High-Shear Viscosity Using A Cone/Plate Viscometer: Standard Test Method For

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Designation: D 4287 – 00 (Reapproved 2005)

Standard Test Method for


High-Shear Viscosity Using a Cone/Plate Viscometer1
This standard is issued under the fixed designation D 4287; 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.

1. Scope application: brushing (see Test Method D 4958), spraying,


1.1 This test method covers the determination of the viscos- electrostatic disk, or roll coating.
ity of paints, varnishes, and related products at a rate of shear 4.2 This test method is suitable for all paints and varnishes
of 12 000 s−1. whether they are Newtonian in behavior or not. However, due
1.2 Paints and varnishes that dry very rapidly may not give to the narrow gap between the stationary and rotary parts of
reproducible results with this test method. Measurements made high-shear viscometers, this test method is more reproducible
at elevated temperatures may also give poor precision due to for paints having finer pigment dispersions as determined by
loss of volatiles and to drying. Test Method D 1210.
1.3 The values stated in SI units are to be regarded as 5. Apparatus
standard. No other units of measurement are included in this
standard. 5.1 Cone/Plate Type Viscometer,with cone/speed combina-
1.4 This standard does not purport to address all of the tion producing a rate of shear of 12 000 s−1. The viscometer
safety concerns, if any, associated with its use. It is the must provide a viscosity measurement rage of either 0 to 10 (P)
responsibility of the user of this standard to establish appro- or 0 to 5 (P) at the above mentioned shear rate. With higher
priate safety and health practices and determine the applica- viscosity materials, other cones and speeds may be used upon
bility of regulatory limitations prior to use. agreement between the producer and the user, but it should be
noted that these may give lower shear rates not truly represen-
2. Referenced Documents tative of application conditions. Refer to Fig. 1 and Fig. 2 of an
2.1 ASTM Standards: 2 analog and digital cone and plate viscometer.
D 1210 Test Method for Fineness of Dispersion of Pigment- NOTE 1—The SI units for viscosity are pascal-seconds (Pa·s = 10 P, 1
Vehicle Systems by Hegman-Type Gage mPa·s = 1 cP).
D 3925 Practice for Sampling Liquid Paints and Related
Pigmented Coatings 6. Reagents and Materials
D 4958 Test Method for Comparison of the Brush Drag of 6.1 Water or Solvent—The viscometer should be zeroed
Latex Paints according to the manufacturer’s specification. Zeroing proce-
dures that require liquid may be satisfied with water or a low
3. Summary of Test Method viscosity solvent such as xylene or mineral spirits.
3.1 The material to be tested is placed between the cone and 6.2 Mineral Oils—Three standard mineral oils with known
plate of a cone/plate viscometer, then subjected to a high shear viscosities (certified by an approved laboratory) lying between
rate while the viscosity is determined. 10 and 90 % of full scale to be used for calibrating the
instrument.3
4. Significance and Use
NOTE 2—Silicone oils should be avoided because of their tendency to
4.1 The viscosity value obtained by this test method gives contaminate instruments, containers and other equipment and because of
information about the flow properties of the material under the possibility of shear thinning behavior at high shear rates.
high-shear conditions similar to those encountered during
7. Sampling
7.1 Take a representative sample of the product to be tested
1
This test method is under the jurisdiction of ASTM Committee D01 on Paint
in accordance with Practice D 3925. If the sample has a
and Related Coatings, Materials, and Applications and is the direct responsibility of tendency to settle or separate on standing, it must be stirred or
Subcommittee D01.24 on Physical Properties of Liquid Paints and Paint Materials. shaken until homogeneous before a test specimen is taken from
Current edition approved May 15, 2005. Published June 2005. Originally it. The specimen must be free of any foreign matter or air
approved in 1983. Last previous edition approved in 2000 as D 4287 – 00.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
3
Standards volume information, refer to the standard’s Document Summary page on Such oils are available from The Cannon Instrument Co., P.O. Box 16, State
the ASTM website. College, PA 16801.

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

1
D 4287 – 00 (2005)

FIG. 2 Digital Cone and Plate Viscometer

constructed by taking viscometer readings for three oils and


plotting measured viscosity versus specified (correct) viscosity
for the oils. Subsequent measurements are corrected to true
viscosities through use of the curve.
8.3 Check the cones periodically for wear. Replace any cone
that shows a definite flattening of the apex. Some users have
FIG. 1 Analog Cone and Plate Viscometer
found it necessary to replace cones every year. Others have had
to do so more often when abrasive paints or pastes were being
tested.
bubbles and its volume must be sufficient to cover the portion 8.4 The determination must be made at a closely controlled
of the viscometer plate under the cone when the latter is temperature of 25 6 0.3°C , unless otherwise agreed. In order
brought into contact with the plate. to check the temperature control, carry out the test as outlined
in 9.1 with the standard refined mineral oil of the highest
8. Preparation of Apparatus viscosity. Allow the viscometer to run with this oil for 5 min
8.1 The viscometer should be zeroed on a daily basis when and determine whether the reading decreases. If the decrease is
in regular use or otherwise before use, according to the more than 10 %, the apparatus is unsuitable for the determina-
viscometer operating manual. With the analog-type viscometer, tion of viscosities at high rates of shear in accordance with this
if the pointer does not indicate zero, it may be adjusted by test method.
means of a lever on the left-hand side of the upper part of the NOTE 3—Many multitemperature cone/plate viscometers have heating,
instrument housing. If the instrument cannot be zeroed, adjust- but not cooling, capabilities. Therefore, runs with these viscometers at
ment should take place according to the manufacturer’s sug- 25°C should only be done at room temperatures at or below 22°C to
gestions. ensure that the plate temperature does not go above 25°C. .
8.2 Verify the calibration of the apparatus by following the
procedure in Section 9, but using standard refined mineral oils 9. Procedure
having Newtonian characteristics and known viscosities. If the 9.1 With the cone in the down position (in contact with the
viscometer reads the correct viscosity (or within 5 % of that plate), turn the instrument on and allow it to warm up for at
value) with two or more oils whose viscosities bracket those of least 5 min. For a multitemperature instrument, set at 25°C or
specimens to be tested, then the viscometer readings may be to an alternatively agreed upon temperature. Raise the cone to
used as is. If the viscometer readings do not give the correct the up position. Transfer a suitable amount of the product to be
viscosities for the oils, then a calibration curve must be tested to the plate, taking care to avoid the inclusion of air

2
D 4287 – 00 (2005)
bubbles, and again lower the cone to the down position. Wait 10.1.4 Rate of shear at which the determination was made
for 30 s to allow the specimen to attain the agreed upon (in reciprocal seconds),
temperature. 10.1.5 Temperature at which the determination was made,
9.2 Start the cone rotating and record the reading. When 10.1.6 Test results in poises, reported to the nearest 1 % of
using an analog viscometer, record the reading when the point the total range, that is, 0.05 P for 0 to 5 P-cones, 0.1 P for 0 to
becomes steady (Note 4). When using a digital viscometer, 10 P-cones, etc.,
record the reading directly from the digital display once it has 10.1.7 Any deviation, by agreement or otherwise, from the
been stabilized (Note 5). test procedures described, and
10.1.8 Date of the test.
NOTE 4—With an analog cone/plate viscometer, whether the reading
gives a direct indication of the viscosity or not, depends on the cone and 11. Precision and Bias 4
scale used.
NOTE 5—In some cases it is difficult to judge whether a constant 11.1 Precision—On the basis of an interlaboratory test of
reading has been obtained. However, if the reading does not become this test method in which eight operators in four laboratories
steady after 15 s, record the reading at 15 s and mention the lack of a tested six paints ranging in viscosity from 0.8 to 7.9 P on
constant reading in the test report. If highly accurate readings are required, analog cone/plate viscometers, the within-laboratory coeffi-
make the readings below 90 % of the scale. cient of variation was found to be 2.2 %, at 40 df. The
9.3 If the reading does not directly indicate the viscosity, between-laboratory coefficient of variation was found to be
multiply the reading by the appropriate conversion factor or 6.9 % at 34 df. Based on these results, the following criteria
use the appropriate calibration curve to obtain the viscosity. should be used for judging the acceptability of results at the
9.4 Clean both the cone and the plate carefully, employing 95 % confidence level:
a cloth or tissue and a suitable solvent. Take care to remove all 11.1.1 Repeatability—Two test results, each the mean of
of the test material and cleaning solvent. Do not use cleaning two determinations, obtained by the same operator should be
utensils that may damage the apparatus. Metal cleaning tools considered suspect if they differ by more than 6.3 % relative.
must never be used. 11.1.2 Reproducibility—Two results, each the mean of two
9.5 Repeat the determination with a second specimen. If the determinations, obtained by operators in different laboratories
two viscosity determinations differ by less than 7 %, calculate should be considered suspect if they differ by more than 19.9 %
their mean and report as the high-shear viscosity for the relative.
material. If they differ by more than 7 %, make a third 11.2 Bias—Since there is no accepted reference material
determination. If no two readings are within 7 % of each other, suitable for determining the bias for the procedure in this test
then the material is not suitable for testing by this test method. method, bias has not been determined.

10. Report 12. Keywords


10.1 Report the following information: 12.1 viscosity–paints/related coatings/materials; viscom-
10.1.1 Reference to this test method and the viscometer eter–ICI cone/plate; viscometer–cone/plate
used,
10.1.2 Type and identification of the product under test, 4
Supporting data are available from ASTM International Headquarters. Request
10.1.3 Type of cone used, RR:D01-1035.

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of infringement of such rights, are entirely their own responsibility.

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