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Designation: D 724 – 99 An American National Standard

AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM

Standard Test Method for

Surface Wettability of Paper (Angle-of-Contact Method)1
This standard is issued under the fixed designation D 724; 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 2.2 TAPPI Standard:

1.1 This test method measures the angle of contact when a TAPPI Test Method T 458 Surface wettability of paper
drop of liquid is applied to the surface of a specimen of paper. (angle of contact method)4
1.2 The measurement of both the initial angle of contact and 3. Significance and Use
the angle of contact after a defined elapsed period of time may
be measured. 3.1 This test method is useful in measuring the interaction
1.3 A standard liquid (ink) for making measurements is of paper with liquids in a variety of applications.
described. 3.2 When using the standard ink described in this test
1.4 Other liquids including printing inks, writing inks, method, the contact angle measured initially is often consid-
adhesives, oils, and coating materials may be used upon ered a measure of the ruling quality of the paper.
agreement of those involved in the testing being done. 3.3 When using the same standard ink, the change in contact
1.5 Two types of apparatus for measuring the contact angle angle between the times specified in this test method, 5 and 60
using the procedure in this test method are described. Addi- s, is often considered a measure of writing quality of the paper
tional instruments that can perform the procedure in this test when an aqueous ink is used.
method may also provide equivalent results. A different proce- 3.4 In many applications, a contact angle between 90 and
dure using an automated instrument for measuring angle of 100 degrees, when a paper is tested with the standard ink,
contact will be found in Test Method D 5725 indicates that the paper will be suitable for general activities
1.6 The values stated in inch-pound units are to be regarded where water-based inks are used.
as the standard. The values given in parentheses are for 3.5 When this test method is used with specific non-
information only. standard inks of interest, or non-aqueous liquids, the users must
1.7 This standard does not purport to address all of the agree in advance the data to be collected and how the data will
safety concerns, if any, associated with its use. It is the be used.
responsibility of the user of this standard to establish appro- 3.6 Additional suggestions for more specific use of this test
priate safety and health practices and determine the applica- method will be found in Section 10.
bility of regulatory limitations prior to use. 4. Apparatus
2. Referenced Documents 4.1 Drop Projection Instrument—An instrument capable of
2.1 ASTM Standards: projecting the image of a drop of liquid on the surface of paper
D 585 Practice for Sampling and Accepting a Single Lot of onto a screen so that the angle of a line tangent with the drop
Paper, Paperboard, Fiberboard, or Related Products2 at the paper surface can be measured. The general concept is
D 685 Practice for Conditioning Paper and Paper Products shown in Fig. 1 and shall consist of the following:
for Testing2 NOTE 1—While the projection instrument illustrated and described is
D 5725 Test Method for Surface Wettability and Absor- antiquated, it describes the concept of the measuring procedure. Instru-
bency of Sheeted Materials Using an Automated Contact ments are available in a more convenient form that serve the same
Angle Tester2 purpose, that is projecting the image of the drop on a screen.
E 122 Practice for Choice of Sample Size to Estimate a 4.1.1 Angle Measuring Device—A protractor or similar
Measure of Quality for a Lot or Process3 device for measurement of contact angle.
4.1.2 Filter, used to reduce the heat on the specimen and
1
drop.
This test method is under the jurisdiction of ASTM Committee D-6 on Paper
and Paper Products and is the direct responsibility of Subcommittee D06.92 on Test
4.1.3 Lamp—A ventilated lamp house containing a light
Methods. source.
Current edition approved Feb. 10, 1999. Published May 1999. Originally
published as D 724 – 43. Last previous edition D 724 – 94.
2 4
Annual Book of ASTM Standards, Vol 15.09. Available from the Technical Association of the Pulp and Paper Industry,
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Annual Book of ASTM Standards, Vol 14.02. Technology Park/Atlanta, P.O. Box 105113, Atlanta, GA 30348.

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 NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.

D 724
Phenol, g 1.0
Soluble blue dye, Color Index 42755, Acid Blue 22, g 3.5
Water, distilled or deionized to make 1000 mL at 20°C (68°F)

All chemicals used in preparing the ink shall be of reagent

grade or equivalent quality. Some blue dyes react with phenol
to cause a film having a metallic appearance and such dyes
shall not be used. The ink shall be prepared as follows:
5.4.1 Dissolve the tannic acid and gallic acid in about 400
mL of water at about 50°C (122°F). In a separate vessel,
dissolve the ferrous sulfate in about 200 mL of water that
contains the hydrochloric acid. In a third vessel dissolve the
FIG. 1 Projection Apparatus dye in about 200 mL of water. Mix the three solutions in a 1-L
volumetric flask, rinse the vessels with small portions of water,
4.1.4 Microscope—A microscope draw tube suitable for and add the rinsings to the flask. Add the phenol. Dilute the
projecting the image of the drop on a screen with an enlarge- water to 1 L at 20°C (68°F).
ment of 25 to 30 times. 5.5 Water—Distilled or deionized.
4.1.5 Screen—A frosted glass screen on which the drop is 5.6 Other Liquids— Other liquids might be either aqueous-
projected is required. or nonaqueous-based. Some examples would be specified inks,
4.1.6 Stage—A horizontal stage capable of holding the test adhesive, oils, and coating materials.
specimen, with means for vertical adjustment of the stage.
6. Sampling
4.1.7 Tube and Lens— A tube capable of containing a lens
to concentrate the beam of light. 6.1 For acceptance sampling, obtain the sample in accor-
4.2 Hypodermic Syringe—A syringe, such as a 1-mL hypo- dance with Practice D 585.
dermic, equipped with a No. 27 stainless steel needle, capable 6.2 When sampling for other purposes, use Practice E 122
of providing 150 to 200 drops, 1 mL, is suitable for use with as an alternative.
water-like liquids. More viscous liquids may require a needle
7. Test Specimens
of different size.
4.3 Other instruments suitable for measuring contact angle 7.1 The test specimens shall be cut to a size appropriate for
include a device where the screen is replaced by a camera using the instrument being used. They shall be cut in such a way as
instant developing film. to be thoroughly representative of the sample. Tests shall be
4.4 Reflective Goniometer—An instrument consisting of a made on both sides of each specimen. The actual test areas
controlled light source, stage to hold the test specimen, and a tested shall not contain water marks or visible blemishes or
microscope for direct viewing of the drop on the paper defects and shall not be touched with the fingers or contami-
specimen is required. The microscope shall be fitted with an nated in any other way.
ocular graduated in degrees and adjustable so that the angle of 7.2 The test specimens shall be conditioned in accordance
contact between a line tangent to the drop at the paper surface with Practice D 685.
can be determined. 8. Procedure
5. Test Liquids 8.1 Test the specimens under standard atmospheric condi-
5.1 The liquid selected for testing purposes is a function of tions in accordance with Practice D 685.
the characteristic to be evaluated. The standard ink (see 5.4) is 8.2 Place the test specimen in the instrument, holding it in
used to determine writing characteristics of paper. The ink close contact with the stage by means of small weights, clips,
described is typical of that used in fluid ink writing instru- or whatever fixtures are associated with the instrument.
ments. 8.3 Set the tip of the hypodermic needle 3.2 mm (1⁄8 in.)
5.2 Water is used for determining wetting characteristics of from the surface of the specimen and deposit a drop of test
that liquid when paper is expected to be exposed to water only. liquid 1⁄150to 1⁄200 mL in size on the specimen.
5.3 Other liquids may be used using the technique described 8.4 For initial wettability, used as a measure of ruling
for special applications. There may be a need under those quality, make the measurement of the angle of contact after the
conditions to modify the test method from the standpoint of drop has been in contact with the paper for 5 s. For rate of
size of droplet used and the time at which contact angle is to be change of wettability, used as a measure of writing quality,
measured. Slow wetting liquids may be evaluated over a longer make two measurements, one after 5 s and the other after 60 s
time period. have elapsed.
5.4 Standard Ink— A standard ink having the following 8.5 Angle of Contact Measurement (see Fig. 2):
composition shall be used for determining the writing qualities 8.5.1 Projected Image Procedure—Project the image of the
of paper: drop enlarged on a glass screen, at the back of which shall be
clamped a sheet of transparent onionskin paper. Draw a
Tannic acid, g 11.5
Gallic acid crystals, g 3.8 horizontal line on the transparent paper coinciding with the
Ferrous sulfate 7 hydrate, g 15.0 image of the base of the drop and as soon as the specified time
Hydrochloric acid 1 N, mL 12.5 of contact of the drop with the specimen has elapsed, quickly

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 NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.

D 724
tendency of a writing paper to feather will be indicated by the
decrease in the angle of contact between measurement after 5
and 60 s. In hard-sized papers, the angle of contact will not
change perceptibly between the measurements at 5 and 60 s. If
the initial wettability is less than 90°, it is quite likely the paper
will feather as soon as it is written upon.
10.4 As the range in contact angle for specific conditions is
A 5 contact angle
D 5 drop of liquid
small, a refined technique is required in performing the test.
P 5 paper This is indicated by the above examples as well as by
T 5 tangent at paper surface theoretical considerations.
FIG. 2 Measuring Angle of Contact 11. Report
11.1 Report the following information:
draw two tangents to the curve at the two points of contact with
11.1.1 Standard Ink:
the base line. Measure the two interior angles between the base
11.1.1.1 The initial wettability or ruling quality shall be
line and the tangents with a protractor.
reported as the average angle of contact after 5-s exposure
8.5.2 Reflective Goniometer Procedure—Adjust the eye
expressed to the nearest degree,
piece and the internal measuring mechanism so that the interior
11.1.1.2 The rate of change of wettability or writing quality
angle of each of the two points of contact can be determined.
is reported as calculated in 9.1,
8.6 Make measurements for 5 drops on each side of the
11.1.1.3 If possible to identify the two sides, the results shall
specimen. The contact angle for each drop shall be the average
be identified as to the wire side and the felt side. Otherwise, the
of the angles at the two edges of the drop. If the two contact
size may be arbitrarily designated, as for example, A and B, and
angles are significantly different, the value should be elimi-
11.1.1.4 Test results shall be expressed as maximum, mini-
nated and the test repeated.
mum, and average for each side of the specimen tested,
9. Calculation reported to two significant figures.
11.1.2 Other Liquids— If liquids other than the standard ink
9.1 Calculation— Calculate the rate of change in wettability
are used, the liquid used along with any modifications of the
as follows:
procedures shall be reported.
R 5 ~A 2 a!/55
12. Precision and Bias
where: 12.1 Precision:
R 5 rate of change in wettability,°/ s, 12.1.1 When the procedure in this test method is applied by
A 5 average angle of contact after 5 s, and a single operator using the same equipment to paper whose
a 5 average angle of contact after 60 s.
surface characteristics impacting this test method are homoge-
10. Interpretation of Results neous, and where ten tests are run on the same side of two test
specimens cut from the same sheet of paper giving a result of
10.1 In considering the results of the angle-of-contact test,
90° or greater using this test method, the repeatability standard
the following factors that all affect the results in different
deviation is approximately 7° and the 95 % repeatability is 2°
degrees shall be considered: (a) the wetting power of the test
(see TAPPI T458).
liquid used, (b) the wettability of the sizing agent used in sizing
12.1.2 Using the data reported by Bristow,5 the reproduc-
the paper, and (c) the surface texture of finish of the paper.
ibility standard deviation is approximately 2.5° and the 95 %
10.2 The standard ink will give smaller angles of contact
reproducibility limit is approximately 7° for two different
than water, indicating that it wets the paper more readily than
operators using the same apparatus.
water. Papers surface-sized with starch will generally show
12.1.3 It is not practicable to specify in greater detail the
smaller angles than papers of about the same finish tube-sized
precision of the procedure for determining contact angle in this
with glue. A machine-finished paper with a grainy surface
test method because of variations in equipment, variations in
would have a greater angle of contact than a plated or
test liquid, and most specifically in paper coating uniformity
calendered paper of equal sizing. It is known that in practice,
which are encountered. It must be left to individual laboratories
ruling results will depend on both the surface wettability and
to determine precision estimates for specific paper grades and
finish of the paper. Thus, the angle of contact should give a
testing needs.
very good idea of what is to be expected. It has been found that
12.2 Bias—No statement can be made about the bias of the
excellent ruling will prevail when the average angle of contact
procedure in this test method because contact angle is defined
with water lies between 90 and 100°; when the angle of contact
in terms of the test method.
is greater than 110°, breaks are likely to occur in the ruled
lines; when the angle is smaller than 90°, the ruling fluid is 13. Keywords
likely to feather. 13.1 angle-of-contact; contact angle; paper; surface wetta-
10.3 In determining the writing qualities of paper by means bility
of the angle-of-contact method, it is necessary to take into
account that medium-sized papers will at times show feather- 5
Bristow, J.A., “The Reproducibility of Contact Angle Measurement,” Paperi ja
ing only after the ink has partly penetrated the paper. The Puu 50 (4a): 171, 1968.

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NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.

D 724
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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.

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if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
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