Wet PVT Lab PETE 310

Lab # 6

Determination of Viscosity for oil samples

Learning Objectives
Gain a basic knowledge of the techniques used to measure viscosity
Learn to use a rotational and a glass capillary viscometer.
Understand the basics of rheological modeling.
General Skills
Use Excel spread sheets and graphs.
Work with different systems of units and convert one set to another.
Background Material
Rheology is the study of the change in form and flow of matter in terms of elasticity,
viscosity and plasticity. A clear understanding of the rheological properties of fluids is
vital in many fields of science and engineering. The purpose of this lab is to introduce
you to the different techniques and approaches to measure viscosity experimentally.
Viscosity is the measure of the internal friction of fluid. This internal friction is caused
when a layer of fluid moves in relation to another layer. The greater the friction, the
greater the amount of force required to cause this movement. This movement is known as
shear.

v
V1
V2

A
A

Figure 1. Deformation of a liquid under the action of a tangential force.

To define viscosity more precisely, lets take a look at figure 1. Two parallel planes of
fluid of equal area A are separated by a distance dx and are moving at different speeds

V1, V2. The force required to maintain the difference in speed is proportional to the
difference in speed through the liquid.
F
dv
= ,
A
dx

(1)

where:
is known as the viscosity, usually in units of centipoises or Pa.s.
dv
is the shear rate. Describes the shearing the fluid experiences when the layers move
dx
with respect of each other. Units in reciprocal second, sec-1.
F
is the force per unit area required for the shearing. This is known as the shear stress
A
and it has units of pressure.

Therefore, we can define viscosity as =

Shear Stress
Shear Rate

Newtonian fluids

Shear rate

A Newtonian fluid is characterized by having a constant viscosity at a given temperature.

This is normally the case for water and most oils. A plot of shear rate versus shear stress
would show a constant slope, (figure 2). This is the simplest and easiest fluids to measure
in the lab.

ni
to
ew

an

Shear Stress

Figure 2. Shear rate versus Shear stress for a newtonian fluid

Non Newtonian fluids

A non-newtonian fluid is characterized by not having an unique value for viscosity. That
is, the relationship stress rate/shear rate is not constant. The viscosity of these fluids will
depend on the shear rate applied.

There are several types of non-newtonian fluid behavior that we can observe in the lab.
The most common are shown in figure 3.
Pseudo plastic fluids : these are fluids like paints and emulsions, there is a decrease in
viscosity as the shear rate increases. Also known as shear thinning fluids.
Dilatant fluids: these are fluids that increase their viscosity as the shear rate increases.
Examples are cement slurries, candy mixtures, corn startch in water. Also known as shear
thickening fluids.

ing

r
ea
Sh

th

ing
inn

stic

ea
Sh

n
ke
h ic
rT

Pla

Shear rate

Plastic fluids: These fluids will behave like solids under static conditions. They will start
to flow only when certain amount of pressure is applied. Examples are tomato catsup and
silly putty.

Shear Stress

Figure 3. Shear rate versus Shear Stress for different types of fluids

Instruments to measure rheological properties

Most instruments designed to measure viscosity can be classified in two general
categories: tube type and rotational type. Figure 4 shows the different types of
instruments available. The selection of a particular instrument must be based on the type
of analysis required and the characteristics of the fluid to be tested. For example,
rotational methods are generally more appropriate for non-newtonian fluids, while glass
capillary viscometers are only suitable for Newtonian fluids.

Figure 4. Classification of rheological instruments.

In this lab, we will use three different instruments to measure viscosity: Cannon Fenske
viscometers, the Ruska Rolling Ball viscometer and the rotational Cone and Plate
viscometer.
Cannon-Fenske Viscometer
The Cannon Fenske tube viscometers are very useful and easy to use to collect
rheological data. This device uses gravity to create flow and its use is limited to
Newtonian fluids with viscosities in the range 0.4 to 20000 cP.
The viscosity obtained from this instrument is typically reported as kinematic viscosity.
The kinematic viscosity can be defined as the viscosity of the fluid divided by its
density .

= ,

(2)

where is the kinematic viscosity, in mm2/s, also known as cSt (centistokes).

Procedure
1- Clean the viscometer using a suitable solvent and dry with clean air
2- To charge the sample into the viscometer, invert the instrument and apply suction
to tube G immersing tube A in the liquid sample. Draw liquid to mark E. Wipe
clean arm A, and turn the instrument to its normal vertical position.
3- Place the viscometer into the holder, and insert it inside the constant temperature
bath. Align the viscometer vertically in the bath.
4- Allow approximately 10 minutes for the sample to come to the bath temperature
at 40 C and 15 minutes at 100 C.

5- Apply suction to tube A or pressure to tube G and draw the liquid above mark C.
6- To measure the efflux time, allow the liquid sample to flow freely down past
mark C, measuring the time for the meniscus to pass from mark C to mark E.
7- Repeat at least once your measurement.
8- Calculate the kinematic viscosity in centistokes of the sample by multiplying the
efflux time in seconds by the viscometer constant.

=Ct
Where:

: kinematic viscosity, mm2/s.

C: viscometer constant, mm2/s2.
t: flow time, s

Figure 5. Cannon-Fenske viscometer

Cone and Plate Viscometer

This method of determining Viscosity uses a cup to contain the sample as the plate and a
spindle with specific dimensions as the cone to determine viscosity. This test has some
very specific advantages over other tests. First it uses a very small sample, usually from
0.5-2 ml of fluid. Second with the correct installation and equipment samples can be
tested at numerous shear rates and temperatures.
The basics of the test are that a spindle which is a flat round plate is attached to the
devices called a rheometer. This round plate has specific properties such as a crosssectional area. This plate is then rotated while in the sample to be measured. The space
between the bottom plate and the bottom of the device is strictly controlled. The plate is
then rotated at a constant speed (rpm). While rotating a strain gauge attached to the shaft

the spindle is mounted on measures the drag produced between the plate and the sample
being tested. This drag force along with the dimensions of the plate are used to
determine the shear stress.
These are measured in dynes/cm2. The physical
characteristics of the spindle are inputted into the device so that it will convert them into
the proper shear stress units.

Figure 6. Cone and Plate diagram

Figure 7. Picture of a small and large spindle and the cone (cup) in which they are installed

.
To determine the viscosity of any sample the following criteria need to be known:
1.
2.
3.
4.
5.
6.
7.

Test temperature
Sample Container size (or sample spindle/chamber geometry)
Sample volume required
Rheometer specifications
Characteristics of the spindle to be installed in the unit
Range of shear rates or speeds to be used
Time required for each test

The above described list is the criteria as required by Brookfield for their unit.
When determining viscosity it helps if the rheological model of the fluid is known. There
are generally four models or fluid types. These are listed below:

Newtonian- Viscosity is not dependent on shear rate.

have the same viscosity as one tested at 500 rpm.

A sample tested at 50 rpm will

Non-Newtonian- These fluids will not have the same viscosity at different shear rates.
The general rule is that as shear rate increases the viscosity will decrease. The general
description for this type of fluid is shear thinning.
Time Dependent- This category has two types, one in which the fluid will continue to
become less viscous as the test progresses at the same shear rate. This fluid would be
considered Thixotropic. A second category is pseudoplastic and the fluid will thin as
rate increases but will return to their original viscosity as the shear rate is decreased.
Of the above described fluid type we will primarily deal with Newtonian fluids in this
experiment. The fluid will have the same viscosity throughout the range of shear rates
and will only change with the temperature of the sample.
The discussion above was borrowed extensively from the Brookfield Engineering Manual
for the instrument.

Test Criteria
1.

Test Temperature

The test of the oil sample in this experiment will begin at room temperature. The
temperature will be increased at some rate until it reaches a temperature near bottom-hole
conditions. Periodically the sample will be tested at different temperatures. The final
temperature will depend on the well the sample came from and in some cases may not be
reached. From the data collected a predicted bottom-hole viscosity of the fluid can be
found from the data.
2.

Sample Container Size

For this test the sample size is dependent on the spindle. It can vary from 0.5-2.0 ml. In
this case we will probably be using 0.5. The volume is not a part of the analysis, but in
the testing procedure.
3.

Sample Volume

This item is keyed or related to item 2. This will be determined by the instructor as part
of the setup of the experiment.
4.

Rheometer Model

For this experiment we are using a Brookfield LDV-III cone and plate viscometer.
5.

Spindle Used

This is determined by the instructor before the lab. The size of the spindle is inversely
proportional to the viscosity. The larger the spindle the lower the range of viscosity
measurements. A better discussion of this will be seen in the attachments to this lab.
6.

Test Speed

This will be determined as we run the test. The greater the speed the more accurate the
test. In this case it is dependent on the spindle used as will as the sample and the range of
temperatures to be tested.
7.

Time Required for Each Test Point

For this item the manual asked for a minimum of 5 revolutions before data is taken.
Hopefully the shear rate will be great enough to limit test time to 1-3 minutes.

Test Procedure
Spindle Selection
To select spindle some idea of the fluid viscosity must be known. For most conventional
crude oils a viscosity range of 100 or less cp can be used. For heavy oils such as found in
Kern River or Venezuela a viscosity range of 10000cp could be used. In this case we will
probably use a range of 100 cp or less.
The following table gives the spindle and the range of shear rates and expected viscosities
for each:
Table 1. Spindle specifications for Brookfield Cone and Plate viscometer
Spindle

Shear Rate
(1/sec)

Viscosity cP

CP-40
CP-41
CP-42
CP-51
CP-52

0-1500
0-400
0-760
0-768
0-400

0.15-3036
0.58-11,510
0.3-6000
2.4-47,990
4.6-92,130

Calibration of Instrument

The instrument will be calibrated before the test but the following criteria must be met.
The measured viscosity of the fluid must be within a range of the viscosity of the
standard +/- 1% of the standards viscosity and 1% +/- the full scale viscosity of that
spindle at the test speed.
The following equation defines the full scale viscosity:
Cp = TK * SMC * 10,000/(test rpm)
TK and SMC are both specific for the spindle and rheometer used.

Table 2. Spindle constants for Cone and Plate viscometer

Spindle
CP-40
CP-41
CP-42
CP-51
CP-52

TK
0.09373
0.09373
0.09373
0.09373
0.09373

SMC
0.327
1.228
0.64
5.12
9.83

SRC
7.5
2
3.8
3.84
2

Calculate allowable range of viscosities for the unit:

RPM 12
Spindle CP-41
Viscosity of standard at 25C 100.2 cp
From the equation we find the full scale viscosity to be: 95.92 cp. The accuracy
variation for this test is +/- 1% or 0.9562 cp.
The accuracy of the viscosity standard is also +/- 1%. For this fluid the accuracy would
be 1.002 cp. By combining these terms the measured accuracy of the fluid during
calibration will be 100.2 cp +/- (0.9562+1.002) or 1.9582 cp.
As long as the unit returns a value within the calculated range for that spindle and fluid it
can be considered calibrated.
Sample Testing Procedure
The unit will be setup and calibrated before the experiment. This will allow more time
for testing and the elimination of problems before the test is conducted.
1.
2.

Take a sample of the appropriate volume as requested by the instructor and

place it in the cup.
Return the cup to the unit and allow the unit to stabilize at temperature. This
should only take a few minutes.

3.
4.
5.
6.

Set the unit to an rpm/shear rate that will be above 10% of the allowable
torque on the unit. Let it run for at least a minute or a minimum of 5
revolutions.
Note the temperature of the test, the shear rate in 1/sec and the shear stress in
dynes/cm2.
Change the shear rate if possible and take a second reading.
Adjust upwards the temperature at least 10C and repeat 3-5.

At the conclusion of the test the data can be used to determine the viscosity of the fluid.
For each temperature the viscosity can be determined by the following equation:
Viscosity (poise) = shear stress/shear rate

Rolling Ball Viscometer

Figure 8. Ruska falling ball viscometer

The Ruska rolling ball viscosimeter is used to determine the viscosity of bottom hole and
surface samples at elevated temperatures and pressures, up to 10,000 psi and 300 F. This
instrument operates on the rolling ball principle, where the roll time of a inch diameter
ball is used to obtain viscosity data.
The viscosity is calculated as

= Kt (ball fluid )

(4)

where
: viscosity
K: constant
ball : Density of the ball
fliud : Density of the fluid
t: roll back time
The driving force in this instrument is the difference in density between the fluid and the
ball. At a fixed temperature, the difference in ball and fluid density will be constant. The
viscosity will be directly proportional to the roll back time. The constant of the
viscometer must be determined by previous calibration using a liquid of known viscosity.
Operating sequence:
1) choose the correct ball size. If the fluid viscosity is estimated to be between 0 and
5 cP, a 0.252 or 0.248 inch diameter ball should be used. Above 25 cP, the 0.234
inch diameter ball will be appropriate
2) Clean the test assemblywith kerosene and vent air to ensure the chamber is free of
dust.
3) Place the ball in the bottom of the empty measuring barrel
4) Evacuate the test assembly. This is done by opening the vacuum pump valve at
the lower end of the unit and closing the charging valve
5) Charge the test sample fluid in the viscometer. The vacuum valve shold be closed
while the high pressure charging valve is reopened.
6) Rock the test assembly to obtain a single phase sample. The presence of gas
bubbles inside the chamber can prevent the ball from moving freely and stop the
experiment completely.
7) Set the temperature of the viscosimeter to the desired value. Allow 3 hours for the
temperature to estabilize.
8) Bring the ball to the hold position, by rotating the test unit 180 degrees.
9) Turn on the coil and switch to HOLD. The yellow light must be on
10) Rotate the assembly to the desired angle (70, 45, or 23), this will depend on
how viscous the fluid is.
11) Switch to FALL. The green light must be on. The ball is released and the time to
travel is displayed. When the ball hits the bottom, a sound alarm will be triggered.
12) Calculate the viscosity by using equation 4. with the appropriate values for the
constant. These values will be provided to you in the lab.
Required
1. Measure the kinematic viscosity of water, kerosene and motor oil at three
different temperatures using the Canon Fenske viscometer. Justify your selection
of tubes.
2. Using the Cone and Plate viscometer, construct a plot of viscosity versus
temperature for a sample of oil (77 to ~150 F). Construct the shear stress versus

shear rate plot for each fixed temperature in your experiment. Discuss your
observations.
3. Using the Ruska rolling ball viscometer, construct a plot of viscosity as a function
of pressure and temperature for a mixture of n-decane-methane. Start at 500 psia,
77 F. Increase the pressure to 700 psia and 1000 psia. Repeat the same
measurements for 100F and 200F. Do each measurement three times, at least at
two different angles.

General Guidelines for the Report

Follow the format for lab reports (check Useful Notes in the Technical Presentations
course as needed).
Abstract: What important lessons did you learn about these viscosity measurements?
Why are they valuable for petroleum engineers to know?
Conclusions: Evaluations, estimations, generalizations..
Introduction: Why is it important to measure rheological properties.
Discussion: You may want to include a Methods section, or you might want to introduce
your method for each part of this exercise as you discuss the various topic areas. Do
not regurgitate the lab manual; instead, tell us how you met its standards. If you made
any other decisions about how to proceed, explain what you did. Remember that we
know the procedure, but we gave you some opportunities to make choices, and we
need to know what choices you made. You have at least a couple of different figures
here. Be sure to have a Discussion section to handle each of them.
End Matter: If you used any symbols, be sure to include a Nomenclature; if you cited
your textbook or other resources for the Introduction, be sure to include a References
list. (Remember that lab notes/class notes cannot be cited.)
Appendix: The table you formatted to make your graphs should not be included in the
body of your report. Instead, include it (or any other extraneous materials) in an
Appendix.