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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 The fundamental unit of viscosity measurement is
the "poise." A material requiring a shear stress of
A material's flow property is an important in-process one dyne per square centimeter to produce a shear
and finished product parameter. It may be an rate of one reciprocal second has a viscosity of one
indicator of a product's performance in a coating poise (P), or 100 centipoise (mPa·s). For this
operation, its penetrating ability or ease of handling method, the units reported will be centipoise
or use. The interrelationship between viscosity and (mPa·s). The Brookfield viscometer rotates a disc
other physical characteristics of a product e.g., or cylinder in a fluid sample and measures the
color, solids content, etc., are useful indicators of torque needed to overcome the viscous resistance
product quality, acceptance and performance. to the induced movement. This is done by rotating
the spindle with an electric motor, through a
Theory beryllium-copper spring. The degree to which the
spring is wound, measured by a deflection of a
Viscosity is the measure of the internal friction of a needle on the viscometer's dial, is proportional to
fluid. This friction becomes apparent when a layer of the viscosity of the fluid. For precision measure-
fluid is made to move in relation to another layer. ments between 0 and 100 centipoise, the UL
The greater the friction, the greater the amount of Adapter is used in conjunction with the viscometer.
force required to cause its movement, which is
called "shear". Shearing occurs whenever the fluid It is important at this time to discuss Newtonian and
is physically moved as in pouring, mixing, etc. The non-Newtonian fluids.
measure of the speed at which these layers move
with respect to each other is called the "shear rate." A Newtonian fluid is a material which has, at a
This has a unit of measurement called the given temperature, a viscosity which is independent
"reciprocal second" (sec-I). Highly viscous materials of the shear rate. In other words, when the "shear
thus require more force to move than less viscous rate" is varied, the "shear stress" varies in the same
materials. The force per unit area required to proportion. Typical Newtonian fluids include water
produce shearing action is called "shear stress." It and thin motor oil. The Brookfield Viscosity
has a unit of measure called "dynes per square Standards are also Newtonian fluids.
centimeter" (dynes/cm2). Viscosity (n) can then be
described by the following equation: In a non-Newtonian fluid, when the "shear rate" is
varied, the "shear stress" doesn't vary in the same
shear stress proportion or even necessarily in the same
n = ------------------- direction. The viscosity of such fluids will change
shear rate 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- Reagents


plastic (the viscosity decreases as the "shear rate"
increases), Dilatent (viscosity increases as the "shear 1. Various Brookfield Viscosity Standards (such as
rate" increases), and Plastic (this type of fluid will nominal 5, 10, 100, 1000, 5000, 12500 mPa·s),
behave as a solid under static conditions). The most or equivalent with NlST Traceable Certificates
common non-Newtonian fluids (paints, emulsions of actual analysis.
and dispersions) are of the Pseudoplastic type. 2. For Merquat™ 2200 polymer:
a. Obazoline 662N.
Some non-Newtonian fluids display a change in b. Deionized water.
viscosity with time under constant shear rate. There
are two categories of this type of fluid: Thixotropic Method Standardization
(the fluid's viscosity decreases with time as it is
sheared at a constant rate); and Rheopectic (the 1. Refer to Site SOP or Site Calibration
fluid's viscosity increases with time as it is sheared at Procedure.
a constant rate).
Instrument Operating Conditions
The information in this section is taken from "MORE
1. lnstrument Operating Conditions will vary
SOLUTIONS TO STICKY PROBLEMS" BROOK-
depending on the Model (Analog or Digital).
FIELD ENGINEERING LABORATORIES, INC.
Refer to Site SOP or lnstrument Operation
Stoughton, Massachusetts.
Manual for current lnstrument Operating
Conditions.
Equipment
2. The Viscometer must be level and the spindle
1. Brookfield Viscometer with UL Adapter, Model suitably centered in the test sample container.
LVF, or equivalent, or as specified in Routine
Product Control or Corporate Routine Raw 3. The spindle must be properly immersed to the
Material Control. groove found on its shaft.
2. Mercury immersion thermometer, glass, 0° to a. To prevent the formation of bubbles under
220°F graduated in at least 2°F increments, or and around the spindle, the spindle should
equivalent temperature indicator. be immersed into the sample at a slight
angle before attaching to the viscometer.
3. Constant temperature water bath or an This is especially true for viscous materials.
equivalent system for adjusting the
measurement temperature of a sample. b. All Brookfield Viscometers are calibrated at
the factory. The calibration of all Brookfield
4. Griffin beakers, 600 mL, or larger, or any similar Viscometers is based on immersion of the
container with a minimum inside diameter of 3 1/4 spindle in a 600 cc low form Griffin beaker
inches (83 mm). Containers of other sizes may be (approximately 3 1/4" internal diameter).
required by Routine Product Controls, Corporate Viscometer ranges will generally change if
Routine Raw Material Controls, an addendum, or smaller vessels are used. They will also
a Site Specific SOP or Policy. change as the spindle is brought near the
5. Brookfield FACTOR FINDER (contains conver- walls of the container. Guard legs must be
sion factors to convert dial readings to viscosities attached if furnished FACTOR FINDER is
in centipoise (mPa·s). 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 5. Position the sample so that the spindle is
ml Griffen beaker, the simplest approach is to centered in the test sample container. The
report the dimensions of the container and ignore Brookfield factory calibration procedure uses
the probable effect on calibration. As long as guard legs. Unless the instrument has been
the same size container is used for all recalibrated without the guard legs or the guard
subsequent test, there will be no correlation legs are not required by Site Specific SOP or
problem. Alternately, the viscometer can be Policy, it will be necessary to use guard legs for
recalibrated to compensate for the smaller viscosity measurements.
container.
6. Check the level of the viscometer with the
Procedure bubble level. For accurate results, it is very
important that the leveling bubble is exactly
1. Consult the Product Specifications for the proper centered.
model spindle number, speed of rotation (rpm),
sample size, sample temperature and, if 7. Unless otherwise instructed, take a reading
necessary, the container size. If not stated there, when the pointer or the digital display is stable.
determine the sample viscosity at the highest Record this reading, and, if necessary, consult
speed of rotation which will give a reading toward the Factor Finder to obtain the proper factor for
full scale. (The precision of the instrument the viscometer model, speed and spindle
increases at this end of the scale). number that was used.

2. Unless otherwise specified, transfer approximate- a. The viscosity specification itself must be
ly 400 mL of sample to a 600 mL beaker and met and reported using the speed, spindle,
adjust sample to the required measurement and temperature listed in the appropriate
temperature. Unless otherwise specified on the document. Any viscosity measurement not
Product Specification, this temperature adjust- meeting these requirements (spindle, speed
ment should be done to within +I°C or +2°F. Use and temperature) will be deemed off-spec.
a water bath, if necessary.
b. If the viscosity measurement is off-scale
3. Insert spindle in the test material until the fluid's high, go to the next higher spindle number
level is at the immersion groove cut in the but do not change the rpm setting. If the
spindle's shaft. With disc type spindles, care viscosity measurement is off-scale low, go
should be taken to avoid trapping air bubbles on to the next lower spindle number but do not
its surface. Tilt the beaker while immersing the change the rpm setting. This is for reporting
spindle or immerse spindle at an angle before purposes only. The measured value will be
attaching to the viscometer. considered out of specification even if the
measured value lies within the specification
4. Thread spindle to the instrument shaft in a range when using different spindle and/or
clockwise direction. Finger tighten the connection. 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 11. If the UL Adapter dial reading is off-scale high,
mPa·s) must be installed following the instruction go to the next lower rpm setting. The UL
in the lnstrument Operations Manual. Adapter is supplied with one spindle.
12. For Merquat™ 2200 polymer:
a. Two UL Adapter tubes are available, an open a. Pour 380 g of deionized water into a 600 ml
tube for measurements in tanks or beakers
beaker.
and a closed tube which holds 16.0 mls of
b. Add 20 g of Merquat 2200 while stirring the
sample. The open tube can be converted to a
solution with a propeller-type stirrer. Mix for
closed tube using a plastic end cap provided
by Brookfield. The closed tubes can be 1 hour.
immersed in a constant temperature bath. c. Add 100 g of Obazoline 662N and mix for
When using an open tube, immerse to the 30 minutes.
groove in the side of the UL Adapter. d. Measure the solution viscosity at 30°C using
a Brookfield viscometer, spindle #2 at 12
NOTE: Check the operating instructions for the rpm.
model used for the current UL Adapter equipment
available. This will also give the correct sample size Calculation and Data Reporting
for measuring viscosity on a UL Adapter.
1. Report viscosity, temperature, spindle number
9. Adjust viscometer to the proper rpm setting as and speed of rotation used. Remember that
stated in the appropriate document. When using the speed and spindle values as well as the
the UL Adapter, the proper rpm setting is measurement temperature are part of the
determined by the expected viscosity range of the product or raw material specification. For a
sample: viscosity measurement to be in specification, it
RPM Range (mPa·s) must be made at the speed, spindle and
60 0 - 10
30 0 - 20
temperature specified. It is possible, therefore,
12 0 - 50 to have a viscosity measurement which meets
6 0 - 100 the centipoise range but be off spec if the
wrong spindle and speed have been used in
10. If the UL Adapter was used on the Analog the measurement of that value.
Viscometer, obtain appropriate factor from the
following chart. This factor compensates for the 2. Viscosity in mPa·s = Dial Reading x Factor.
windage resistance encountered by the needle Newer models (Digital) can be programmed to
indicate. THIS MAY NOT APPLY TO THE read viscosity directly.
MODELS WITH A DIGITAL READOUT. CHECK
THE OPERATING INSTRUCTIONS FOR THE Performance Data
MODEL USED.
1. Range: 0 - 100,000 mPa·s.
Multiply scale reading by this factor to get correct
2. Accuracy: The results obtained agree with
viscosity.
RPM Factor
theoretical to within 1%. Brookfield viscome-
Range (mPa·s)
ters are guaranteed to be accurate to within
60 0 - 10 0.1*
30 0 - 20 0.2**
+I% of its full scale range.
12 0 - 50 0.5 3. Precision: The original performance data is
6 0 - 100 1.0 based on duplicate analyses of five samples
* Deduct 0.4 from reading off 100 scale before multiplying performed by each of three operators. Pooled
to correct for air resistance to rotation at 60 rpm. Standard Deviation: 27.21 mPa·s. Therefore,
**Deduct 0.1 from reading off 100 scale before multiplying the precision without the UL adapter is
to correct for air resistance to rotation at 30 rpm. 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 standard deviation 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).