Designation: D2196 − 15

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.

1. Scope or more speeds give better characterization of a non-Newtonian

1.1 These test methods cover the determination of the material than does a single viscosity measurement.
apparent viscosity and the shear thinning and thixotropic 3.2 With Test Methods B and C, the extent of shear thinning
properties of non-Newtonian materials in the shear rate range is indicated by the drop in viscosity with increasing rotational
from 0.1 to 50 s−1 using a rotational viscometer operating in a speed. The degree of thixotropy is indicated by comparison of
fluid of “infinite” dimensions. viscosities at increasing and decreasing rotational speeds (Test
1.2 The values stated in SI units are to be regarded as the Method B), viscosity recovery (Test Method B), or viscosities
standard. The values given in parentheses are for information before and after high shear (combination of Test Methods B
only. and C). The high-shear treatment in Test Method C approxi-
mates shearing during paint application. The viscosity behavior
1.3 This standard does not purport to address the safety measured after high shear is indicative of the characteristics of
concerns, if any, associated with its use. It is the responsibility the paint soon after application.
of the user of this standard to establish appropriate safety and
health practices and determine the applicability of regulatory
4. Apparatus
limitations prior to use.
4.1 Rotational Viscometer—The essential instrumentation
2. Summary of Test Method required providing the minimum rotational viscometer analyti-
2.1 Test Method A consists of determining the apparent cal capabilities for this method include:
viscosity of coatings and related materials by measuring the 4.1.1 A drive motor, to apply a unidirectional rotational
torque on a spindle rotating at a constant speed in the material. displacement to the specimen at at least for rotational speeds
between 0.05 and 6 rad/s (0.5 and 60 r/min) constant to within
2.2 Test Methods B and C consist of determining the shear 1 %.
thinning and thixotropic (time-dependent) rheological proper- 4.1.2 A force sensor to measure the torque developed by the
ties of the materials.2 The viscosities of these materials are specimen to the rotational displacement of the rotational
determined at a series of prescribed speeds of a rotational-type element to within 1 %.
viscometer operating in a fluid of “infinite” dimensions. The 4.1.3 A coupling shaft, or other means, to transmit the
agitation of the material immediately preceding the viscosity rotational displacement from the motor to the rotational ele-
measurements is carefully controlled. ment.
4.1.4 A rotational element, spindle, or tool, such as the
3. Significance and Use
cylindrical shape shown in Fig. 1, to fix the specimen between
3.1 Test Method A is used for determining the apparent the drive shaft and a stationary position.
viscosity at a given rotational speed, although viscosities at two
NOTE 1—Each rotational element covers a range of about 1.5 decades
of viscosity. The rotational element is selected so that the measured
1
viscosity (or torque) is between 10 and 90 % of the range of the rotational
These test methods are under the jurisdiction of ASTM Committee D01 on element.
Paint and Related Coatings, Materials, and Applications and are the direct
responsibility of Subcommittee D01.24 on Physical Properties of Liquid Paints & 4.1.5 A data collection device, to provide a means of
Paint Materials. acquiring, storing, and displaying measured or calculated
Current edition approved Feb. 15, 2015. Published April 2015. Originally
approved in 1963. Last previous edition approved in 2010 as D2196 – 10. DOI:
signals, or both. The minimum output signals required for
10.1520/D2196-15. rotational viscosity are torque, rotational speed, temperature,
2
Pierce, P. E., “Measurement of Rheology of Thixotropic Organic Coatings and and time.
Resins with the Brookfield Viscometer,” Journal of Paint Technology, Vol 43, No.
557, 1971, pp. 35–43. NOTE 2—Manual observation and recording of data are acceptable.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

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 D2196 − 15
NOTE 5—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 If the viscosities determined in 6.1 differ from the stated
values of the viscosity standard by more than 5 %, calculate
new calibration factors for each spindle/speed combination as
follows:
f 5 V/s (1)

where:
f = new factor for converting scale reading to viscosity,
mPa·s (cP),
V = viscosity of reference oil, mPa·s, and
s = reading of the viscometer.
6.3 Prepare a table of new calibration factors similar to that
furnished with the viscometer for the spindle/speed combina-
tions in 6.2. Spindle/speed factors vary inversely with speed.
FIG. 1 Cylindrical Rotational Element Configuration 7. Preparation of Specimen
7.1 Fill a 0.5-L (1-pt) or 1-L (1-qt) container with sample to
4.1.6 A stand, to support, level, and adjust the height of the
within 25 mm (1 in.) of the top with the sample and bring it to
drive motor, shaft and rotational element.
a temperature of 25°C 6 0.5°C or other agreed-upon tempera-
4.1.7 A level to indicate the vertical plumb of the drive
ture prior to test.
motor, shaft and rotational element.
4.1.8 Auxiliary instrumentation considered useful in con- 7.2 Vigorously shake the specimen on the shaker or equiva-
ducting this method includes: lent for 10 min, remove it from the shaker, and allow it to stand
4.1.8.1 Data analysis capability to provide viscosity, stress undisturbed for 60 min at 25°C prior to testing. Start the test no
or other useful parameters derived from the measured signals. later than 65 min after removing the container from the shaker.
Do not transfer the specimen from the container in which it was
4.2 A temperature measuring and recording device to pro-
shaken. Shake time may be reduced if necessary, or as agreed
vide specimen temperature of the fluid near the rotational
upon between the purchaser and manufacturer, but, in any case,
element over the range of 20 to 70°C to within 0.1°C (see Note
shall not be less than 3 min.
2). NOTE 6—Shake time may be reduced if necessary, if agreed upon
4.3 A cylindrical container with a capacity of 0.5-L (1-pt), between the purchaser and manufacturer, but, in any case, shall not be less
85 mm (33⁄8 in.) in diameter, or 1-L (1-qt), 100 mm (4 in.) in than 3 min.
diameter to contain the test specimen during testing. TEST METHOD A—APPARENT VISCOSITY
4.4 Shaker, or equivalent, machine capable of vigorously
shaking the test specimen. 8. Procedure
8.1 Make all measurements at 25 6 0.5°C, or other agreed-
5. Materials upon temperature.
5.1 Viscosity Reference Oils, calibrated in absolute 8.2 Place the instrument on the adjustable stand. Lower the
viscosity, milliPascal seconds. viscometer to a level that will immerse the spindle to the proper
6. Calibration of Apparatus depth. Level the instrument.
6.1 Select at least two reference oils of viscosities differing 8.3 Tilt the selected spindle (Note 3), insert it into one side
by at least 0.5 Pa·s (5P) within the viscosity range of the of the center of the surface of the material, and attach the
material being measured and in the range of the viscometer. spindle to the instrument.
Condition the oils to 25.0°C 60.5°C (or other agreed-upon NOTE 7—When connecting the spindle to the viscometer avoid undue
temperature) for 1 h in a 0.5-L (1-pt) container. Measure the side pressure which might affect alignment. Avoid rotating the spindle so
viscosities of each oil as described in Test Method B (Section that the viscometer indicator touches the stops at either extreme of the
scale.
12) taking readings only at increasing speeds (12.4). NOTE 8—Select the spindle/speed combination that will give a mini-
NOTE 3—Ensure that the spindle is centered in the container prior to mum scale reading of 10 % but preferably in the middle or upper portion
taking measurements. of the scale. The speed and spindle to be used may differ from this by
NOTE 4—Combining the tolerance of the viscometer (61 %, equal to agreement between user and producer.
the spindle/speed combination factor) and the tolerance of the temperature 8.4 Lower the viscometer until the immersion mark on the
control (typically 60.5°C at 25°C) it is reasonable to assume that a
shaft just touches the specimen. Adjust the viscometer level if
viscometer is calibrated if the calculated viscosities are within 65 % of
the stated values. necessary. Move the container slowly in a horizontal plane
until the spindle is located in the approximate center of the
container.

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 D2196 − 15
8.5 Initiate the rotation of the spindle. Adjust the rotational undisturbed for an agreed-upon rest period typically 1 minute.
speed so that the torque reads between 10 and 90 % of full. At the end of the rest period, start the spindle rotation at the
Allow the viscometer to run until reading stabilizes. Record the slowest speed and record the reading after ten revolutions (or
torque or viscosity reading. other agreed-upon number of revolutions).
NOTE 9—In thixotropic paints, the reading does not always stabilize. On
occasion it reaches a peak and then gradually declines as the structure is 13. Calculations and Interpretation of Results
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 13.1 Calculate the apparent viscosity at each speed as
manufacturer. shown in Section 8.
9. Calculation (Dial Reading Viscometer) 13.2 If desired, determine the degree of shear thinning by
the following method:
9.1 Calculate the apparent viscosity at each speed, as
13.2.1 Shear Thinning Index (sometimes erroneously called
follows:
the thixotropic index)—Divide the apparent viscosity at a low
V 5 fs (2) rotational speed by the viscosity at a speed ten times higher.
where: Typical speed combinations are 0.2 and 2 rad/s (2 and 20
r/min), 0.5 and 5 rad/s (–5 and 50 r/min), 0.6 and 6 rad/s (–6
V = viscosity of sample in mPa·s,
f = calibration factor furnished with instrument or deter- and 60 r/min) but selection is subject to agreement between
mined in Section 6, and producer and user. The resultant viscosity ratio is an index of
s = reading of viscometer. the degree of shear thinning over that range of rotational speed
with higher ratios indicating greater shear thinning.
10. Report 13.2.2 A regular or log-log plot of viscosity versus rota-
10.1 Report the following information: tional speed may also be useful in characterizing the shear-
10.1.1 The viscometer manufacturer, model and spindle, thinning behavior of the material. Such plots may be used for
10.1.2 The viscosity at the spindle and speed utilized, making comparisons between paints or other materials.
10.1.3 The specimen temperature in degrees Celsius, and 13.3 If desired, estimate the degree of thixotropy (under
10.1.4 The shake time and rest period, if other than speci- conditions of limited shearing-out of structure) by one of the
fied. following methods:
13.3.1 Calculate the ratio of the viscosity at the slowest
11. Precision and Bias rotational speed with increasing speed to that with decreasing
11.1 Precision—See Section 22 for precision, including that speed. The higher the ratio, the greater the thixotropy.
for measurement at a single speed. 13.3.2 Calculate the ratio of the viscosity at the slowest
11.2 Bias—No statement of bias is possible with this test speed taken after the rest period to that viscosity before the rest
method. period. The higher the ratio, the greater the thixotropy.

TEST METHOD B—VISCOSITY UNDER CHANGING 14. Report

SPEED CONDITIONS, DEGREE OF SHEAR 14.1 Report the following information:
THINNING AND THIXOTROPY 14.1.1 The viscometer manufacturer, model and spindle,
12. Procedure 14.1.2 The viscosities at increasing and decreasing spindle
speeds,
12.1 Make all viscosity (or torque) measurements at 25 6 14.1.3 The rest period time and the viscosity at the end of
5°C, or other agreed upon temperature. that time,
12.2 Adjust the instrument and attach the spindle as in 8.2 – 14.1.4 The specimen temperature in degrees Celsius, and
8.4. 14.1.5 The shake time if other than that specified.
12.3 Set the viscometer at the slowest rotational speed (Note 14.2 Optional Reporting:
9). Initiate the spindle rotation and record the reading after ten 14.2.1 Degree of Shear Thinning—Shear thinning index and
revolutions (or other agreed-upon number of revolutions). speeds over which it was measured (13.2).
14.2.2 Estimated Degree of Thixotropy (under conditions of
NOTE 10—A higher initial rotational speed may be used upon agree-
ment between producer and user. shearing-out of structure)—Ratio of the viscosities at the
lowest speed, for both increasing and decreasing speeds; or
12.4 Increase the rotational speed in steps and record the ratio of the viscosity at the lowest speeds before and after the
reading after ten revolutions (or equivalent time for each rest period, and speed at which they were measured (13.3).
spindle/speed combination) at each speed. After an observation
has been made at the top speed, decrease the rotational speed 15. Precision and Bias
in steps to the slowest speed, recording the reading after ten
revolutions (or equivalent time) at each speed. 15.1 Precision—See Section 22 for precision, including that
for measurement of the shear thinning index (ratio of viscosity
NOTE 11—It is preferable to change speed when the motor is running. at 0.5 rad/s to that at 5 rad/s (5 r/min to that at 50 r/min). It has
12.5 After the last reading has been taken at the slowest not been possible to devise a method for determining precision
speed, stop the rotation and allow the specimen to stand for viscosities at increasing and decreasing speeds other than as

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 D2196 − 15
individual measurements. No attempt was made to determine 20. Report
the precision of the measurement of the degree of thixotropy 20.1 Report the following information:
because this parameter is dependent on the material, the time of 20.1.1 The viscometer manufacturer, model and spindle,
the test, and other variables. 20.1.2 The viscosities at decreasing spindle speeds,
15.2 Bias—No statement of bias is possible with this test 20.1.3 The specimen temperature in degrees Celsius, and
method. 20.1.4 The speed of the high-speed mixer, size of blade, and
time of mixing if different from method.
TEST METHOD C—VISCOSITY AND SHEAR
20.2 Optional Reporting:
THINNING OF A SHEARED MATERIAL
20.2.1 Degree of Shear Thinning—Shear thinning index and
speed over which it was measured (13.2).
16. Apparatus
20.2.2 Estimated Thixotropy—Ratio of viscosities at lowest
16.1 High-speed laboratory stirrer with speeds of at least speed viscosities before and after shearing and the rotational
200 rad/s (2000 r/min) and equipped with a 50-mm (2-in.) speed at which they were measured.
diameter circular dispersion blade.3
21. Precision and Bias
17. Preparation of Specimen 21.1 Precision—The precision for individual viscosity mea-
17.1 Insert the 50-mm (2-in.) blade into the center of the surements is the same as for Test Method A in Section 22. No
container (7.1) so that the blade is about 25 mm (1 in.) from the attempt has been made to determine the precision of the shear
bottom. Run the mixer at 200 rad/s (2000 r/min) (Note 12) for thinning index or degree of thixotropy for Test Method C for
1 min. the reasons given in 15.1.
21.2 Bias—No statement of bias is possible with this test
NOTE 12—Materials may be sheared at other speeds using other size
blades upon agreement between producer and user.
method.
22. Summary of Precision
18. Procedure
22.1 In an interlaboratory study of Test Methods A and B,
18.1 Immediately insert the same spindle used in Test eight operators in six laboratories using dial reading apparatus
Method B into the sheared material in the same manner as in from a single supplier (Brookfield Engineering) measured on
Section 8. two days the viscosities of four architectural paints comprising
18.2 Initiate the spindle rotation at the highest speed used in a latex flat, a latex semi-gloss, a water-reducible gloss enamel,
Test Method B (12.5). Record the scale reading after ten and an alkyd semi-gloss, that covered a reasonable range in
revolutions (or other agreed-upon number of revolutions). 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
18.3 Decrease the rotational speed (Note 11) in steps and r/min) (equivalent to eight operators testing 16 samples) were
record the readings at each speed down to the lowest speed used to obtain the precision of Test Method A. The within-
used in Test Method B, recording the reading after ten laboratory coefficient of variation for Test Method A (single
revolutions at each speed (or other agreed-upon number of speed) was found to be 2.5 % with 121 df and for Test Method
revolutions). B (Shear Thinning Index) 3.3 % with 31 df. The corresponding
between-laboratories coefficients are 7.7 % with 105 df and
19. Calculations and Interpretation of Results 7.6 % with 27 df. Based on these coefficients the following
19.1 As in Test Method B, calculate the viscosities at each criteria should be used for judging the acceptability of results
decreasing speed. at the 95 % confidence level:
19.2 If desired, calculate the degree of shear thinning by the 22.1.1 Repeatability—Two results obtained by the same
method given in Test Method B, 13.2. The measured viscosity operator at different times should be considered suspect if they
behavior after shearing is essentially that of the paint immedi- differ by more than 7.0 % relative for single speed viscosity
ately after application (disregarding changes in solids). and 9.5 % relative for shear thinning index.
22.1.2 Reproducibility—Two results obtained by operators
19.3 If desired, estimate the degree of thixotropy (under in different laboratories should be considered suspect if they
conditions of complete shearing-out of structure) by calculating differ by more than 22 % relative, respectively, for the same
the ratio of the viscosities at the lowest speeds before and after two test methods.
shear. The viscosity at the lowest speed before-shearing is
taken from Test Method B, 13.1, at the lowest increasing speed. NOTE 13—Measurements made by digital apparatus from the same
supplier or apparatus from other suppliers may have different precision
The viscosity at lowest speed after-shear is taken from 19.1.
The higher the ratio, the greater the thixotropy. 23. Keywords
23.1 non-Newtonian; rheological properties; rheology; rota-
tional viscometer; rotational viscosity; shear thinning; thixo-
3
Cowles or Shar type mixer/disperser. tropic; thixotropy; viscometer; viscosity

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 D2196 − 15
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