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Astm D-4212

Viscosidad con copa Zahn

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100% found this document useful (2 votes)
397 views6 pages

Astm D-4212

Viscosidad con copa Zahn

Uploaded by

Dan Mat
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Designation: D 4212 – 99

Standard Test Method for


Viscosity by Dip-Type Viscosity Cups1
This standard is issued under the fixed designation D 4212; 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 3.1.2 Newtonian liquid—a liquid in which the viscosity is


1.1 This test method covers the determination of viscosity independent of the shear stress or shear rate. If the ratio of
of paints, varnishes, lacquers, inks, and related liquid materials shear stress to shear rate is not constant, the liquid is non-
by dip-type viscosity cups. This test method is recommended Newtonian.
for viscosity control work within one plant or laboratory and 4. Summary of Test Method
should be used to check compliance with specifications only
when sufficient controls have been instituted to ensure ad- 4.1 The cup is completely immersed in the material to be
equate comparability of results. tested, withdrawn, and the time for the material to flow through
1.2 Viscosity cups are designed for testing of Newtonian a hole in the base of the cup is measured.
and near-Newtonian liquids. If the test material is non- 5. Significance and Use
Newtonian, for example, shear-thinning or thixotropic, another
method, such as Test Methods D 2196, should be used. Under 5.1 Viscosity is a measure of the fluidity of a material.
controlled conditions, comparisons of the viscosity of non- Viscosity data are useful in the determination of the ease of
newtonian materials may be helpful, but viscosity determina- stirring, pumping, dip coating, or other flow-related properties
tion methods using controlled shear rate or shear stress are of paints and related fluids.
preferred. 5.2 This type of cup is used to measure viscosity because it
1.3 This standard does not purport to address all of the is easy to use, robust, and may be used in tanks, reservoirs, and
safety concerns, if any, associated with its use. It is the reactors.
responsibility of the user of this standard to establish appro- 5.3 There are other types of apparatus for measuring vis-
priate safety and health practices and determine the applica- cosity in the laboratory that provide better precision and bias,
bility of regulatory limitations prior to use. including the Ford viscosity cup (Test Method D 1200), and the
Brookfield viscometer (Test Methods D 2196).
2. Referenced Documents 5.4 Certain higher shear rate devices such as cone/plate
2.1 ASTM Standards: viscometers (Test Method D 4287) provide more information
D 1200 Test Method for Viscosity by Ford Viscosity Cup2 about sprayability, roll coatability, and other high-shear rate
D 2196 Test Methods for Rheological Properties of Non- related properties of coatings.
Newtonian Materials by Rotational (Brookfield) Viscom- 6. Apparatus
eter2
D 4287 Test Method for High Shear Viscosity Using the ICI 6.1 Zahn Viscosity Cup—No. 1 through No. 5 Zahn viscos-
Cone/Plate Viscometer2 ity cups made of corrosion- and solvent-resistant materials.
E 1 Specification for ASTM Thermometers3 The nominal capacity of the cup is 44 mL, but may vary from
43 to 49 mL, depending on the manufacturer. A diagram of a
3. Terminology Zahn cup is given in Fig. 1. The dimensions, including orifices,
3.1 Definitions: are only approximate because the cups are not made to a
3.1.1 near-Newtonian liquid—a liquid in which the varia- uniform specification. Each manufacturer produces a different
tion of viscosity with shear rate is small and the effect on cup and considerable variation between batches from some
viscosity of mechanical disturbances such as stirring is negli- manufacturers has been noted in the past. This is a major
gible. reason why Zahn cups should not be referenced in specifica-
tions between producer and user only when controls sufficient
1
to ensure adequate cup-to-cup and operator-to-operator com-
This test method is under the jurisdiction of ASTM Committee D-1 on Paint
and Related Coatings, Materials, and Applications and is the direct responsibility of
parison are included. (See Appendix X1 for additional infor-
Subcommittee D01.24 on Physical Properties of Liquid Paints and Paint Materials. mation on Zahn Cups.)
Current edition approved May 10, 1999. Published July 1999. Originally
published as D 4212 – 82. Last previous edition D 4212 – 93. NOTE 1—The various cup numbers are for identification of the viscosity
2
Annual Book of ASTM Standards, Vol 06.01. ranges within the series only and should not be used for comparison
3
Annual Book of ASTM Standards, Vol 14.03. between different kinds of cups, that is, a No. 2 Zahn cup has no

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

1
D 4212

NOTE 1—Dimensions are approximate only and may vary with the manufacturer and from batch to batch
FIG. 1 Zahn Cup Nominal Dimensions

relationship whatsoever with a No. 2 Shell cup. 6.2.1 Nominal Shell cup orifice diameters are listed in Table
X2.1. Cup Nos. 1 through 21⁄2 are recommended for use with
6.1.1 Nominal Zahn cup orifice diameters are listed in Table
X2.1. Cup No. 1 with the smallest orifice is used for determin- reduced rotogravure inks; No. 2 is for use with flexographic
ing the viscosity of thin-bodied materials. Cup No. 2 is for use inks; Nos. 3 through 4 are used for industrial enamels,
with clears, lacquers, enamels, and press-side adjustment of lacquers, flexographic, and gravure inks; Nos. 5 and 6 are used
flexographic inks; cups Nos. 3 and 4 are for use with more for heavy materials.
viscous paints and inks (No. 3 for manufacturing of flexo- 6.3 Calibration Thermometer—ASTM Saybolt Viscosity
graphic inks); and cup No. 5 is used for silk screen inks. Thermometer 17F having a range of 66 to 80°F and subdivi-
6.2 Shell Viscosity Cup4—No. 1 through No. 6 Shell vis- sions of 0.2°F, or 17C having a range of 19 to 27°C and
cosity cups made of stainless steel with a capacity of 23 mL subdivisions of 0.1°C, both conforming to the requirements of
and a 1-in. (25-mm) long capillary in the bottom and conform- Specification E 1. Thermometers having subdivisions other
ing to the dimensions shown in Fig. 2. than these may be used depending on the sensitivity of the
material to be tested, the demands of the application, and the
agreement between the purchaser and seller.
4
Shell cups may be obtained from the Norcross Corp., 255 Newtonville Ave.,
Newton, MA 02158. This committee is not aware of any other source for flow cups 6.4 Timer—Any timing device may be used provided that
having properties similar enough to the Shell cup to be included in this test method. the readings can be taken with a discrimination of 0.1 s or
If you have knowledge of a cup that should be considered, please provide details to better.
ASTM Headquarters. Your comments will receive careful consideration at a meeting
of the responsible technical committee,1 which you may attend.

2
D 4212

FIG. 2 Shell Cup

7. Test Materials perature and due to difficulty in obtaining adequate temperature


7.1 The material to be tested should be visibly homoge- control with dip cups, calibration is a difficult procedure that
neous and free from any foreign material or air bubbles. must be done with great care and knowledge.
10. Procedure
8. Temperature of Testing
10.1 Choose the proper cup so that the time of efflux will be
8.1 Measurements should be made at 77°F (25°C) unless
between 20 and 80 s. See Table 1 for viscosity ranges for the
otherwise specified. Temperature drift during the test should be
various cups.
kept to a minimum. The viscosities of paints and related
materials are highly dependent on temperature. Differences in NOTE 3—The formulas used in this test method to describe the
temperature between measurements can give substantially conversion from Zahn seconds to stokes are linear, the actual cup response
different viscosities (up to 5 % per °F). For careful work, the is not. The range of 20 to 80 s covers the most linear portion of each cup.
In addition, below 20 s, turbulent flow may cause additional inconsisten-
temperature should be taken in the efflux stream, but for
cies. Above 80 s, factors that may impact on the precision include; loss of
process control (such as monitoring a dip tank), this is not solvent (and therefore varying viscosity), “skinning” of the liquid in the
necessary. cup, intermittent flow.
8.2 A temperature correction curve may be constructed for
10.2 Immerse the cup in the container, which may be a can
each liquid by plotting viscosity (seconds) against temperature
or beaker, but is more likely to be a thinning or mixing tank or
over the expected temperature range. With this curve, a
even a resin reactor. Stir or agitate the fluid well to give
viscosity determined at one measured temperature may be
uniform temperature and density. Allow the cup to remain in
converted quickly to a viscosity at another temperature.
the fluid for 1 to 5 min to attain thermal equilibrium. (Because
NOTE 2—When dip cups are used for original purposes, that is thinning of their greater mass, Shell cups should remain in the fluid for
or monitoring of materials in tanks, coaters, etc., temperature is not the full 5 min.)
important. This is because the key to good operation is to maintain the
fluid within a certain range of dip cup-seconds regardless of the tempera- TABLE 1 Approximate Viscosity Ranges, cST (mm2/s) (Roughly
ture of the fluid. Corresponding to 20 to 80 s Flow Time)
9. Checking and Calibration of Cups Cup Number Zahn Cup Shell Cup
1A 5–60 2–20
9.1 Cups should be checked in accordance with the proce- 2 20–250 10–50
dure described in Appendix X2. The frequency of this depends 21⁄2 ... 20–80
upon the amount of use and care that the individual cup 3 100–800 30–120
31⁄2 ... 40–170
receives, and the level of precision required. 4 200–1200 70–270
9.2 Cups may be calibrated with standard fluids according 5 400–1800 125–520
to the procedure in Appendix X3. However, because the 6 ... 320–1300
viscosity of standard fluids can vary significantly with tem- A
The lower limit for the Zahn No. 1 cup is 35 s rather than 20 s.

3
D 4212
NOTE 4—Dip cups are not recommended for use with thixotropic (time between-laboratories coefficient of variation was 11.5 %.
dependent) materials but if used for them (such as gravure or flexographic Based on these coefficients the following criteria should be
inks), more vigorous agitation will be necessary to break up the structure used for judging the acceptability of results at the 95 %
before the measurement is made.
confidence level:
10.3 Lift the cup vertically out of the material in a quick, 13.1.1.1 Repeatability—Two results, each the mean of two
steady motion. As the top edge of the cup breaks the surface, measurements, obtained by the same operator should be
start the timer. During the time of flow, hold the cup vertically considered suspect if they differ by more than 11 % of their
no more than 15.2 cm (6 in.) above the level of the liquid. Stop mean value.
the timer at the first definite break in the stream at the base of 13.1.1.2 Reproducibility—Two results, each the mean of
the cup. The efflux time in seconds constitutes the viscosity. It two measurements, obtained by operators in different labora-
is common to make only a single measurement, but for greater tories should be considered suspect if they differ by more than
precision and accuracy the mean of two or more measurements 33 % of their mean value.
should be taken.
NOTE 6—The values used to determine the precision were obtained
NOTE 5—The cup should not be held by the loop handle during the under ideal conditions (a single set of cups), reproducibility in practice can
measurement process. Most manufacturers equip the cup with a ring be just as good, by employing strict controls and good techniques.
through the loop handle. Holding the cup by this ring will help to ensure
that the cup hangs vertically. 13.1.1.3 Bias—Bias does not apply to this test method as no
acceptable standards exist.
11. Care of Cups
NOTE 7—Since the precision values were obtained under ideal condi-
11.1 Following each determination, clean the cup with a tions (a single set of cups), reproducibility in practice probably is poorer
suitable solvent and a soft brush. Use no metal tools in contact than that given (perhaps as bad as 50 %).
with the instrument as nicks or wear of the drilled orifice affect
13.1.2 Shell Cups—Precision was determined on the basis
the accuracy of the cup.
of an interlaboratory test in which four laboratories tested
12. Report seven paints covering a broad range of viscosities. The
12.1 Report the efflux time to the nearest 0.2 s for Zahn or within-laboratory coefficient of variation was 3.2 % and the
Shell cup No. ___, manufactured by _____, (in the case of between-laboratories coefficient of variation was 6.3 %. Based
Zahn cups) the temperature of the fluid (where measured), and on these coefficients the following criteria should be used for
whether the result is from a single measurement or the mean of judging the acceptability of results at the 95 % confidence
two of more measurements. level:
13.1.2.1 Repeatability—Two results, each the mean of two
13. Precision and Bias measurements, obtained by the same operator should be
13.1 The most satisfactory results when using dip cups are considered suspect if they differ by more than 9 % of their
obtained when viscosity is being controlled at a single location mean value.
only. However, when comparisons between locations are made, 13.1.2.2 Reproducibility—Two results, each the mean of
cups from the same manufacturer must be used or other action two measurements, obtained by operators in different labora-
taken to ensure compatibility of results. The following criteria tories should be considered suspect if they differ by more than
can be used for judging the acceptability of results at the 95 % 18 % of their mean value.
confidence level: 13.1.2.3 Bias—Bias does not apply to this test method as no
13.1.1 Zahn Cups—Precision was determined on the basis acceptable standards exist.
of an interlaboratory test in which six laboratories used new
Zahn cups (all from the same set from the same manufacturer) 14. Keywords
to test eight paints covering a broad range of viscosities. The 14.1 dip cup(s); flow cup(s); Shell cup(s); viscosity; Zahn
within-laboratory coefficient of variation was 3.7 % and the cup(s)

4
D 4212
APPENDIXES

(Nonmandatory Information)

X1. ZAHN CUP DESIGN, MANUFACTURE, AND USE

X1.1 Zahn cups were designed (and manufactured by X1.2 Zahn cup patents have expired and Zahn-type cups
General Electric) as simple flow property devices for use in dip are available from several sources. Each manufacturer makes
tanks, flow coat reservoirs, etc. They were not designed to be cups that are somewhat different from those made by others.
viscometers or to be used as such. Zahn cup use usually Considerable batch-to-batch difference has been noted in the
involves thinning or maintaining a coating, adhesive, or ink at past from some manufacturers. Cup variations are not a
a certain consistency (so many Zahn-seconds) regardless of problem for consistent control of a bath or tank as long as
temperature. This is the beauty of dip cups. The operator appropriate comparisons are made with old cups, if required, to
knows that his or her tank, bath, or coater runs well over a maintain continuity of data. However, cup differences can
certain range of Zahn-seconds whether the plant temperature is cause great difficulty if cups are used to set producer-user
50°F or 100°F. The operator does whatever is necessary to keep specifications. Comparisons under such conditions require
the fluid within the range. In such an application the viscosity considerable attention to detail and practiced expertise.
at 25.0°C (77.0°F) is not important.

X2. DIP CUP CHECKING PROCEDURES

X2.1 The viscosity versus efflux time formulas published TABLE X2.1 Viscosity Standards Recommended for Checking
here are in wide use, however, not all Zahn-type cups are Cups
designed to comply with these formulas. Techniques for Cup Number Approximate Oil Viscosity
Nominal Orifice Diameter,
at 77°F (25°C), cST
ensuring continued calibration of cups that do not claim (mm)
(mm2/s)
compliance with these formulas include; comparison of current
Zahn
flow times for a standard fluid against the original flow time, 1 2.0 20
and comparison against a verified standard cup. The same 2 2.7 120
3 3.8 480
calibration verification methods of comparing a cup against 4 4.3 480
one in known condition applied to Zahn-type cups can be used 5 5.3 900, 1600
with Shell cups.
Shell
X2.2 Monitoring Cup Characteristics—A useful checking 1 1.8 9
2 2.4 9, 20
technique is to measure the efflux time for a new cup with a 21⁄2 2.7 35
given standard fluid, then check the cup periodically with the 3 3.1 35, 120
same oil at the same temperature to determine if the efflux time 31⁄2 3.5 120
4 3.8 120
has changed. If the time changes more than 20 % (or more than 5 4.6 120, 480
your process tolerance permits), the cup should be replaced. If 6 5.8 480
the change is small, it may be appropriate to use the cup as is,
or by applying a correction factor to subsequent efflux times,
depending on the degree of precision required. The correction
have a tendency to contaminate cups and containers and to change the
factor is equal to original standard–fluid efflux time divided by drainage characteristics of cups (especially cups with capillaries).
the current one. Recommended viscosities for standard fluids
for such tests are given in Table X2.1. X2.4 Comparing Cups—It sometimes is necessary to
compare one Zahn-type cup with another in order to settle a
X2.3 The viscosity of many standard fluids is very sensitive dispute, determine whether a new cup will give similar times to
to temperature variations, therefore, the temperature of the an old one, etc. The most usual technique is to dip both cups
fluid must be controlled closely during calibration testing. It is into the same container of standard fluid at the same time and
recommended that the fluid (and the cup) be held at the test once the temperature of both cups has stabilized, pull them out
temperature for at least 15 min prior to testing. together, timing both of them. The efflux times are compared
NOTE X2.1—Silicone fluid viscosity standards are not recommended. and a correction factor can be calculated. Sometimes paint or
Although they exhibit very little viscosity change with temperature, they another material is substituted for the oil.

5
D 4212

X3. CALIBRATION OF DIP CUPS

X3.1 Select the appropriate standard oil for the cup to be TABLE X3.1 ConstantsA for Use with Viscosity Formulas
checked (see Table X2.1). Cup K C

X3.2 Bring the cup and the standard fluid to a constant Zahn
1 1.1 29
temperature as close as possible to 77.0°F (25.0°C). Some 2 3.5 14
fluids sold as viscosity standards can vary in viscosity by 2 to 3 11.7 7.5
18 % per degree centigrade, higher viscosities typically having 4 14.8 5
5 23 0
the higher rate of change. Determine the time of efflux to the Shell
nearest 0.2 s using the procedure detailed in Section 10. Record 1 0.226 13
2 0.576 5
the temperature of the efflux stream. If it is not 77°F, correct the
21⁄2 0.925 3
viscosity of the standard fluid to the actual temperature. 3 1.51 2
Temperature versus viscosity data is available from most 31⁄2 2.17 1.5
4 3.45 1
suppliers of viscosity standards. 5 6.5 1
X3.3 Convert the time of flow in seconds to kinematic 6 16.2 0.5
A
viscosity as follows: Cup constants from Patton, T. C., Paint Flow and Pigment Dispersion, second
edition, John Wiley & Sons, New York, 1979, p. 82.
V 5 K ~t 2 c! (X3.1)

where: literature.5,6 No equations for Shell cups have been published.


V 5 kinematic viscosity, cST (mm2/s)
t 5 efflux time, s, and, X3.4 Calculate the correction factor by dividing the true
K, c 5 appropriate constants (from Table X3.1). kinematic viscosity of the standard fluid by the kinematic
X3.3.1 These equations represent linear or relatively linear viscosity calculated from the efflux time. This factor may then
portions of the overall viscosity-time curves for the cups. The be used to correct viscosity readings taken with the cup. The
linear equations have been chosen because it is much more product of the factor and an efflux time gives a corrected
straightforward to make time corrections based on linear viscosity in Zahn or Shell seconds.
equations than on nonlinear ones and they are adequate for
most applications. Zahn cup nonlinear equations that better fit 5
Euverard, M., ASTM Bulletin, Vol 162, No. 67, October 1950.
viscosity curves for some cups better may be found in the 6
Pierce, P. E., Journal of Paint Technology, Vol 42, No. 533, 1969, p. 383.

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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 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, 100 Barr Harbor Drive, West Conshohocken, PA 19428.

This standard is copyrighted by ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States. Individual
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