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LUBRIZOL TEST PROCEDURE
TP-N01004
Edition: December 2, 2013
Previous Editions: August 10, 2000 / November 1, 2011
Determination of Viscosity Using A Brookfield
Viscometer for Conditioning Polymers
Scope
A material's flow property is an important in-process
and finished product parameter. It may be an
indicator of a product's performance in a coating
operation, its penetrating ability or ease of handling
or use. The interrelationship between viscosity and
other physical characteristics of a product e.g.,
color, solids content, etc., are useful indicators of
product quality, acceptance and performance.
Theory
Viscosity is the measure of the internal friction of a
fluid. This friction becomes apparent when a layer of
fluid is made to move in relation to another layer.
The greater the friction, the greater the amount of
force required to cause its movement, which is
called "shear". Shearing occurs whenever the fluid
is physically moved as in pouring, mixing, etc. The
measure of the speed at which these layers move
with respect to each other is called the "shear rate."
This has a unit of measurement called the
"reciprocal second" (sec-I). Highly viscous materials
thus require more force to move than less viscous
materials. The force per unit area required to
produce shearing action is called "shear stress." It
has a unit of measure called "dynes per square
centimeter" (dynes/cm2). Viscosity (n) can then be
described by the following equation:
shear stress
n = -------------------
shear rate
The fundamental unit of viscosity measurement is
the "poise." A material requiring a shear stress of
one dyne per square centimeter to produce a shear
rate of one reciprocal second has a viscosity of one
poise (P), or 100 centipoise (mPa·s). For this
method, the units reported will be centipoise
(mPa·s). The Brookfield viscometer rotates a disc
or cylinder in a fluid sample and measures the
torque needed to overcome the viscous resistance
to the induced movement. This is done by rotating
the spindle with an electric motor, through a
beryllium-copper spring. The degree to which the
spring is wound, measured by a deflection of a
needle on the viscometer's dial, is proportional to
the viscosity of the fluid. For precision measure-
ments between 0 and 100 centipoise, the UL
Adapter is used in conjunction with the viscometer.
It is important at this time to discuss Newtonian and
non-Newtonian fluids.
A Newtonian fluid is a material which has, at a
given temperature, a viscosity which is independent
of the shear rate. In other words, when the "shear
rate" is varied, the "shear stress" varies in the same
proportion. Typical Newtonian fluids include water
and thin motor oil. The Brookfield Viscosity
Standards are also Newtonian fluids.
In a non-Newtonian fluid, when the "shear rate" is
varied, the "shear stress" doesn't vary in the same
proportion or even necessarily in the same
direction. The viscosity of such fluids will change
as the shear rate is varied. The most common
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Lubrizol Test Procedure TP-N01004
Determination of Viscosity Using a Brookfield
Viscometer for Conditioning Polymers
Page 2 of 5
type of non-Newtonian fluids are called Pseudo-
plastic (the viscosity decreases as the "shear rate"
increases), Dilatent (viscosity increases as the "shear
rate" increases), and Plastic (this type of fluid will
behave as a solid under static conditions). The most
common non-Newtonian fluids (paints, emulsions
and dispersions) are of the Pseudoplastic type.
Some non-Newtonian fluids display a change in
viscosity with time under constant shear rate. There
are two categories of this type of fluid: Thixotropic
(the fluid's viscosity decreases with time as it is
sheared at a constant rate); and Rheopectic (the
fluid's viscosity increases with time as it is sheared at
a constant rate).
The information in this section is taken from "MORE
SOLUTIONS TO STICKY PROBLEMS" BROOK-
FIELD ENGINEERING LABORATORIES, INC.
Stoughton, Massachusetts.
Equipment
1. Brookfield Viscometer with UL Adapter, Model
LVF, or equivalent, or as specified in Routine
Product Control or Corporate Routine Raw
Material Control.
2. Mercury immersion thermometer, glass, 0° to
220°F graduated in at least 2°F increments, or
equivalent temperature indicator.
3. Constant temperature water bath or an
equivalent system for adjusting the
measurement temperature of a sample.
4. Griffin beakers, 600 mL, or larger, or any similar
container with a minimum inside diameter of 3 1/4
inches (83 mm). Containers of other sizes may be
required by Routine Product Controls, Corporate
Routine Raw Material Controls, an addendum, or
a Site Specific SOP or Policy.
5. Brookfield FACTOR FINDER (contains conver-
sion factors to convert dial readings to viscosities
in centipoise (mPa·s).
Reagents
1. Various Brookfield Viscosity Standards (such as
nominal 5, 10, 100, 1000, 5000, 12500 mPa·s),
or equivalent with NlST Traceable Certificates
of actual analysis.
2. For Merquat™ 2200 polymer:
a. Obazoline 662N.
b. Deionized water.
Method Standardization
1. Refer to Site SOP or Site Calibration
Procedure.
Instrument Operating Conditions
1. lnstrument Operating Conditions will vary
depending on the Model (Analog or Digital).
Refer to Site SOP or lnstrument Operation
Manual for current lnstrument Operating
Conditions.
2. The Viscometer must be level and the spindle
suitably centered in the test sample container.
3. The spindle must be properly immersed to the
groove found on its shaft.
a. To prevent the formation of bubbles under
and around the spindle, the spindle should
be immersed into the sample at a slight
angle before attaching to the viscometer.
This is especially true for viscous materials.b. All Brookfield Viscometers are calibrated at
the factory. The calibration of all Brookfield
Viscometers is based on immersion of the
spindle in a 600 cc low form Griffin beaker
(approximately 3 1/4" internal diameter).
Viscometer ranges will generally change if
smaller vessels are used. They will also
change as the spindle is brought near the
walls of the container. Guard legs must be
attached if furnished FACTOR FINDER is
used, particularly with the first two spindles
(#1 and #2).
c. The use of a container smaller than the 600
ml low form Griffen beaker will result in an
increase in viscosity readings, particularly
with the #1 and #2 spindles.
Lubrizol Test Procedure TP-N01004
Determination of Viscosity Using a Brookfield
Viscometer for Conditioning Polymers
Page 3 of 5
d. If specified, use a container smaller than the 600
ml Griffen beaker, the simplest approach is to
report the dimensions of the container and ignore
the probable effect on calibration. As long as
the same size container is used for all
subsequent test, there will be no correlation
problem. Alternately, the viscometer can be
recalibrated to compensate for the smaller
container.
Procedure
1. Consult the Product Specifications for the proper
model spindle number, speed of rotation (rpm),
sample size, sample temperature and, if
necessary, the container size. If not stated there,
determine the sample viscosity at the highest
speed of rotation which will give a reading toward
full scale. (The precision of the instrument
increases at this end of the scale).
2. Unless otherwise specified, transfer approximate-
ly 400 mL of sample to a 600 mL beaker and
adjust sample to the required measurement
temperature. Unless otherwise specified on the
Product Specification, this temperature adjust-
ment should be done to within +I°C or +2°F. Use
a water bath, if necessary.
3. Insert spindle in the test material until the fluid's
level is at the immersion groove cut in the
spindle's shaft. With disc type spindles, care
should be taken to avoid trapping air bubbles on
its surface. Tilt the beaker while immersing the
spindle or immerse spindle at an angle before
attaching to the viscometer.
4. Thread spindle to the instrument shaft in a
clockwise direction. Finger tighten the connection.
5. Position the sample so that the spindle is
centered in the test sample container. The
Brookfield factory calibration procedure uses
guard legs. Unless the instrument has been
recalibrated without the guard legs or the guard
legs are not required by Site Specific SOP or
Policy, it will be necessary to use guard legs for
viscosity measurements.
6. Check the level of the viscometer with the
bubble level. For accurate results, it is very
important that the leveling bubble is exactly
centered.
7. Unless otherwise instructed, take a reading
when the pointer or the digital display is stable.
Record this reading, and, if necessary, consult
the Factor Finder to obtain the proper factor for
the viscometer model, speed and spindle
number that was used.
a. The viscosity specification itself must be
met and reported using the speed, spindle,
and temperature listed in the appropriate
document. Any viscosity measurement not
meeting these requirements (spindle, speed
and temperature) will be deemed off-spec.
b. If the viscosity measurement is off-scale
high, go to the next higher spindle number
but do not change the rpm setting. If the
viscosity measurement is off-scale low, go
to the next lower spindle number but do not
change the rpm setting. This is for reporting
purposes only. The measured value will be
considered out of specification even if the
measured value lies within the specification
range when using different spindle and/or
speed.
Lubrizol Test Procedure TP-N01004
Determination of Viscosity Using a Brookfield
Viscometer for Conditioning Polymers
Page 4 of 5
8. UL Adapter - If specified, the UL Adapter (1-100
mPa·s) must be installed following the instruction
in the lnstrument Operations Manual.
a. Two UL Adapter tubes are available, an open
tube for measurements in tanks or beakers
and a closed tube which holds 16.0 mls of
sample. The open tube can be converted to a
closed tube using a plastic end cap provided
by Brookfield. The closed tubes can be
immersed in a constant temperature bath.
When using an open tube, immerse to the
groove in the side of the UL Adapter.
NOTE: Check the operating instructions for the
model used for the current UL Adapter equipment
available. This will also give the correct sample size
for measuring viscosity on a UL Adapter.
9. Adjust viscometer to the proper rpm setting as
stated in the appropriate document. When using
the UL Adapter, the proper rpm setting is
determined by the expected viscosity range of the
sample:
RPM Range (mPa·s)
60 0 - 10
30 0 - 20
12 0 - 50
6 0 - 100
10. If the UL Adapter was used on the Analog
Viscometer, obtain appropriate factor from the
following chart. This factor compensates for the
windage resistance encountered by the needle
indicate. THIS MAY NOT APPLY TO THE
MODELS WITH A DIGITAL READOUT. CHECK
THE OPERATING INSTRUCTIONS FOR THE
MODEL USED.
Multiply scale reading by this factor to get correct
viscosity.
RPM Range (mPa·s) Factor
60 0 - 10 0.1*
30 0 - 20 0.2**
12 0 - 50 0.5
6 0 - 100 1.0
* Deduct 0.4 from reading off 100 scale before multiplying
to correct for air resistance to rotation at 60 rpm.
**Deduct 0.1 from reading off 100 scale before multiplying
to correct for air resistance to rotation at 30 rpm.
11. If the UL Adapter dial reading is off-scale high,
go to the next lower rpm setting. The UL
Adapter is supplied with one spindle.
12. For Merquat™ 2200 polymer:
a. Pour 380 g of deionized water into a 600 ml
beaker.
b. Add 20 g of Merquat 2200 while stirring the
solution with a propeller-type stirrer. Mix for
1 hour.
c. Add 100 g of Obazoline 662N and mix for
30 minutes.
d. Measure the solution viscosity at 30°C using
a Brookfield viscometer, spindle #2 at 12
rpm.
Calculation and Data Reporting
1. Report viscosity, temperature, spindle number
and speed of rotation used. Remember that
the speed and spindle values as well as the
measurement temperature are part of the
product or raw material specification. For a
viscosity measurement to be in specification, it
must be made at the speed, spindle and
temperature specified. It is possible, therefore,
to have a viscosity measurement which meets
the centipoise range but be off spec if the
wrong spindle and speed have been used in
the measurement of that value.
2. Viscosity in mPa·s = Dial Reading x Factor.
Newer models (Digital) can be programmed to
read viscosity directly.
Performance Data
1. Range: 0 - 100,000 mPa·s.
2. Accuracy: The results obtained agree with
theoretical to within 1%. Brookfield viscome-
ters are guaranteed to be accurate to within
+I% of its full scale range.
3. Precision: The original performance data is
based on duplicate analyses of five samples
performed by each of three operators. Pooled
Standard Deviation: 27.21 mPa·s. Therefore,
the precision without the UL adapter is
estimated to be 282 mPa·s.
Lubrizol Test Procedure TP-N01004
Determination of Viscosity Using a Brookfield
Viscometer for Conditioning Polymers
Page 5 of 5
The standard deviation using the UL Adapter is
0.019 mPa·s as determined by one operator on
one sample of a Newtonian fluid (average 4.81
mPa·s) with a total of nine replicates yielding
eight degrees of freedom. The precision of the
test method is three times the standard deviation
and therefore estimated to be plus or minus 0.057
mPa·s. The method has percent relative standard
deviation (%RSD) of 1.2%.
The standarddeviation using a #2 spindle at 30
rpms is 1 .I3 mPa·s as determined by one
operator on one sample of a Newtonian fluid
(average 951.4 mPa·s) with a total of nine
replicates yielding eight degrees of freedom. The
precision of the test method is three times the
standard deviation, and therefore, estimated to be
k3.39 mPa·s. The method has percent relative
standard deviation (%RSD) of 0.36%.
4. Detection Limit: If you chose a spindle and speed
such that your full scale range is 0-1 00 mPa·s,
the Viscometer will measure any viscosity in this
region to 1.0 mPa·s.
5. Elapsed Time: 10 minutes
6. Operator Time: 10 minutes
References
See Restricted Page.
1. F. Daniels, R. A. Alberty, PHYSICAL CHEMISTRY,
4th Edition, John Wiley & Sons, lnc., NY, 1975
2. "Brookfield Synchro-Lectric Viscometer Instruction
Manual".
3. “More Solutions to Sticky Problems, A Guide To
Getting More From Your Brookfield Viscometer”,
Brookfield Engineering Labs, Inc.
4. Brookfield Engineering Laboratories Data Sheet
034-c, The Brookfield U.L. Adapter.
5. Brookfield Engineering Laboratories maintains a
library of technical papers on viscosity
measurement and control. Reprints are available
upon request at no charge. A current listing of
available papers and an order form are provided in
the booklet, TECHNICAL PAPERS ON
VISCOSITY MEASUREMENT AND CONTROL
(Data Sheet 091-C).
Determination of Viscosity Using A Brookfield
Viscometer for Conditioning Polymers