Professional Documents
Culture Documents
Rheological Properties of Non-Newtonian Materials by Rotational Viscometer
Rheological Properties of Non-Newtonian Materials by Rotational Viscometer
for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D2196 − 20
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
Copyright by ASTM Int'l (all rights reserved); Fri Jul 23 12:13:27 EDT 2021
1
Downloaded/printed by
Universidad Industrial de Santander (Universidad Industrial de Santander) pursuant to License Agreement. No further reproductions authorized.
D2196 − 20
5. Materials
5.1 Viscosity Reference Oils, calibrated in scientific units of
either Pascal-seconds, milliPascal-seconds, Poise, or centi-
poises.
Copyright by ASTM Int'l (all rights reserved); Fri Jul 23 12:13:27 EDT 2021
2
Downloaded/printed by
Universidad Industrial de Santander (Universidad Industrial de Santander) pursuant to License Agreement. No further reproductions authorized.
D2196 − 20
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°C 6 0.5°C, or other
agreed-upon temperature. 12. Procedure
8.2 Place the instrument on the adjustable stand. Lower the 12.1 Make all viscosity (or torque) measurements at 25°C 6
viscometer to a level that will immerse the spindle to the proper 0.5°C, or other agreed upon temperature.
depth. Level the instrument.
12.2 Adjust the instrument and attach the spindle as in 8.2 –
8.3 Tilt the selected spindle (Note 3), insert it into one side 8.4.
of the center of the surface of the material, and attach the
spindle to the instrument. 12.3 Decide upon the different rotational speeds to be used
for the test; a minimum of three speeds is recommended. Set
NOTE 6—When connecting the spindle to the viscometer avoid undue the viscometer at the slowest rotational speed chosen for the
side pressure which might affect alignment. Avoid rotating the spindle so
test (Note 8). Initiate the spindle rotation and record the
that the viscometer indicator touches the stops at either extreme of the
scale. reading after ten revolutions (or other agreed-upon number of
NOTE 7—Select the spindle/speed combination that will give a mini- revolutions).
mum scale reading of 10 % but preferably in the middle or upper portion
of the scale. The speed and spindle to be used may differ from this by NOTE 9—A higher initial rotational speed may be used upon agreement
agreement between user and producer. between producer and user.
8.4 Lower the viscometer until the immersion mark on the 12.4 Increase the rotational speed in steps and record the
shaft just touches the specimen. Adjust the viscometer level if reading after ten revolutions (or equivalent time for each
necessary. Move the container slowly in a horizontal plane spindle/speed combination) at each speed. After an observation
until the spindle is located in the approximate center of the has been made at the top speed, decrease the rotational speed
container. in steps to the slowest speed, recording the reading after ten
8.5 Initiate the rotation of the spindle. Adjust the rotational revolutions (or equivalent time) at each speed.
speed so that the torque reads between 10 % and 100 %. Allow 12.5 After the last reading has been taken at the slowest
the viscometer to run until reading stabilizes. Record the torque speed, stop the rotation and allow the specimen to stand
and the viscosity reading. undisturbed for an agreed-upon rest period, typically 1 minute.
NOTE 8—In thixotropic paints, the reading does not always stabilize. On At the end of the rest period, start the spindle rotation at the
occasion it reaches a peak and then gradually declines as the structure is
broken down. In these cases, the time of rotation or number of revolutions
slowest speed and record the reading after ten revolutions (or
prior to reading the viscometer should be agreed to between user and other agreed-upon number of revolutions).
manufacturer.
13. Calculations and Interpretation of Results
9. Calculation (Dial Reading Viscometer)
13.1 Calculate the apparent viscosity at each speed as
9.1 Calculate the apparent viscosity at each speed, as shown in Section 8. If using a dial reading viscometer,
follows: calculate the equivalent viscosity value for each torque value as
V 5 fs (1) shown in Section 10.
where: 13.2 If desired, determine the degree of shear thinning by
V = viscosity of sample in mPa·s, the following method:
f = conversion factor for spindle/speed combination fur- 13.2.1 Shear Thinning Index (sometimes called the thix
nished with instrument, index)—Divide the apparent viscosity at a low rotational speed
s = % torque reading of viscometer. by the viscosity at a speed ten times higher. Typical speed
combinations are 0.2 r/min and 2 r/min (2 r/min and 20 r/min),
10. Report 0.5 r/min and 5 r/min (5 r/min and 50 r/min), 0.6 r/min and 6
10.1 Report the following information: r/min (6 r/min and 60 r/min) but selection is subject to
10.1.1 The viscometer manufacturer, model and spindle, agreement between producer and user. The resultant viscosity
10.1.2 The viscosity at the spindle and speed utilized, ratio is an index of the degree of shear thinning over that range
10.1.3 The specimen temperature in degrees Celsius, and of rotational speed with higher ratios indicating greater shear
10.1.4 The shake time and rest period, if other than speci- thinning.
fied. 13.2.2 A regular or log-log plot of viscosity versus rota-
tional speed may also be useful in characterizing the shear-
11. Precision and Bias thinning behavior of the material. Such plots may be used for
11.1 Precision—See Section 22 for precision, including that making comparisons between paints or other materials.
for measurement at a single speed. 13.3 If desired, estimate the degree of thixotropy (under
11.2 Bias—No statement of bias is possible with this test conditions of limited shearing-out of structure) by one of the
method. following methods:
Copyright by ASTM Int'l (all rights reserved); Fri Jul 23 12:13:27 EDT 2021
3
Downloaded/printed by
Universidad Industrial de Santander (Universidad Industrial de Santander) pursuant to License Agreement. No further reproductions authorized.
D2196 − 20
13.3.1 Calculate the ratio of the initial viscosity reading to 18. Procedure
the final viscosity reading. Note that both readings were taken 18.1 Immediately insert the same spindle used in Test
at the same rotational speed. The higher the ratio, the greater Method B into the sheared material in the same manner as in
the thixotropy. Section 8.
13.3.2 Calculate the ratio of the viscosity at the slowest
speed taken after the rest period to that viscosity before the rest 18.2 Initiate the spindle rotation at the highest speed used in
period. The higher the ratio, the greater the thixotropy. Test Method B (12.5). Record the scale reading after ten
revolutions (or other agreed-upon number of revolutions).
14. Report 18.3 Decrease the rotational speed in steps and record the
14.1 Report the following information: readings at each speed down to the lowest speed used in Test
14.1.1 The viscometer manufacturer, model and spindle, Method B, recording the reading after ten revolutions at each
14.1.2 The viscosities at increasing and decreasing spindle speed (or other agreed-upon number of revolutions).
speeds,
19. Calculations and Interpretation of Results
14.1.3 The rest period time and the viscosity at the end of
that time, 19.1 As in Test Method B, calculate the viscosities at each
14.1.4 The specimen temperature in degrees Celsius, and decreasing speed if you are using a dial reading viscometer.
14.1.5 The shake time if other than that specified. 19.2 If desired, calculate the degree of shear thinning by the
14.2 Optional Reporting: method given in Test Method B, 13.2. The measured viscosity
14.2.1 Degree of Shear Thinning—Shear thinning index and behavior after shearing is essentially that of the paint immedi-
speeds over which it was measured (13.2). ately after application (disregarding changes in solids).
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 r/min to that at 5 r/min). 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
thinning index or degree of thixotropy for Test Method C for
17. Preparation of Specimen the reasons given in 15.1.
17.1 Insert the 50-mm (2-in.) blade into the center of the 21.2 Bias—No statement of bias is possible with this test
container (7.1) so that the blade is about 25 mm (1 in.) from the method.
bottom. Run the mixer at 200 rad/s (2000 r/min) (Note 10) for
1 min. 22. Summary of Precision
NOTE 10—Materials may be sheared at other speeds using other size 22.1 In an interlaboratory study of Test Methods A and B,
blades upon agreement between producer and user. eight operators in six laboratories using dial reading apparatus
from a single supplier (Brookfield Engineering) measured on
two days the viscosities of four architectural paints comprising
3
Cowles or Shar type mixer/disperser. a latex flat, a latex semi-gloss, a water-reducible gloss enamel,
Copyright by ASTM Int'l (all rights reserved); Fri Jul 23 12:13:27 EDT 2021
4
Downloaded/printed by
Universidad Industrial de Santander (Universidad Industrial de Santander) pursuant to License Agreement. No further reproductions authorized.
D2196 − 20
and an alkyd semi-gloss, that covered a reasonable range in differ by more than 7.0 % relative for single speed viscosity
viscosities and were shear thinning. Measurements at increas- and 9.5 % relative for shear thinning index.
ing speeds of 0.5 rad/s, 1.0 rad/s, 2.0 rad/s, and 5.0 rad/s (5 22.1.2 Reproducibility—Two results obtained by operators
r/min, 10 r/min, 20 r/min, and 50 r/min) (equivalent to eight in different laboratories should be considered suspect if they
operators testing 16 samples) were used to obtain the precision differ by more than 22 % relative, respectively, for the same
of Test Method A. The within-laboratory coefficient of varia- two test methods.
tion for Test Method A (single speed) was found to be 2.5 %
with 121 df and for Test Method B (Shear Thinning Index) NOTE 11—Measurements made by digital apparatus from the same
3.3 % with 31 df. The corresponding between-laboratories supplier or apparatus from other suppliers may have different precision
coefficients are 7.7 % with 105 df and 7.6 % with 27 df. Based
on these coefficients the following criteria should be used for 23. Keywords
judging the acceptability of results at the 95 % confidence 23.1 non-Newtonian; rheological properties; rheology; rota-
level: tional viscometer; rotational viscosity; shear thinning; thix
22.1.1 Repeatability—Two results obtained by the same index; thixotropic; thixotropy; viscometer; viscosity
operator at different times should be considered suspect if they
ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.
This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222
Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http://www.copyright.com/
Copyright by ASTM Int'l (all rights reserved); Fri Jul 23 12:13:27 EDT 2021
5
Downloaded/printed by
Universidad Industrial de Santander (Universidad Industrial de Santander) pursuant to License Agreement. No further reproductions authorized.