D413-98 (Reapproved 2013)

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Designation: D413 − 98 (Reapproved 2013)

Standard Test Methods for


Rubber Property—Adhesion to Flexible Substrate1
This standard is issued under the fixed designation D413; 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 Purposes from Products


1.1 These test methods cover the determination of the 3. Summary of Test Method
adhesion strength between plies of fabric bonded with rubber
or the adhesion of the rubber layer in articles made from rubber 3.1 Two general test methods are given:
attached to other material. They are applicable only when the 3.1.1 Static-Mass Method, in which the force required to
adhered surfaces are approximately plane or uniformly circular cause separation between adhered surfaces is applied by means
as in belting, hose, tire carcasses, or rubber-covered sheet of gravity acting on a mass.
metal. 3.1.2 Machine Method, in which the force required to cause
separation between adhered surfaces is applied by means of a
1.2 When the adhered surfaces contain sharp bends, angles, tension machine.
or other gross irregularities that cannot be avoided in preparing
test specimens, special test methods must be employed for 3.2 Except as may be otherwise specified in these test
evaluating adhesion. methods, the requirements of Practices D3182 and D3183,
shall be complied with and are made a part of these test
1.3 The values stated in SI units are to be regarded as the methods.
standard. The values given in parentheses are for information
only. 3.3 In case of conflict between the provisions of these test
methods and those of detailed specifications or test methods for
1.4 This standard does not purport to address all of the a particular material, the latter shall take precedence.
safety problems, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 3.4 As covered by these test methods, an adhesion test
priate safety and health practices and determine the applica- consists of applying to a test specimen, under specified
bility of regulatory limitations prior to use. conditions, a (measured) force sufficient to strip from the
specimen at a measured rate, a layer of moderate thickness
2. Referenced Documents with separation (rupture, tearing) at the adhered surfaces. The
numerical value of the adhesion is expressed as (1) the average
2.1 ASTM Standards:2
force required to cause separation at a definite rate, or (2) the
D3040 Practice for Preparing Precision Statements for Stan-
average rate of separation caused by a known or specified
dards Related to Rubber and Rubber Testing (Withdrawn
force. In the machine test method, the rate of separation is fixed
1987)3
and the adhesion value must be expressed in terms of the
D3182 Practice for Rubber—Materials, Equipment, and Pro-
measured force. With the static-mass test method, either (1) or
cedures for Mixing Standard Compounds and Preparing
(2) can be used, but the latter is preferable and will be here
Standard Vulcanized Sheets
employed.
D3183 Practice for Rubber—Preparation of Pieces for Test
4. Significance and Use
1
These test methods are under the jurisdiction of ASTM Committee D11 on
4.1 These test methods are used to ensure the quality of a
Rubber and are the direct responsibility of Subcommittee D11.25 on Rubber product by determining the force per unit width required to
Adhesive Systems. separate a rubber layer from a flexible substrate such as fabric,
Current edition approved Nov. 1, 2013. Published January 2014. Originally fibre, wire, or sheet metal. The acceptable value of adhesion
approved in 1935. Last previous edition approved in 2007 as D413 – 98 (2007).
DOI: 10.1520/D0413-98R13. measured will, of course, vary from product to product due to
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or different rubber formulations, flexible substrates, and types of
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM products. However, once a product is established, minimum
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
values of separation force can be determined and agreed to by
3
The last approved version of this historical standard is referenced on producer and consumer and both can monitor to assure
www.astm.org. maintenance of the agreed-upon minimum value.

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

1
D413 − 98 (2013)
STATIC-MASS METHOD 6.1.1 Cut the specimen to 25 + 3, − 0 mm (1 + 0.125 − 0
in.) wide. The thickness will vary according to the construction
5. Apparatus of the article being tested. The maximum thickness of the
5.1 The apparatus required for the adhesion test by the specimen is limited to 13 mm (0.5 in.). To comply with this
static-mass test method consists of a supporting frame, testing requirement, slice or buff the specimen. The ply or layer being
clamps, mandrels, calibrated masses, and mass carriers. The separated should never be over 6.5 mm (0.25 in.) thick.
supporting frame is of such design that clamps for strip 6.1.2 Cut the specimen from the article in such a manner
specimens hang on it vertically and that mandrels for ring that the adhered parts have the same width where practicable.
specimens are supported on it horizontally. The frame has The technique used in 6.2.2 and 6.2.3 may be applied here.
sufficient height to permit the mass carrier to be suspended When necessary, or specified, cut only the layer to be separated
from the test specimens by means of clamps and to hang freely (by application of load) to the prescribed width. In such cases,
during the progress of the test. Provision also is made to remove the portions of that layer remaining outside of the test
support the mandrels so that they revolve freely with minimum width to avoid edge constriction during separation.
friction. Suitable apparatus is shown in Fig. 1 and Fig. 2. 6.1.3 Curved specimens for test in strip form shall have
curvature only in the length dimension of the specimen.
6. Test Specimens 6.2 Strip Specimens—Type B—The same as Type A, with
6.1 Strip Specimens—Type A—Plane strips having a width the exception of 90° peel and the separation line in the center
of 25 + 3, − 0 mm (1 + 0.125, − 0 in.), and a minimum length of the specimen.
such as to permit 180° peel separation over sufficient distance 6.2.1 Cut the specimen 35 mm (1 3⁄8 in.) wide. Remove the
to indicate the adhesion value. excess plies to obtain a thickness of 6 mm (1⁄4 in.) and leave the
separation line in the center of the specimen to ensure a 90°
peel.
6.2.2 Buff to a width of 30 mm (1 1⁄8 in.) with a coarse grit
emery cloth (grit No. 40) with care to prevent burning or
gumming the sides of the specimen.
6.2.3 Make a 2-mm (1⁄16-in.) deep slit with a knife along
each side exactly where the specimen is to be separated during
testing. Use a knife with an adjustable blade where only the
desired depth of cut (2 mm) of blade is exposed.
6.3 Ring Specimens—Closed rings having a width of 25 mm
(1 in.) and maximum internal diameter of 100 mm (4 in.).
6.3.1 Mount the article on a smooth, close-fitting, slightly
tapered wooden mandrel.
6.3.2 Rotate the mandrel (a lathe is preferred) and cut
25-mm (1-in.) wide ring sections by forcing a sharp pointed
knife gradually through the article.
6.3.3 Cut rings with internal diameters over 100 mm (4 in.)
through and open to form strip specimens.

7. Procedure
7.1 Strip Specimen: Type A, 180° Peel—Measure the width
of the strip cut to the nearest 0.2 mm (0.01 in.) and record.
Separate the parts to be tested by hand at one end of the strip
specimen and at a sufficient distance to permit the jaws of the
testing clamp to be attached. Suspend the strip from the
Dimen- Dimen-
sion
mm in.
sion
mm in. supporting frame by the separated end, holding in the jaws of
A 75.0 3 N 10.0 1⁄ 8
the testing clamp all separated ends except the one under test.
B 45.0 11⁄4 P 90.0 31⁄2 Attach to the lower end of the test specimen a minimum mass
C 37.5 11⁄2 R 30.0 11⁄4 sufficient to maintain the strip specimen in approximately a
D 15.0 3⁄8 S 20.0 3⁄ 4

E 40.0 111⁄16 T 18.0 23⁄32


vertical position. Or, hold the specimen against a vertical plate
F 15.0 1⁄8 U 30.0 11⁄8 in such a manner as to keep the specimen in approximately a
G 10.0 11⁄18 V 3.0 1⁄ 8
vertical position during the test to ensure a 180° peel. Apply a
H 11.0 13⁄32 W 6.0 1⁄ 4

J 13.0 1⁄2 X 3.0 1⁄ 8


specified or known mass by means of a clamp and mass carrier
K 8.0 1⁄16 Y 3.0 7⁄64 to the layer of which the adhesion is being determined. Include
L 16.0 3⁄8 Z 8.0 5⁄16
the mass of the clamp and carrier in the total mass causing
M 50.0 11⁄8 AA 6.0 7⁄32

AB 75.0 3
separation. Release the mass slowly without jerking and in
such a manner that the separating layer is stripped from the
FIG. 1 Clamp for Adhesion Test specimen at an angle of approximately 180°.

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D413 − 98 (2013)

FIG. 2 Mandrels and Frame for Static Mass Adhesion Test

7.2 Strip Specimen: Type B, 90° Peel—Test specimens in the 8.2 Testing Machine:
same manner as Type A, with the exception that the unpeeled 8.2.1 The testing machine shall be capable of being operated
portion of the specimen is kept in a horizontal position using a without any device for maintaining maximum load indication.
plate, if necessary, to ensure a 90° peel. For pendulum-type machines, do not engage pawls that prevent
7.3 Ring Specimens—Place the ring specimen snugly on a the mass lever from swinging freely.
mandrel that has an outside diameter substantially the same as 8.2.2 The machine shall be equipped with the chart where
the internal diameter of the ring. Separate the parts to be tested the distance separated is one axis and the applied force is the
sufficiently by hand to permit the jaws of the testing clamp to other axis of coordinates. The preferred chart speed is the same
be attached. With the mandrel resting on the supporting frame, as the cross-head speed for ring specimens and one half the
apply a known or specified mass by means of the clamp and a cross-head speed for strip specimens.
mass carrier to the layer of which the adhesion is being tested. 8.2.3 The force applied shall be greater than 15 % and less
Include the mass of the clamp and carrier in the total mass than 85 % of the capacity of the machine.
causing separation. Release the mass slowly without jerking 8.2.4 Grips—Strip specimens shall be held in the testing
and in such a manner that the separating layer is stripped from machine by grips that clamp firmly and prevent slipping at all
the specimen at an angle of approximately 90°. times during the test. For ring specimens, replace the grip
attached to the recording head of the machine with a freely
7.4 Rate of Separation—Record the time needed to com- rotating mandrel with an outside diameter substantially the
plete the separation using a stop watch or a watch having a same as the inside diameter of the ring specimen. Mount the
second hand. Remove the mass and measure the length mandrel so that its axis of rotation is in the plane of the ply
stripped between marks placed at the beginning and end of the being separated and the applied force is normal to the tangent
test on the portion other than that stripped. of the ring circumference at the line of separation.
8.2.5 The preferred rate of travel of the power-actuated grip
MACHINE METHOD is 0.8 mm/s (2 in./min) for strip specimen Type A, 2.5 mm/s (6
in./min) for Type B, and 0.4 mm/s (1 in./min) for ring
8. Apparatus specimens. These rates are to be uniform throughout the tests.
8.1 A tension testing machine, power-driven, accurate to
9. Test Specimens
within 61 % is used for measuring the force required to
separate the layers of the test specimen. A constant rate of 9.1 Prepare the specimens in accordance with Section 6.
extension testing machine satisfies this condition and is pre-
ferred although an inclination-balance, pendulum-type, or a 10. Procedure
spring-balance apparatus may be used. Requirements of the 10.1 Strip Specimens: Type A, 180° Peel—Measure the
testing machine are in 8.2.1 to 8.2.5. width of the cut strip to the nearest 0.2 mm (0.01 in.) and

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D413 − 98 (2013)
record. Separate the parts to be tested by hand at one end of the 11.2 Effect of Temperature—The results of this test are
test specimen and at a sufficient distance to permit grips of the affected by temperature. Elevating the temperature causes a
machine to be attached. Attach the separated end of the faster rate of stripping under a given load. The temperature
specimen, with all separate parts except the one under test during test shall therefore be 23 6 2°C (73.1 6 3.6°F) and the
securely gripped, to the recording head by means of a clamp, actual temperature shall be recorded.
using care to adjust it symmetrically in order that the tension
shall be distributed uniformly. Provide for maintaining the strip 12. Interpretation of Results
during the test approximately in the plane of the clamps. This 12.1 In the static-mass test method, no stripping is started
may be done either by attaching the minimum mass required to unless a certain mass is used. Small increments in mass do not
the free end of the specimen or by holding the specimen against progressively cause proportional increases in rate of separa-
a plate attached to the stationary clamp but, in either case, take tion. With increasing mass the rate increases slowly at first and
into account the added mass in determining the force causing finally very rapidly. Rate of separation must therefore be
separation. Grip that layer of the specimen of which the interpreted carefully. A specimen required to separate not more
adhesion is to be tested symmetrically and firmly without than 0.4 mm/s (1 in./min) under a force of 90 N (20 lbf) might
twisting in the power-actuated clamp. Adjust the autographic be regarded as very inferior if the test result was 2 mm/s (5
mechanism and chart to zero and start the machine. Strip the in./min). The same specimen might not strip at all under a force
separating layer from the specimen at an angle of approxi- of 67 N (15 lbf) and might meet the requirement with a force
mately 180°, and continue the separation for a sufficient of 80 N (18 lbf).
distance to indicate the adhesion value. 12.2 The true adhesion value is not determined in case the
10.2 Strip Specimen: Type B, 90° Peel—Separate by hand a specimens repeatedly tear. The test, however, indicates that the
sufficient distance along the separation line in the center of the strength of adhesion exceeds the strength of the material and
strip to permit the grips of the machine to be attached. Make that the adhesion value is not less than the result obtained. In
provision to keep the unpeeled portion of the test specimen in cases of tearing, the results should be so designated.
a horizontal position using a plate if necessary to ensure a 90° 12.3 Adhesion values may differ between different plies of
peel. Peel along the previously cut separation layer for 40 to the same article of plied construction and also at different
100 mm (11⁄2 to 4 in.). points along the same ply. The adhesion value of one ply to
10.3 Ring Specimens—Separate by hand a sufficient length another is taken as the average result of the test over a
of a layer of the specimen to be tested to permit the power- reasonable distance of separation. When possible, a distance of
actuated clamp of the machine to be attached. Place the separation of at least 100 mm (4 in.) shall be used.
specimen snugly on the test mandrel. With the mandrel 13. Calculation
attached to the recording head of the machine and the separated
layer gripped symmetrically and firmly without twisting in the 13.1 For the Static-Mass Test Method, report the adhesion
power-actuated clamp, adjust the autographic mechanism and value as separation rate per unit width under a stated force, as
chart to zero and start the machine. Strip the separating layer follows:
from the specimen at an angle of approximately 90° to the _mm/s for 25 2 mm width under_N force (1)
tangent of the specimen surface, and continue the separation
for a sufficient distance to indicate the adhesion value. During _in./s for 1 2 in. width under_lbf
the test, the mandrel shall rotate freely so as to maintain the If a width other than 25 mm (1 in.) was used, correct the
line of separation at all times approximately in the same separation by multiplying the rate by the ratio of actual width
position. to the desired width. Include both the rate and the actual width
PRECAUTIONS, INTERPRETATION, CALCULATION, in the report.
AND REPORT 13.2 For the machine test method, the autographic chart
constitutes the report, but the value of the adhesion is deter-
11. Precautions mined by drawing on the chart the best average line between
the maximum and minimum force values. The force so
11.1 Tearing: indicated, expressed in newtons per metre (or pounds-force per
11.1.1 If, during a test, the substrate rubber begins to tear inch) is divided by the width measured in 10.1 for separation at
instead of separating at the bonded interface, cut the material the rate used and is reported as the adhesion strength, as
being torn with a knife up to the surface of contact between the follows:
two parts and start the test again.
Adhesion Strength 5 N/m ~ lbf/in.! 5 force/actual width (2)
11.1.2 If one of the substrate rubbers repeatedly tears,
instead of separating from the other part at the bonded Show both the force and actual width in the report.
interface, a satisfactory result may be secured in the static-mass
method by reducing the amount of the mass used if this is 14. Report
permitted. In case of repeated tearing when using the machine 14.1 The report shall include the following:
test method, take as the result of the test the average load at 14.1.1 Results of the adhesion test expressed in accordance
which tearing of the substrate rubber occurs. with Sections 12 and 13,

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D413 − 98 (2013)
14.1.2 All observations and recorded data on which the 14.1.7 Dimensions of the test specimen.
results are based,
15. Precision and Bias
14.1.3 Date of manufacture or vulcanization of rubber, if
known, 15.1 Precision and bias do not exist for this method because
resources necessary for round-robin testing have not been
14.1.4 Date of test,
forthcoming.
14.1.5 Statement of the method used, (Strip Type A, Strip
Type B, or Ring; Static-Mass or Machine), 16. Keywords
14.1.6 Temperature of test room, and 16.1 adhesion; fabric; rubber

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