effect, as will
good design.

ACB Cell

C1
C2
C3
G as

Mercury

C4

V1

Video
Camera
P3

Condensate

P4

Light
Source

P0

B
P2

Computer-controlled
Mercury Pumps

P6

C5

Stirring
Motor

SAMPLE

MERCURY

P7

P8

Figure 12: High pressure Gas Condensate Cell

4-6-2

EQUILIBRATION TIMES

In 1988 Eyton presented a paper talking about the practical limitations of obtaining PVT
data for Gas Condensate systems. He reported that the amount of liquid seen in the cell
depends upon the times the cell is left to stabilise, which was assumed to be due to
drainage from liquid hold-up on the internal surfaces. He also stated that the laboratory
considered that most of the liquid had drained in the first 2.5 hours. In the paper Eyton
presented a plot of the liquid saturation curve for a CME (CCE) experiment with the liquid
volume as a function of time at each pressure step included.
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Petroleum Fluid Properties

However, other workers have found that by leaving the cell overnight after waiting over two
hours for cell stabilisation that the volume of liquid in the morning has increased
substantially. Many research workers in this area believe that the time required to reach
equilibrium at each pressure step may be of the order of 24 hours or more. However, there
are no literature reports of liquid saturation curves as a function of time. At the present
tme, this question of liquid losses within cells has not been resolved satisfactorily.

Hg Inlet Port
High Pressure
Seal

End Closure
Assembly

Piston

Sliding Seal

Upper Chamber
Sampling Por t
and Valve
Viewing Windows
Lower Chamber

Stirrer Assembly

Suppor t Stand

Hg Inlet Port
Figure 13 : Gas Condensate (Sloane) Cell for Operation to 392 oF (200 oC) and
17,500 psi (1200 bar)

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