This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles

for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D2196 − 18´1

Standard Test Methods for

Rheological Properties of Non-Newtonian Materials by
Rotational Viscometer1
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 (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.

ε1 NOTE—Editorial corrections were made throughout in September 2018.

1. Scope determined at a series of prescribed speeds of a rotational

1.1 These test methods cover the determination of the viscometer with a spindle operating in a fluid contained in a
apparent viscosity and the shear thinning and thixotropic 600 mL low form Griffin beaker. The agitation of the material
properties of non-Newtonian materials in the shear rate range immediately preceding the viscosity measurements is carefully
from 0.1 to 50 s−1 using a rotational viscometer operating in a controlled.
fluid contained in a 600 mL low form Griffin beaker.
3. Significance and Use
1.2 The values stated in SI units are to be regarded as the
standard. The values given in parentheses are for information 3.1 Test Method A is used for determining the apparent
only. viscosity at a given rotational speed, although viscosities at two
or more speeds give better characterization of a non-Newtonian
1.3 This standard does not purport to address all of the material than does a single viscosity measurement.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 3.2 With Test Methods B and C, the extent of shear thinning
priate safety, health, and environmental practices and deter- is indicated by the drop in viscosity with increasing rotational
mine the applicability of regulatory limitations prior to use. speed. The degree of thixotropy is indicated by comparison of
1.4 This international standard was developed in accor- viscosities at increasing and decreasing rotational speeds (Test
dance with internationally recognized principles on standard- Method B), viscosity recovery (Test Method B), or viscosities
ization established in the Decision on Principles for the before and after high shear (combination of Test Methods B
Development of International Standards, Guides and Recom- and C). The high-shear treatment in Test Method C approxi-
mendations issued by the World Trade Organization Technical mates shearing during paint application. The viscosity behavior
Barriers to Trade (TBT) Committee. measured after high shear is indicative of the characteristics of
the paint soon after application.
2. Summary of Test Method
4. Apparatus
2.1 Test Method A consists of determining the apparent
viscosity of coatings and related materials by measuring the 4.1 Rotational Viscometer—The essential instrument will
torque on a spindle rotating at a constant speed in a 600 mL have the following capabilities at a minimum:
low form Griffin beaker. 4.1.1 A drive motor, to apply a unidirectional rotational
displacement to the spindle immersed in the specimen for
2.2 Test Methods B and C consist of determining the shear
rotational speeds between 0.307 and 10.24 rad/sec (0.3 and 100
thinning and thixotropic (time-dependent) rheological proper-
rpm) constant to within 0.01%.
ties of the materials.2 The viscosities of these materials are
4.1.2 A force sensor to measure the torque required to drive
the spindle immersed in the specimen at each of the defined
1
These test methods are under the jurisdiction of ASTM Committee D01 on speed settings to within 0.1%.
Paint and Related Coatings, Materials, and Applications and are the direct 4.1.3 A coupling shaft, or other means, to transmit the
responsibility of Subcommittee D01.24 on Physical Properties of Liquid Paints &
Paint Materials. rotational displacement from the motor to the spindle.
Current edition approved June 1, 2018. Published August 2018. Originally 4.1.4 A rotational element, spindle, or tool, such as the
approved in 1963. Last previous edition approved in 2015 as D2196 – 15. DOI: shapes shown in Fig. 1 to fix the specimen between the spindle
10.1520/D2196-18E01.
2
and a stationary surface. The protective bracket, which attaches
Pierce, P. E., “Measurement of Rheology of Thixotropic Organic Coatings and
Resins with the Brookfield Viscometer,” Journal of Paint Technology, Vol 43, No. to the viscometer and protects the spindle, provides the
557, 1971, pp. 35–43. stationary surface described in the preceding sentence.

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 D2196 − 18´1
5. Materials
5.1 Viscosity Reference Oils, calibrated in scientific units of
either Pascal-seconds, milliPascal-seconds, Poise, or centi-
poises.

6. Calibration Verification of Apparatus

6.1 Select one viscosity reference oil within the viscosity
range of the material being measured. Condition the oil to
25.0°C 6 0.1°C (or other agreed-upon temperature) for 1 h in
a 600 mL low form Griffin beaker (or equivalent container).
Select an appropriate spindle, connect it to the viscometer, and
attach the bracket. Immerse the spindle and bracket into the oil
and allow these items to equilibrate to temperature during the
1 h period. Measure the oil viscosity at three increasing
rotational speeds which give torque readings between 10 %
and 100 %.
NOTE 3—Ensure that the spindle is centered in the container prior to
taking measurements.
NOTE 4—Reference oils can exhibit a change in viscosity of about
7 % ⁄°C. If measurements are not made at 25°C, then the stated viscosities
shall be corrected to the temperature at which they are measured.
6.2 Each measured viscosity value must be within the
following calculation for the viscometer to pass the calibration
FIG. 1 Cylindrical and Disc Rotational Element Configuration check.
6.2.1 Determine the full scale viscosity range for the
NOTE 1—Each spindle can measure a range of almost four decades in spindle/speed combination being used. Calculate 1 % of this
viscosity for the speed settings specified in this method. The spindle is number.
selected so that the measured torque value is between 10 % and 100 %.
6.2.2 Calculate 1 % of the viscosity value for the reference
4.1.5 A data collection device, to provide a means of oil.
acquiring, storing, and displaying measured or calculated
6.2.3 Add the viscosity values obtained in the two previous
signals, or both. The minimum output signals required for a
calculations. Add and subtract this sum from the actual
viscosity measurement are rotational speed of the spindle and
viscosity value for the reference oil. The measured viscosity
torque. Best practice is to record output signals for time of
value must fall between these calculated limits for the viscom-
spindle rotation when making the viscosity measurement and
the temperature of the specimen. eter to pass the calibration check.
6.2.4 If any of the three viscosity measurements do not pass,
NOTE 2—Manual observation and recording of data are acceptable. repeat the test. If the test is still not successful, contact the
4.1.6 A stand, to support, level, and adjust the height of the instrument manufacturer for service of the rotational viscom-
drive motor, shaft and rotational element. eter.
4.1.7 A level to indicate the vertical plumb of the drive
motor, shaft and rotational element. 7. Preparation of Specimen
4.1.8 Auxiliary instrumentation considered useful in con-
ducting this method includes: 7.1 Fill a 0.5-L (1-pt) or 1-L (1-qt) container with sample to
4.1.8.1 Data analysis capability to provide viscosity, stress within 25 mm (1 in.) of the top with the sample and bring it to
or other useful parameters derived from the measured signals. a temperature of 25°C 6 0.5°C or other agreed-upon tempera-
ture prior to test.
4.2 A temperature measuring and recording device to pro-
vide specimen temperature of the fluid near the rotational 7.2 Vigorously shake the specimen on the shaker or equiva-
element over the range of 20 to 70°C to within 0.1°C (see Note lent for 10 min, remove it from the shaker, and allow it to stand
2). undisturbed for 60 min at 25°C prior to testing. Start the test no
later than 65 min after removing the container from the shaker.
4.3 A 600 mL low form Griffin beaker or equivalent
Do not transfer the specimen from the container in which it was
cylindrical container with minimum volume capacity of 500
shaken. Shake time may be reduced if necessary, or as agreed
mL, minimum diameter of 85 mm (3.35 in.), and minimum
depth of 100 mm (3.94 in.) to contain the specimen during upon between the purchaser and manufacturer, but, in any case,
testing. shall not be less than 3 min.
NOTE 5—Shake time may be reduced if necessary, if agreed upon
4.4 Shaker, or equivalent, machine capable of vigorously between the purchaser and manufacturer, but, in any case, shall not be less
shaking the test specimen. than 3 min.

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 D2196 − 18´1
TEST METHOD A—APPARENT VISCOSITY TEST METHOD B—VISCOSITY UNDER CHANGING
SPEED CONDITIONS, DEGREE OF SHEAR
8. Procedure THINNING AND THIXOTROPY
8.1 Make all measurements at 25 6 0.5°C, or other agreed- 12. Procedure
upon temperature.
12.1 Make all viscosity (or torque) measurements at 25 6
8.2 Place the instrument on the adjustable stand. Lower the 0.5°C, or other agreed upon temperature.
viscometer to a level that will immerse the spindle to the proper
depth. Level the instrument. 12.2 Adjust the instrument and attach the spindle as in 8.2 –
8.4.
8.3 Tilt the selected spindle (Note 3), insert it into one side
of the center of the surface of the material, and attach the 12.3 Decide upon the different rotational speeds to be used
spindle to the instrument. for the test; a minimum of three speeds is recommended. Set
the viscometer at the slowest rotational speed chosen for the
NOTE 6—When connecting the spindle to the viscometer avoid undue test (Note 8). Initiate the spindle rotation and record the
side pressure which might affect alignment. Avoid rotating the spindle so reading after ten revolutions (or other agreed-upon number of
that the viscometer indicator touches the stops at either extreme of the
scale. revolutions).
NOTE 7—Select the spindle/speed combination that will give a mini- NOTE 9—A higher initial rotational speed may be used upon agreement
mum scale reading of 10 % but preferably in the middle or upper portion between producer and user.
of the scale. The speed and spindle to be used may differ from this by
agreement between user and producer. 12.4 Increase the rotational speed in steps and record the
8.4 Lower the viscometer until the immersion mark on the reading after ten revolutions (or equivalent time for each
shaft just touches the specimen. Adjust the viscometer level if spindle/speed combination) at each speed. After an observation
necessary. Move the container slowly in a horizontal plane has been made at the top speed, decrease the rotational speed
until the spindle is located in the approximate center of the in steps to the slowest speed, recording the reading after ten
container. revolutions (or equivalent time) at each speed.

8.5 Initiate the rotation of the spindle. Adjust the rotational 12.5 After the last reading has been taken at the slowest
speed so that the torque reads between 10 and 100 %. Allow speed, stop the rotation and allow the specimen to stand
the viscometer to run until reading stabilizes. Record the torque undisturbed for an agreed-upon rest period typically 1 minute.
and the viscosity reading. At the end of the rest period, start the spindle rotation at the
NOTE 8—In thixotropic paints, the reading does not always stabilize. On slowest speed and record the reading after ten revolutions (or
occasion it reaches a peak and then gradually declines as the structure is other agreed-upon number of revolutions).
broken down. In these cases, the time of rotation or number of revolutions
prior to reading the viscometer should be agreed to between user and 13. Calculations and Interpretation of Results
manufacturer. 13.1 Calculate the apparent viscosity at each speed as
shown in Section 8. If using a dial reading viscometer,
9. Calculation (Dial Reading Viscometer) calculate the equivalent viscosity value for each torque value as
9.1 Calculate the apparent viscosity at each speed, as shown in Section 10.
follows: 13.2 If desired, determine the degree of shear thinning by
V 5 fs (1) the following method:
where: 13.2.1 Shear Thinning Index (sometimes called the thix
index)—Divide the apparent viscosity at a low rotational speed
V = viscosity of sample in mPa·s, by the viscosity at a speed ten times higher. Typical speed
f = conversion factor for spindle/speed combination fur-
combinations are 0.2 and 2 rpm (2 and 20 rpm), 0.5 and 5 rpm
nished with instrument,
(5 and 50 rpm), 0.6 and 6 rpm (6 and 60 rpm) but selection is
s = % torque reading of viscometer.
subject to agreement between producer and user. The resultant
10. Report viscosity ratio is an index of the degree of shear thinning over
that range of rotational speed with higher ratios indicating
10.1 Report the following information: greater shear thinning.
10.1.1 The viscometer manufacturer, model and spindle, 13.2.2 A regular or log-log plot of viscosity versus rota-
10.1.2 The viscosity at the spindle and speed utilized, tional speed may also be useful in characterizing the shear-
10.1.3 The specimen temperature in degrees Celsius, and thinning behavior of the material. Such plots may be used for
10.1.4 The shake time and rest period, if other than speci- making comparisons between paints or other materials.
fied.
13.3 If desired, estimate the degree of thixotropy (under
11. Precision and Bias conditions of limited shearing-out of structure) by one of the
following methods:
11.1 Precision—See Section 22 for precision, including that 13.3.1 Calculate the ratio of the initial viscosity reading to
for measurement at a single speed. the final viscosity reading. Note that both readings were taken
11.2 Bias—No statement of bias is possible with this test at the same rotational speed. The higher the ratio, the greater
method. the thixotropy.

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 D2196 − 18´1
13.3.2 Calculate the ratio of the viscosity at the slowest 18.2 Initiate the spindle rotation at the highest speed used in
speed taken after the rest period to that viscosity before the rest Test Method B (12.5). Record the scale reading after ten
period. The higher the ratio, the greater the thixotropy. revolutions (or other agreed-upon number of revolutions).

14. Report 18.3 Decrease the rotational speed in steps and record the
readings at each speed down to the lowest speed used in Test
14.1 Report the following information: Method B, recording the reading after ten revolutions at each
14.1.1 The viscometer manufacturer, model and spindle, speed (or other agreed-upon number of revolutions).
14.1.2 The viscosities at increasing and decreasing spindle
speeds, 19. Calculations and Interpretation of Results
14.1.3 The rest period time and the viscosity at the end of
19.1 As in Test Method B, calculate the viscosities at each
that time,
decreasing speed if you are using a dial reading viscometer.
14.1.4 The specimen temperature in degrees Celsius, and
14.1.5 The shake time if other than that specified. 19.2 If desired, calculate the degree of shear thinning by the
method given in Test Method B, 13.2. The measured viscosity
14.2 Optional Reporting:
behavior after shearing is essentially that of the paint immedi-
14.2.1 Degree of Shear Thinning—Shear thinning index and
ately after application (disregarding changes in solids).
speeds over which it was measured (13.2).
14.2.2 Estimated Degree of Thixotropy (under conditions of 19.3 If desired, estimate the degree of thixotropy (under
shearing-out of structure)—Ratio of the viscosities at the conditions of complete shearing-out of structure) by calculating
lowest speed, for both increasing and decreasing speeds; or the ratio of the viscosities at the lowest speeds before and after
ratio of the viscosity at the lowest speeds before and after the shear. The viscosity at the lowest speed before-shearing is
rest period, and speed at which they were measured (13.3). taken from Test Method B, 13.1, at the lowest increasing speed.
The viscosity at lowest speed after-shear is taken from 19.1.
15. Precision and Bias The higher the ratio, the greater the thixotropy.
15.1 Precision—See Section 22 for precision, including that
for measurement of the shear thinning index (ratio of viscosity 20. Report
at 0.5 rpm to that at 5 rpm. It has not been possible to devise 20.1 Report the following information:
a method for determining precision for viscosities at increasing 20.1.1 The viscometer manufacturer, model and spindle,
and decreasing speeds other than as individual measurements. 20.1.2 The viscosities at decreasing spindle speeds,
No attempt was made to determine the precision of the 20.1.3 The specimen temperature in degrees Celsius, and
measurement of the degree of thixotropy because this param- 20.1.4 The speed of the high-speed mixer, size of blade, and
eter is dependent on the material, the time of the test, and other time of mixing if different from method.
variables. 20.2 Optional Reporting:
15.2 Bias—No statement of bias is possible with this test 20.2.1 Degree of Shear Thinning—Shear thinning index and
method. speed over which it was measured (13.2).
20.2.2 Estimated Thixotropy—Ratio of viscosities at lowest
TEST METHOD C—VISCOSITY AND SHEAR speed viscosities before and after shearing and the rotational
THINNING OF A SHEARED MATERIAL speed at which they were measured.
16. Apparatus
21. Precision and Bias
16.1 High-speed laboratory stirrer with speeds of at least
21.1 Precision—The precision for individual viscosity mea-
200 rad/s (2000 r/min) and equipped with a 50-mm (2-in.)
surements is the same as for Test Method A in Section 22. No
diameter circular dispersion blade.3
attempt has been made to determine the precision of the shear
17. Preparation of Specimen thinning index or degree of thixotropy for Test Method C for
the reasons given in 15.1.
17.1 Insert the 50-mm (2-in.) blade into the center of the
container (7.1) so that the blade is about 25 mm (1 in.) from the 21.2 Bias—No statement of bias is possible with this test
bottom. Run the mixer at 200 rad/s (2000 r/min) (Note 10) for method.
1 min.
22. Summary of Precision
NOTE 10—Materials may be sheared at other speeds using other size
blades upon agreement between producer and user. 22.1 In an interlaboratory study of Test Methods A and B,
eight operators in six laboratories using dial reading apparatus
18. Procedure from a single supplier (Brookfield Engineering) measured on
18.1 Immediately insert the same spindle used in Test two days the viscosities of four architectural paints comprising
Method B into the sheared material in the same manner as in a latex flat, a latex semi-gloss, a water-reducible gloss enamel,
Section 8. and an alkyd semi-gloss, that covered a reasonable range in
viscosities and were shear thinning. Measurements at increas-
ing speeds of 0.5, 1.0, 2.0, and 5.0 rad/s (5, 10, 20, and 50
3
Cowles or Shar type mixer/disperser. r/min) (equivalent to eight operators testing 16 samples) were

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 D2196 − 18´1
used to obtain the precision of Test Method A. The within- 22.1.2 Reproducibility—Two results obtained by operators
laboratory coefficient of variation for Test Method A (single in different laboratories should be considered suspect if they
speed) was found to be 2.5 % with 121 df and for Test Method differ by more than 22 % relative, respectively, for the same
B (Shear Thinning Index) 3.3 % with 31 df. The corresponding two test methods.
between-laboratories coefficients are 7.7 % with 105 df and
7.6 % with 27 df. Based on these coefficients the following NOTE 11—Measurements made by digital apparatus from the same
supplier or apparatus from other suppliers may have different precision
criteria should be used for judging the acceptability of results
at the 95 % confidence level:
22.1.1 Repeatability—Two results obtained by the same 23. Keywords
operator at different times should be considered suspect if they 23.1 non-Newtonian; rheological properties; rheology; rota-
differ by more than 7.0 % relative for single speed viscosity tional viscometer; rotational viscosity; shear thinning; thix
and 9.5 % relative for shear thinning index. index; thixotropic; thixotropy; viscometer; viscosity

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