ASTM D2196-99
(Test Method)Standard Test Methods for Rheological Properties of Non-Newtonian Materials by Rotational (Brookfield type) Viscometer
Standard Test Methods for Rheological Properties of Non-Newtonian Materials by Rotational (Brookfield type) Viscometer
SCOPE
1.1 These test methods cover the determination of the apparent viscosity and the shear thinning and thixotropic properties of non-Newtonian materials in the shear rate range from 0.1 to 50 s .
1.2 This standard does not purport to address the safety problems associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.>
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Designation: D 2196 – 99
Standard Test Methods for
Rheological Properties of Non-Newtonian Materials by
Rotational (Brookfield type) Viscometer
This standard is issued under the fixed designation D2196; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope 4.2 WithTestMethodsBandC,theextentofshearthinning
isindicatedbythedropinviscositywithincreasingviscometer
1.1 These test methods cover the determination of the
speed. The degree of thixotropy is indicated by comparison of
apparent viscosity and the shear thinning and thixotropic
viscosities at increasing and decreasing viscometer speeds
properties of non-Newtonian materials in the shear rate range
−1
(Test Method B), viscosity recovery (Test Method B), or
from 0.1 to 50 s .
viscosities before and after high shear (combination of Test
1.2 This standard does not purport to address the safety
Methods B and C).The high-shear treatment inTest Method C
concerns, if any, associated with its use. It is the responsibility
approximates shearing during paint application. The viscosity
of the user of this standard to establish appropriate safety and
behavior measured after high shear is indicative of the char-
health practices and determine the applicability of regulatory
acteristics of the paint soon after application.
limitations prior to use.
5. Apparatus
2. Referenced Documents
5.1 Rotational-type viscometers having at least four speeds,
2.1 ASTM Standards:
such as:
E1 Specification for ASTM Thermometers
5.1.1 Brookfield Viscometer, ModelLVF,orequivalenthav-
3. Summary of Test Method
ing four rotational speeds, or Model LVT having eight rota-
tional speeds, with set of four spindles; or
3.1 Test Method A consists of determining the apparent
5.1.2 Brookfield Viscometer, Model RVF, having four rota-
viscosity of coatings and related materials by measuring the
tional speeds, or Model RVT or equivalent having eight
torque on a spindle rotating at a constant speed in the material.
rotational speeds, with set of seven spindles.
3.2 Test Methods B and C consist of determining the shear
5.2 Thermometer—ASTM thermometer having a range
thinning and thixotropic (time-dependent) rheological proper-
from 20 to 70°C and conforming to the requirements for
ties of the materials. The viscosities of these materials are
Thermometer 49C as prescribed in Specification E1.
determined at a series of prescribed speeds of a rotational-type
5.3 Containers, round 1-pt (0.5-L) can, 3 ⁄8 in. (85 mm) in
viscometer. The agitation of the material immediately preced-
diameter, or 1-qt (1-L) can, 4 in. (100 mm) in diameter.
ing the viscosity measurements is carefully controlled.
5.4 Shaker, or equivalent machine capable of vigorously
4. Significance and Use
shaking the test specimen.
4.1 Test Method A is used for determining the apparent
6. Materials
viscosityatagivenrotationalspeed,althoughviscositiesattwo
6.1 Standard Oils, calibratedinabsoluteviscosity,millipas-
or more speeds better characterize a non-Newtonian material
cal seconds.
than does the single viscosity measurement.
7. Calibration of Apparatus
ThesetestmethodsareunderthejurisdictionofASTMCommitteeD-1onPaint 7.1 Select at least two standard oils of viscosities differing
and Related Coatings, Materials, and Applications and are the direct responsibility
by at least 5 P (0.5 Pa·s) within the viscosity range of the
of Subcommittee D01.24 on Physical Properties of Liquid Paints and Paint
material being measured and in the range of the viscometer.
Materials.
Condition the oils as closely as possible to 25.0°C (or other
Current edition approved April 10, 1999. Published May 1999. Originally
{1
published as D2196–63T. Last previous edition D2196–86 (1991) .
agreed-upon temperature) for 1 h in a 1-pt (0.5-L) can, 3 ⁄8in.
Annual Book of ASTM Standards, Vol 14.03.
(85 mm) in diameter. Measure the viscosities of each oil as
Pierce, P. E., “Measurement of Rheology of Thixotropic Organic Coatings and
described in Test Method B (Section 13) taking readings only
Resins with the Brookfield Viscometer,” Journal of Paint Technology, Vol 43, No.
557, 1971, pp. 35–43.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 2196
TABLE 2 Viscosity Variation of Cannon Viscosity Standards
at increasing speeds (13.7). Make certain that the spindle is
About the 25°C Temperature Point
centered in the container prior to taking measurements.
Cannon Viscosity Viscosity at 25°C, Viscosity Change With + 1°C
Standard cP (mPa·s) at 25°C, cP (mPa·s)
NOTE 1—The Brookfield LV and RV series viscometers are equipped
with a spindle guard leg. The spindle/speed multiplying factors (Table 1)
S-600 1 400 87.7 (6.26 %)
are designed for use with the guard leg in place except for the following S-2000 4 900 332 (6.77 %)
S-8000 20 000 1462.3 (7.31 %)
conditions: RV series when the factors are the same with or without the
guard leg for spindles No. 3 through 7; or LV series when the factors are
the same with or without the guard leg for spindles No. 3 and 4.
7.1.1 Calibration in a 1-pt (0.5-L) can is always possible
7.3 Prepare a table of new factors similar to that furnished
with the LV series viscometer with the guard leg attached.
with the viscometer (Table 1) for the spindle/speed combina-
Calibration of the RVseries viscometer in the 1-pt can must be tions worked out in 7.2. Spindle/speed factors vary inversely
donewithspindlesNo.3through7withouttheguardleg.Ifthe with speed.
No.1orNo.2spindlesaretobeused,calibrationiscarriedout
in the 1-qt (1-L) can with the guard leg attached. 8. Preparation of Specimen
7.2 Combining the tolerance of the viscometer (61%,
8.1 Fill a 1-pt or 1-qt can with sample to within 1 in. (25
equal to the spindle/speed factor) and the tolerance of the
mm)ofthetopwiththesampleandbringitascloseaspossible
temperaturecontrol(typically 60.5°Cat25°C)itisreasonable
to a temperature of 25°C or other agreed-upon temperature
to assume that a viscometer is calibrated if the calculated prior to test.
viscositiesarewithin 65%ofthestatedvalues(seeTable2for
8.2 Vigorously shake the specimen on the shaker or equiva-
examplesoftheconsiderablechangeinviscositywithtempera- lentfor10min,removeitfromtheshaker,andallowittostand
ture exhibited by standard oils). If measurements are not made undisturbed for 60 min at 25°C prior to testing (Note 2). Start
at 25°C, then the stated viscosities should be corrected to the the test no later than 65 min after removing the can from the
temperature at which they are measured. If the viscosities shaker. Do not transfer the specimen from the container in
which it was shaken.
determined in 7.1 differ from the stated values of the viscosity
standard by more than 5%, calculate new factors for each
NOTE 2—Shake time may be reduced if necessary, or as agreed upon
spindle/speed combination as follows:
between the purchaser and manufacturer, but, in any case, should not be
less than 3 min.
f 5 V/s (1)
TEST METHOD A—APPARENT VISCOSITY
where:
f 5 new factor for converting scale reading to viscosity,
cP (mPa·s),
9. Procedure
V 5 viscosity of standard oil, mPa·s, and
9.1 Make all measurements as close as possible to 25°C, or
s 5 scale reading of the viscometer.
other agreed-upon temperature.
9.2 Place the instrument on the adjustable stand. Lower the
viscometertoalevelthatwillimmersethespindletotheproper
TABLE 1 Factors for Converting Brookfield Dial Readings to depth. Level the instrument using the attached spirit level.
Centipoises (Millipascal Seconds)
9.3 Tilt the selected spindle (Note 3), insert it into one side
of the center of the surface of the material, and attach the
NOTE 1—M 51000.
spindle to the instrument as follows: Firmly hold the upper
RV Series Factors Spindles
Speed, rpm
shaft coupling with thumb and forefinger; screw left-hand
1 2 345 6 7
thread spindle coupling securely to the upper shaft coupling
0.5 200 800 2000 4000 8000 20M 80M
being very careful when connecting to avoid undue side
1 100 400 1000 2000 4000 10M 40M
pressure which might affect alignment.Avoid rotating the dial
2 50 200 500 1000 2000 5M 20M
2.5 40 160 400 800 1600 4M 16M
so that pointer touches the stops at either extreme of the scale.
4 25 100 250 500 1000 2.5M 10M
5 20 80 200 400 800 2M 8M NOTE 3—Select the spindle/speed combination that will give a mini-
10 10 40 100 200 400 1M 4M
mum scale reading of 10 but preferably in the middle or upper portion of
20 5 20 50 100 200 500 2M
the scale. The speed and spindle to be used may differ from this by
50 2 8 20 40 80 200 800
agreement between user and producer.
100 1 4 10 20 40 100 400
LV Series Factors Spindles
9.4 Lower the viscometer until the groove (immersion
Speed, rpm
12 3 4 mark) on the shaft just touches the material. Adjust the
viscometer level if necessary. Move the container slowly in a
0.3 200 1000 4000 20M
0.6 100 500 2000 10M
horizontal plane until the spindle is located in approximately
1.5 40 200 800 4M
thecenterofthecontainersothatthetestwillberuninaregion
3.0 20 100 400 2M
undisturbed by the lowering of the spindle.
6 10 50 200 1M
12 5 25 100 500
9.5 Turn on the viscometer. Adjust the viscometer to the
30 2 10 40 200
rpm selected (Note 3) for the material under test. Allow the
60 1 5 20 100
viscometertorununtilthepointerhasstabilized(Note4).After
D 2196
the pointer has stabilized, depress the clutch and switch off the 13.5 After the last reading has been taken at the slowest
motor so that when it stops, the pointer will be in view (Note speed, shut off the viscometer and allow it and the specimen to
5). stand undisturbed for an agreed-upon rest period.At the end of
the rest period, start the viscometer at the slowest speed and
NOTE 4—Inthixotropicpaints,thepointerdoesnotalwaysstabilize.On
record the scale rea
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