Designation: D429 − 14

Standard Test Methods for

Rubber Property—Adhesion to Rigid Substrates1
This standard is issued under the fixed designation D429; 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 2. Referenced Documents

1.1 These test methods cover procedures for testing the 2.1 ASTM Standards:2
static adhesional strength of rubber to rigid materials (in most B117 Practice for Operating Salt Spray (Fog) Apparatus
cases metals). D395 Test Methods for Rubber Property—Compression Set
Method A—Rubber Part Assembled Between Two Parallel D412 Test Methods for Vulcanized Rubber and Thermoplas-
Metal Plates. tic Elastomers—Tension
Method B—90° Stripping Test—Rubber Part Assembled to D471 Test Method for Rubber Property—Effect of Liquids
One Metal Plate. D572 Test Method for Rubber—Deterioration by Heat and
Oxygen
Method C—Measuring Adhesion of Rubber to Metal with a
D573 Test Method for Rubber—Deterioration in an Air
Conical Specimen.
Oven
Method D—Adhesion Test—Post-Vulcanization (PV) Bond- D1149 Test Methods for Rubber Deterioration—Cracking in
ing of Rubber to Metal. an Ozone Controlled Environment
Method E—90° Stripping Test—Rubber Tank Lining— E4 Practices for Force Verification of Testing Machines
Assembled to One Metal Plate. G153 Practice for Operating Enclosed Carbon Arc Light
Method F—Rubber Part Assembled Between Two Parallel Apparatus for Exposure of Nonmetallic Materials
Convex-Shaped Metal Plates 2.2 ASTM Adjuncts:
Method G—Measuring Bond Durability for Rubber-to-Metal Holding Fixture Drawings3
Bonded Components with a Double Shear Cylindrical Speci-
men 3. Significance and Use
Method H—Measuring Bond Durability for Rubber-to-Metal 3.1 These test methods are designed primarily for speci-
Bonded Components with a Quadruple Shear Specimen mens prepared in a laboratory under standardized conditions

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such as may be used to provide data for development and
1.2 While the test method may be used with a wide variety control of rubber compounds and methods of manufacture.
of rigid materials, use of materials other than metals is the With slight modifications as indicated, Methods A, B, C, D,
exception. For this reason, we have used the word “metal” in and E are also used for obtaining comparative adhesion test
the text rather than “rigid materials.” values of production parts whenever the design permits prepa-
1.3 The values stated in SI units are to be regarded as the ration of suitable test specimens. Methods A, B, C, and D are
standard. The values given in parentheses are for information applicable in the case of many products in which rubber is used
only. for controlling vibration.
1.4 This standard does not purport to address all of the METHOD A—RUBBER PART ASSEMBLED
safety concerns, if any, associated with its use. It is the BETWEEN
responsibility of the user of this standard to establish appro- TWO PARALLEL METAL PLATES
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. 4. Adhesion Failure Terminology
4.1 R indicates the failure is in the rubber.

1 2
These test methods are under the jurisdiction of ASTM Committee D11 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Rubberand are the direct responsibility of Subcommittee D11.25 on Rubber contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
Adhesive Systems. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved May 1, 2014. Published May 2014. Originally the ASTM website.
3
approved in 1935. Last previous edition approved in 2008 as D429 – 08. DOI: Complete detail drawings of the fixture are available from ASTM International
10.1520/D0429-14. Headquarters. Order Adjunct No. ADJD0429. Original adjunct produced in 1959.

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FIG. 1 An Example of an Adhesion Test Specimen Attached in a Testing Machine

4.2 RC indicates the failure is at the rubber-cover cement 6.2 Grips—The fixtures for holding the specimen in the
interface. testing machine will depend on the type of specimen, but in all
4.3 CP indicates the failure is at the cover cement-prime cases shall be provided with ball seats, or another device, to
cement interface. permit centering of the load during the test. A typical adhesion
test assembly is shown in Fig. 1. Specially molded laboratory
4.4 M (can also be denoted as CM) indicates the failure is at specimens shall be attached by means of threaded studs on the
the metal-prime cement interface. metal parts as shown in Fig. 2. Specimens cut from production
NOTE 1—Example—The percentages of the various types of failure parts may be clamped as illustrated in Fig. 3.
may be estimated as in the following examples:
R-50, RC-50 means that roughly one half or 50 % of the area showed 7. Standard Test Specimens
failure in the rubber and the other 50 % showed failure at the rubber cover
cement interface.
7.1 After assembly, the standard test specimen shall consist
R-25, RC-25, M-50 means three types of failure were present with the of a cylinder of cured rubber 3.2 6 0.1 mm (0.125 6 0.005 in.)
M indicating 50 % failure at the metal-primer interface. Determining the thick and with a diameter of 39.9 6 0.1 mm (1.597 6 0.005
locus of failure can normally be determined visually, but may require in.), which results in a surface area of 1250 6 5 mm2 (2.00 6
analytical test methods. 0.01 in.2). This will be attached to the faces of two metal plates,
each at least 9.5 mm (0.37 in.) in thickness and of the same
5. Significance and Use
diameter as the rubber cylinder. The metal plates shall have flat
5.1 Method A is used to determine adhesion values in faces that shall be parallel in the finished specimen. The
instances where users feel this design is more reflective of an cylindrical shape is used to eliminate sharp corners and to give
actual product and where control tests have been set up as a uniform distribution of the pulling force.
result. The sample also lends itself to testing the effectiveness
NOTE 2—While a 1250 mm2 (2 in.2) area test specimen shall be
of different processing techniques and various adhesive sys- considered the standard for reference purposes, it shall be permissible to
tems. use a specimen of only 625 mm2 (1 in.2) in area, when it is desirable to
prepare and cure a large number of test specimens at one time. The
6. Apparatus diameter of this test specimen shall be 28.21 6 0.02 mm (1.129 6 0.001
in.) and the unvulcanized piece shall be cut to dimensions of approxi-
6.1 Testing Machine—A tension testing machine conform- mately 24 mm (15⁄16 in.) in diameter and approximately 5 mm (3⁄16 in.) in
ing to the requirements of Practices E4 shall be used for thickness (approximately 10 % volume excess).
measuring the strength of adhesion. The moving head of the
machine shall travel at the uniform rate of 0.40 6 0.04 mm/s 8. Laboratory Preparation of Standard Test Specimens
(1.0 6 0.1 in./min). The machine shall be provided with a 8.1 Prepare the standard test specimen to be used for
recording device to give the total force in Newtons or pouds- development and control purposes in the laboratory as de-
force at the conclusion of the test. A machine with a capacity scribed in 8.2 through 8.6. Methods other than those specified
no greater than 44.5 kN (10 000 lbf) will be found suitable in in 8.2 to 8.6 may be applied and must be described in the test
most cases. report.
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FIG. 2 Views of a Typical Test Specimen Showing Individual Metal Parts and Rubber Cylinders

8.2 Machine circular metal parts of standard dimensions 9.2 In routine production testing, it is sometimes necessary
from rolled bar steel SAE No. 10204 for standard reference to test specimens of different size and shape than those
pieces. However, other metals may be used if in conformity specified as standard. In such cases, the test method of
with the essential dimensions. Prepare smoothly machined test preparation shall be similar to that given in 9.1, but the test
faces of the metals in accordance with any test method for results secured shall not be compared with those obtained using
securing adhesion that may be under investigation. the standard test specimen.
8.3 Cut unvulcanized rubber pieces to dimensions of ap- 10. Procedure
proximately 35 mm (1 3⁄8 in.) in diameter and approximately 5
mm (3⁄16 in.) in thickness so as to give maximum pressure of 10.1 Mount the vulcanized standard test specimen or the
the rubber against the metal surface during vulcanization (see specimen cut from a production part in the testing machine, as
Fig. 2). Clean or treat surfaces to be adhered in accordance shown in Fig. 1, so that the tension shall be uniformly
with the method being investigated. distributed. Test at a rate of 0.40 6 0.04 mm/s (1.0 6 0.1
in./min), or at 0.083 6 0.08 mm/s (2.0 6 0.2 in./min), until the
8.4 Assemble the metal parts and rubber pieces for vulca- rubber either separates from the metal surface or ruptures.
nization in the mold. A typical mold and test piece are shown Record the total force at the time of failure. Typically 3
in Fig. 4. The assembly is illustrated in Fig. 2. After specimens are tested per condition, but other sample sizes can
vulcanization, approximately 0.039 mm (0.0015 in.) of rubber be used, if reported.
should be over the edge of the metal substrate. Prior to
vulcanization, take great care to keep the surfaces to be 10.2 In case of rupture in the rubber, the strength of the
adhered clean and free of dust, moisture, or other foreign adhesion bond is obviously not measured, but is shown to be
material. Do not touch surfaces. greater than the strength of the rubber itself. Record the type or
types of failure, and express in accordance with the adhesion
8.5 Vulcanize by heating the mold for a definite time at a failure terminology described in Section 4. Estimate and record
controlled temperature in a hydraulic vulcanization press. the percentages of the various types of failures.
Choose the time and temperature of cure according to the
rubber compound used. Take care in removing the specimens 11. Calculation
from the mold to avoid subjecting the adhered surfaces to stress
11.1 Express the adhesion value in pascals or pounds-force
before the specimens have cooled.
per square inch. Calculate by dividing the tension force causing
8.6 After vulcanization, store the specimens at a tempera- failure by the original area of the adhered surface. In case of
ture of 23 6 2°C (73.4 6 3.6°F) at least 16 h prior to testing. rubber failure, the adhesion value is recognized as being higher
than that reported.
9. Test Specimens from Production Parts
9.1 For comparative test of adhesion in production parts, 12. Report
select a portion of the production-made part so that a specimen 12.1 The report shall include the following:
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consisting of a rubber piece sandwiched between two parallel 12.1.1 The result, calculated in accordance with Section 11,
plates of metal may be cut. Hollow-mill a specimen out of the 12.1.2 All observed and recorded data including the number
production part and finish the piece either by turning or of test pieces involved,
grinding down to size in such a manner that the surfaces of the 12.1.3 Notation of type or types of failure, and the estimated
rubber and metal shall be free of imperfections, which have a percentages of the various types of failures (Section 10),
tendency to start a tear in the rubber part during the application 12.1.4 A description of the specimen and a notation indicat-
of tension while testing. ing whether the specimen was molded in the laboratory or
prepared from a production part,
4
Supporting data have been filed at ASTM International Headquarters and may 12.1.5 Dimensions of the test specimen (comparisons may
be obtained by requesting Research Report RR:D11-1040. be made only among specimens of the same size and shape),

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D429 − 14
METHOD B—90° STRIPPING TEST—RUBBER
PART ASSEMBLED TO ONE METAL PLATE

14. Significance and Use

14.1 This test is intended to determine the adhesive strength
of rubber-to-metal bonding agents. The results are obtained by
measuring the force necessary to separate a rubber from a
metal surface. The data obtained indicates the strength of
adhesion along a line across the width of the rubber strip being
separated from a metal plate at a 90° angle. The test provides
valuable data for development and control of rubber com-
pounds and test methods of bonding. It also serves as a
screening test for the evaluation of various bonding agents,
techniques, or both.
NOTE 3—It is permissible to use a 45° angle to bring about separation,
but if this is done, the same should be indicated on the form on which the
data are recorded. If this notation does not appear, it must be assumed that
the 90° angle has been used. The angle of pull, in this case 45°, merely
means that the equipment has been so designed that the angle made by that
face of the rubber being stripped from the metal and the metal to which it
has been adhered is 45°. Experience indicates a lower force is obtained for
the 45° angle than for the 90° angle, and also a break significantly closer
to the bond interface.

15. Adhesion Failure Terminology

15.1 R indicates the failure is in the rubber.
15.2 RC indicates the failure is at the rubber-cover cement
interface.
15.3 CP indicates the failure is at the cover cement-prime
cement interface.
15.4 M (can also be denoted as CM) indicates the failure is
at the metal-prime cement interface.
NOTE 4—Example—The percentages of the various types of failure
may be estimated as in the following examples:
R-50, RC-50 means that roughly one half or 50 % of the area showed
failure in the rubber and the other 50 % showed failure at the rubber-cover
cement interface.
R-25, RC-25, M-50 means that three types of failure are present with
the M indicating 50 % failure at the metal-primer interface.

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16. Apparatus
FIG. 3 Method of Testing Adhesion When Sample Section is 16.1 Testing Machine—A power driven test machine
Taken from Production Parts equipped to produce a uniform rate of grip separation shall be
used for measuring the strength of adhesion. The head of the
12.1.6 Test method used for determining adhesion specified machine shall travel at the uniform rate of 0.83 6 0.08 mm/s
in this standard, including the test rate, (2 6 0.2 in./min).
12.1.7 Surface finish of substrate, if known,
16.2 Fixture—Any suitable fixture for holding the test
12.1.8 Date of manufacture or vulcanization, if known,
specimen to the upper head of the machine may be used
12.1.9 Time and temperature of vulcanization, if known,
provided the direction of pull to cause separation is as
12.1.10 Temperature and humidity of test room,
perpendicular as possible at all times during the test. This
12.1.11 Date of test, and
means making a 90° angle with the top holding fixture. The test
12.1.12 Any deviations from this test method.
fixture shown in operation in Fig. 5 complies with the above
13. Precision and Bias4 and provides the ease and simplicity of testing.3
13.1 Precision and bias do not exist for this test method 16.3 Grips—Any suitable grip may be used, provided it
because resources necessary for round-robin testing have not does not slip or rupture the rubber strip. The grip shown in Fig.
been forthcoming. 5 complies and provides ease and simplicity of operation.

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D429 − 14

in. mm
1⁄16 2
1⁄ 8 3
3⁄16 5
3⁄ 8 10
1⁄ 2 13
5⁄ 8 16
3⁄ 4 19

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1 1⁄ 2 38
2 1⁄ 8 54
2 1⁄ 4 57
2 7⁄ 8 73
3 76
6 1⁄ 2 165
8 203
0.375 ± 0.002 9.53 ± 0.05
0.125 ± 0.005 3.2 ± 0.1
1.597 ± 0.001 15.16 ± 0.03
1.600 ± 0.001 40.64 ± 0.03

FIG. 4 Detailed Drawing of a Mold for Adhesion Test Pieces

17. Standard Test Specimen adhesion that may be under investigation. Mask both ends with
17.1 The standard test specimen shall consist of a strip of pressure-sensitive tape so that only the area described in
rubber 6.3 6 0.1 mm (0.250 6 0.005 in.) in thickness, 25 6 Section 17 will be available for adhesion.
0.5 mm (1.000 6 0.02 in.) in width, and 125 mm (5 in.) in 18.1.2 Cut unvulcanized rubber slabs approximately 8 mm
length adhered to the face of a metal strip 1.6 6 0.1 mm (0.062 (0.3 in.) in thickness to dimensions of the required size for the
6 0.004 in.) in thickness, 25 6 0.5 mm (1.000 6 0.02 in.) in mold, so as to provide maximum pressure of the rubber against
width, and 60 6 1 mm (2.36 6 0.04 in.) in length. The test the metal surfaces during vulcanization. (See Fig. 6 for suitable
specimen shall be so prepared that the bonded area of 25 by 25 mold design.) The inside mold dimensions parallel to the
mm (1 by 1 in.) is fixed approximately in the middle of the longitudinal axis of the metal part shall be 125 mm for nominal
metal member as shown in Fig. 6. 5 in. The dimension along the transverse axis of the metal part
can be altered according to the number of pieces required for
NOTE 5—In cases where the 1.6-mm (0.062-in.) thick metal is perma-
nently deformed during testing, a thicker metal may be used when agreed
any one cure. This will leave sufficient length of rubber strip
upon between the purchaser and the supplier. for fastening in the grip shown in Fig. 5. Solvent-wash rubber
surface to be adhered or treat in accordance with the method
18. Preparation of Standard Test Specimen being investigated. Freshly milled rubber need not be solvent
18.1 Prepare the standard test specimen as described in wiped.
18.1.1 to 18.1.6: 18.1.3 Assemble the metal parts and rubber pieces for
18.1.1 Rectangular metal parts of the standard dimensions vulcanization as shown in Fig. 6, properly spacing the metal
described in Section 17 shall have the area to be bonded parts along one edge of the rubber slab and then placing the
prepared in accordance with the test method for determining assembly, metal parts down, in the mold cavity. Cure the whole

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NOTE 7—This specimen lends itself to the determination of the relative
effect of environmental conditions on possible bond deterioration. Speci-
mens may be exposed unstressed or under a constant, relatively low bond
stress. It is recommended that one of the standard ASTM environmental
exposure conditions be used. Among those applicable are the following:
Test Methods D471, D572, D573, D1149, Practice G153, and Practice
B117. If environments other than the above are used, they shall be
described completely. This should include the conditions of the exposure
such as time, temperature, etc.

20. Calculations
20.1 Express the adhesion value in newtons per millimetre
or pounds-force per inch of width.

21. Report
21.1 The report shall include the following, preferably
reported on an Adhesion Test Data Sheet illustrated in Table 1:
21.1.1 The results calculated in accordance with Section 20.
21.1.2 All observed and recorded data,
21.1.3 Notation of the type or types of failures and the
estimated percentages of the various types of failures (Section
15),
21.1.4 Description of the specimen including statement of
FIG. 5 Adhesion Tensile Testing Fixture in Operation
method of determining adhesion, if known,
21.1.5 Date of vulcanization, if known,
assembly in accordance with the method being investigated. 21.1.6 Time and temperature of vulcanization, if known,
Prior to assembly and vulcanization, take great care to keep the 21.1.7 Temperature of test room, and
surfaces to be adhered clean and free of dust, moisture, or other 21.1.8 Date of test.
foreign material.
18.1.4 Vulcanize by heating the mold under pressure for a 22. Precision and Bias4
definite time at a controlled temperature in a hydraulic vulca- 22.1 Precision and bias do not exist for this test method
nizing press. The time and temperature of cure shall be in because resources necessary for round-robin testing have not
accordance with the system being investigated. At the conclu- been forthcoming.
sion of the cure, take care in removing the specimens from the
mold to avoid subjecting the adhered surfaces to stress before METHOD C—MEASURING ADHESION OF
the specimens have cooled. RUBBER-TO-METAL WITH A CONICAL
18.1.5 After vulcanization, store the specimens at a tem- SPECIMEN
perature of 23 6 2°C (73.4 6 3.6°F) for at least 16 h.
23. Significance and Use
18.1.6 Separate the specimens from each other in prepara-
tion for testing. This is done by cutting with a scissors, 23.1 The test method is designed primarily to test pieces
handknife, or other suitable equipment. The edges of the prepared in the laboratory under standard conditions to provide
specimen may then be buffed on a belt sander to bring the edge data for development and control of bonding systems and their
of the rubber flush with the edge of the metal strips (Note 6). components, such as cements or special rubber compounds,
Take care not to overheat the metal parts or the rubber and not and of test methods of manufacture. While intended to be
to reduce the width of the sample being tested beyond the applied where rubber is bonded to supporting rigid pieces, it
tolerances described. may not cover such cases where the support, a high modulus
material, has low rigidity due to small transverse dimensions,
NOTE 6—Present experience indicates negligible differences in results
between samples buffed clean and samples tested without buffing, because
as in the case of rubber bonded to metal wires, cords, or thin
edges of metal parts are not specifically prepared for adhesion and the sheets. The particular geometry of the test piece produces, in
edge contact area, given a metal part thickness of 1.6 mm (0.062 in.) is not most cases, an interfacial failure between the rubber and
significant. conical part, because of a stress concentration at the tip of the
cone.
19. Procedure
19.1 Place the test specimen (Note 7) symmetrically in the 24. Adhesion Failure Terminology
jaws attached to the fixed grip with the separating edge toward 24.1 Express the type of adhesion failure as determined by
the operator, as shown in Fig. 5. Place the tab in the grip and examination of broken test pieces by one or more of the
apply a steady load at the rate of 50 mm (2.0 in.)/min until following symbols:
separation is complete. Use the autographic recorder in order to
show graphically the adhesion values over the full length of the 24.2 R indicates failure in the rubber.
test specimen. --```,```,,,`,,,```,,,``,`,,,`-`-`,,`,,`,`,,`---
24.3 RC indicates failure in the rubber-cover cement.

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Section A-A
in. 0.06 0.12 0.31 1 1.5 2.38 5 6 7 8
mm 1.5 3 7.9 25 38 60.5 127 152 178 203

FIG. 6 Adhesion Test Specimen Mold

TABLE 1 Example of Form for Reporting Adhesion test Results

Pull Type of Break, %
Metal and Metal
Stock Cure Sample, Average,
Finishing Used R RC CP M
lbf/in. lbf/in.

Date___________ By________________________

24.4 CP indicates failure in the cover cement-prime cement. 25.2 Grips—The fixtures for holding the specimen in the
24.5 M (can also be denoted as CM) indicates failure in the test machine will depend on the type of specimen but in all
prime cement-metal interface. cases shall be provided with ball seats to permit proper
centering of the applied load during the test. These grips can be
NOTE 8—Example—The percentages of the various types of failure of two types: (1) a simple slip-in type which engages in the
may be estimated as in the following examples:
grooved section of the conical specimen, or (2) a threaded stud
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R-50, RC-50 means that roughly one half or 50 % of the area showed
failure in the rubber and the other 50 % showed failure at the rubber-cover with a locknut. This could be a combination fixture.
cement interface.
R-25, RC-25, M-50 means three types of failure present with the M 26. Standard Test Specimen
indicating 50 % failure at the metal primer interface. 26.1 A standard test specimen shall consist of a rubber
compound bonded to two conical metal end pieces. The
25. Apparatus diameter of the test specimen shall be 25 6 0.5 mm (1.00 6
25.1 Testing Machine—A tension testing machine conform- 0.2 in.). The distance between the opposed conical end pieces
ing to the requirements of Practices E4 shall be used for shall be 11.5 6 1.2 mm (0.45 6 0.05 in.). For the test specimen
measuring the strength of adhesion. The moving head of the in Fig. 7, the height of each conical end piece shall be 23.4 6
machine shall travel at the uniform rate of 0.83 6 0.08 mm/s 0.5 mm (0.92 6 0.02 in.) (Note 9). The half-angle of the cone
(2.06 0.2 in./min). The machine shall be provided with a vertex shall be 45 6 1° and the tip shall not be rounded to
recording device to give the total force in newtons or pounds- radius greater than 0.8 mm (0.03 in.).
force at the conclusion of the test. A machine with a capacity NOTE 9—Theoretically, the height of end pieces could be any length.
no greater than 44.5 kN (10 000 lbf) will be found suitable in The end pieces in Fig. 7 have been the most practical size for molding and
most cases. testing.

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28. Procedure
28.1 Mount the test specimens in the grips of the test
machine using the appropriate fixtures. Take care in centering
and adjusting the test specimen so the tension is symmetrically
distributed in the cross section during the test. Apply the
tension load until the rubber either separates from the adhesive
surface or ruptures. Record the total load at the time of failure.
Record type or types of failure and express in accordance with
the standard adhesion failure terminology (see Section 24).

mm in. 29. Calculations

A 25.0 ± 0.5 1.00 ± 0.02
BA 23.5 ± 0.5 0.92 ± 0.02 29.1 Express the adhesion value in Newtons or pounds-
C 11.5 ± 1.2 0.45 ± 0.05 force required to produce failure. In cases where the failure is
D 45°± 1 in the rubber, the adhesion value is recognized as being higher
E (radius) 0.8 max 0.03 max
than that recorded.
A
Suggested dimension.
30. Report
FIG. 7 Test Specimens with Conical Adhesion Areas 30.1 The report shall include the following, preferably
reported on an Adhesion Test Data Sheet illustrated in Table 1:
27. Laboratory Preparation of Standard Test Specimens 30.1.1 Type and code number of the rubber compound,
27.1 The standard test specimen is formed by two cylindri- 30.1.2 Cure time and temperature,
cal rigid parts terminated by opposite conical ends, and a 30.1.3 Type of metal or rigid substrate used and surface
cylinder of rubber bonded to the conical ends. Prepare in the preparation,
laboratory in accordance with 27.1.1 through 27.1.7. 30.1.4 Adhesive and dilution,
27.1.1 Machine conical metal parts from rolled bar steel 30.1.5 The adhesion value for each test piece,
SAE No. 10204 or SAE No. 1010 for standard reference pieces. 30.1.6 Type and percentage of failure,
However, other rigid materials may be used if in conformity 30.1.7 Date of vulcanization and date of test, and
with the essential dimensions to determine the effect of 30.1.8 Temperature of test room.
adhesion on other rigid materials. Prepare the test face of the 31. Precision and Bias
cone in accordance with any test method for securing adhesion
that may be under investigation. 31.1 Precision and bias do not exist for this test method
27.1.2 Vulcanize the specimens in a transfer mold. For the because resources necessary for round-robin testing have not
six-cavity transfer mold shown in Fig. 8, the unvulcanized been forthcoming.
rubber piece shall be approximately 20 mm (0.8 in.) in
32. Salvaging of Bonded Metal Parts
thickness and approximately 110 mm (4.3 in.) in diameter.
Sufficient rubber stock should be used to fill the pot and 32.1 Bonded metal parts may be salvaged by the usual
provide some excess after filling the mold cavities. burning or chemical stripping techniques. Mechanical or
27.1.3 Clean or treat the surface of the conical ends in chemical surface treatments are used to re-establish a clean
accordance with the adhesion system under investigation. Coat bonding surface. The sharpness of the conical tip may be
the treated metal surface with the adhesive over the conical reduced during salvaging. This affects reproducibility of the
area only. test results and care must be taken to re-establish the sharpness
27.1.4 Place the rigid parts and the rubber compound in the of this cone to 0.8-mm (0.03-in.) radius (maximum).
preheated mold for vulcanization.
METHOD D—ADHESION TEST: POST-
27.1.5 Vulcanize with conditions of time, temperature, and
VULCANIZATION
pressure being regulated by their interrelationship effect on
(PV) BONDING OF RUBBER TO METAL
adhesion to be determined. It may be necessary to surround the
mold with an insulating shield to maintain proper temperature 33. Significance and Use
during cure.
27.1.5.1 At the conclusion of the cure, take great care when 33.1 Methods A, B, and C of this standard cover procedures
removing the test specimens from the mold to avoid subjecting for testing the strength of adhesion of rubber to metal when the
the bonded surfaces to undue stress before the test specimens bond is formed during vulcanization. Method D may be used to
have cooled. determine the strength of adhesion of rubber to metal when the
27.1.6 After vulcanization, store the specimens at a tem- bond is formed after the rubber has been vulcanized. In the
perature of 23 6 2°C (73.4 6 3.6°F) for at least 16 h prior to rubber industry, this is commonly referred to as post-
testing. vulcanization (PV) bonding.
27.1.7 Fig. 8 shows a mold, unvulcanized rubber 33.2 In the test, a vulcanized circular disk that has been
compound, molded test specimens, and adhesive coated coni- adhesive coated on both ends, is assembled between two
cal pieces. parallel metal parts. The rubber-metal assembly is then placed
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FIG. 8 Mold and Conical Test Specimens

in a fixture under compression and heated in an oven for a 35. Standard Test Specimens
specified time at a specified temperature.
35.1 Prepare the vulcanized rubber test specimen in accor-
33.3 When tested to rupture in an axial direction, a mea- dance with the procedure given in Test Methods D395.
surement of rubber-to-metal adhesion is obtained. The rupture
force and type of failure are recorded. 35.2 The metal test specimen is identical to the standard
metal test specimen described in Section 6, Method A, of this
34. Apparatus standard.
34.1 Testing Machine, A tension testing machine conform- 36. Preparation of Standard Test Specimens
ing to the requirements of Practices E4 shall be used for
measuring the strength of adhesion. The crosshead of the 36.1 Soak lint-free paper towel in methyl ethyl ketone
machine shall travel at the uniform rate of 0.83 6 0.08 mm/s (MEK), or another suitable cleaning solvent, and lay flat on a
(2.0 6 0.2 in.)/min. The machine shall be provided with a clean surface. Wipe the rubber surfaces to be bonded several
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device to record the maximum force in Newtons or pounds- times across the paper to remove any residual surface contami-
force at the conclusion of the test. A machine of at least nants. Following air-drying for at least 15 min, post-dry the
44.5-kN (10 000-lbf) capacity is suitable. cleaned rubber specimens for 10 min at 70°C in a circulating
34.2 Grips—The fixtures for holding the specimen in the air oven. Remove the rubber specimens from the oven and
testing machine will depend on the type of specimen but in all allow to condition at Standard Laboratory Temperature (23 6
cases shall be provided with ball seats, or a suitable 2°C) for at least 30 min prior to adhesive coating, preferably by
mechanism, to permit proper centering of the load during the brush application.
test. These grips can be of the type described in 6.2 of Method 36.2 Dip each surface of the adhesive-coated specimen
A and are illustrated in Fig. 1 and Fig. 3. alternately into a suitable assembly oil5 to a depth slightly
34.3 Details of the apparatus used to hold and compress the greater than the surface to be covered. Place the specimen on
rubber metal bonded assembly during oven cure are shown in its side and allow excess oil to drain off for about 5 min prior
Fig. 9 (outside plates) and Fig. 10 (center aligning plate). The to assembly.
center aligning plate, which controls compression of the
bonded assembly to 10.0 6 0.1 %, is held to the outside plates
by means of two bolts, washers, and nuts. The bolts are 5
Rubber assembly oil—Ex. Seagul Type R, Clark Oil and Chemical Co.,
tightened until the metal pieces compress the rubber properly. Cleveland, OH.

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in. mm
⁄
12 12.7
33/64 13.10
41/64 16.27
0.875 22.23
1.250 31.75
1.625 41.28
2.250 57.15
2.500 63.50
3.250 82.55
4.50 114.30
5.00 127.0

FIG. 9 Outside Plates (Two Required) Low-Carbon Steel

36.3 Assemble the test unit in accordance with Fig. 11. until destruction of the bonded assembly is complete. Record
Required compression is automatically obtained by the spacer the type of failure, expressed in accordance with the adhesion
as the unit is tightened. failure terminology described in Section 4 under Method A of
36.4 Place the test unit in a circulating air oven at 150°C for this standard.
a period of 60 6 10 min, or at a time and temperature
recommended by the adhesive supplier. Remove the unit and 38. Calculations
immediately cool in room temperature tap water for at least 20 38.1 Express the adhesion value in pascals (or kPa, MPa) or
min. Following cooling, disassemble the test unit and store the
pounds-force per square inch and calculate by dividing the
individual test specimens at a temperature of 23 6 2°C at least
tension force by the original area of the adhered surface. In the
48 h prior to testing.
case of rupture of the rubber, the adhesion value is recognized
37. Procedure as being higher than the rupture strength that is calculated as
37.1 Attach the bonded assembly to the tension testing described above.
machine using the appropriate fixtures or grips. Apply a force

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in. mm
0.150 3.81
0.45 11.40
41/64 16.27
0.875 22.23
1 1⁄ 4 31.75
1.250 31.75
1.50 38.10
1.625 41.28
2.500 63.50
2.700 68.58
3.00 76.20
5.00 127.00

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FIG. 10 Center Aligning Plate (One Required) Low-Carbon Steel

PARTS LIST
No.
No. Description Req’d
1 5⁄8-16 UNC 3-in. long hex bolt 2
2 Fig. 9 – outside plate 2
3 Metal test specimen 12
4 Vulcanized rubber puck 6
5 Fig. 10 – center aligning plate 1
6 Washer 2
7 5⁄8-16 UNC nut 2

FIG. 11 Total Assembly

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39. Report
39.1 The report shall include the following, preferably
reported on an Adhesion Test Data Sheet illustrated in Table 1:
39.1.1 Type and code number of the rubber compound,
39.1.2 Bonded assembly preparation; cure time and
temperature,
39.1.3 Type of metal and surface preparation,
39.1.4 Adhesive and dilution,
39.1.5 Method of application,
39.1.6 Failure or rupture stress measured in pascals or
pounds-force per square inch,
39.1.7 Type of failure, and
39.1.8 Date of test.

40. Precision and Bias4

40.1 Precision and bias do not exist for this test method
because resources necessary for round-robin testing have not
been forthcoming.
METHOD E—90° STRIPPING TEST—RUBBER TANK
LINING—ASSEMBLED TO ONE METAL PLATE

41. Significance and Use

41.1 This test is intended to determine the adhesive strength
of rubber tank lining to tank wall. The results are obtained by
measuring the pull necessary to separate a rubber strip from a
metal surface. The data obtained indicate the strength of
adhesion along a line across the width of the rubber strip being
separated from a plate at a 90° angle. The test provides
valuable data for development and control of rubber com-
pounds and methods of bonding. It also serves as a screening FIG. 12 Test Apparatus For Static Mass Adhesion Test on Rub-
test for the evaluation of various bonding agents, techniques, or ber Tank Lining
both.

42. Adhesion Failure Terminology 43.1.3 A photograph of a suitable support frame, together
with test specimen, clamp, mass carrier, and calibrated masses,
42.1 R indicates the failure is in the rubber. is shown in Fig. 12.
42.2 RC indicates the failure is at the rubber-cover cement
interface. 44. Standard Test Specimen
42.3 CP indicates the failure is at the cover cement-prime 44.1 A standard test specimen is shown in Fig. 13 and the 25
cement interface. 6 0.05-mm (1.000 6 0.002-in.) wide strip of rubber is fixed
approximately in the center of the metal plate. Overall size of
42.4 M (can also be denoted as CM) indicates the failure is the prepared test specimen from which the 25 mm wide strip is
at the metal-prime cement interface. taken is 150 6 3 mm (6.000 6 0.15 in.) square. One end of the
NOTE 10—Example—The percentages of the various types of failure cemented plate is to be masked with approximately 25 mm (1
may be estimated as in the following examples: in.) wide pressure-sensitive tape.
R-50, RC-50 means that roughly one half or 50 % of the area showed
failure in the rubber and the other 50 % showed failure at the rub- 45. Laboratory Preparation of Standard Test Pieces
ber – cover cement interface.
R-25, RC-25, M-50 means that three types of failure are present with 45.1 The standard test specimens shall be as described in
the M indicating 50 % failure at the metal – primer interface. 45.1.1 to 45.1.4.
45.1.1 Prepare contact area of hot-rolled, mild black steel in
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43. Static-Mass Method (SM) accordance with the method for securing adhesion that is
43.1 Apparatus: specified by supplier, or that may be under investigation. Size
43.1.1 The apparatus required for the adhesion test by the of metal plate is approximately 150 mm2 (6 in.2) and at least
static-mass test method consists of a supporting frame, testing 3.4 mm (0.13 in.) in thickness. Mask one end with approxi-
clamps, calibrated masses, and a mass carrier. mately 25 mm (1.0 in.) wide pressure-sensitive tape.
43.1.2 The frame has sufficient height to permit the mass NOTE 11—In cases where the 3.18-mm (0.135-in.) thick metal is
carrier to be suspended from the clamp holding the test permanently deformed during testing, a thicker metal plate may be used.
specimen and to hang freely during the progress of the test. Likewise, a different grade of steel may be specified when agreed upon

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FIG. 13 Adhesion Test Specimen for Rubber Tank Lining

FIG. 14 An Example of a Rubber Tank Lining Adhesion Specimen in a Testing Machine

between the purchaser and the supplier. 45.1.4 After vulcanization, store the specimens at a tem-
45.1.2 Apply unvulcanized rubber slabs, 6.3 6 0.5 mm perature of 23 6 2°C (73.4 6 3.6°F) at least 16 h. Cut a 25-mm
(0.25 6 0.02 in.) thick to the prepared surface of the metal wide strip as shown in Fig. 9.
plate.
46. Procedure
NOTE 12—Other thickness of rubber may be used to correspond to
actual ordered gage of tank lining stock if so noted on test report. 46.1 Separate the part to be tested by hand at the masked
45.1.3 Vulcanize the rubber in the same manner as recom- area end and at a sufficient distance to permit jaws of the
mended by the rubber tank lining manufacturer; that is, cured testing clamp to be attached. Mount the plate on a support
by exhaust steam, steam pressure, or chemical cure at the frame, attach a clamp to the test specimen at separated end.
recommended time, temperature, and procedure. Suspend a mass carrier to the clamp and apply known masses
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to the carrier until the mass causes a constant rate of travel of 51.2 Effect of Temperature—The results of this test are
0.4 mm/s (1 in./min) throughout the test. affected by temperature. Elevating the temperature causes a
faster rate of stripping under a given load. The temperature
47. Machine Method (M) during test shall therefore be 23 6 2°C (73.1 6 3.6°F) and the
47.1 Apparatus: actual temperature shall be recorded.
47.1.1 Testing Machine—Paragraph 6.1 of Test Methods 52. Calculations
D412 describes the testing machine that shall be used for
measuring the strength of adhesion. The head of the machine 52.1 For the static-mass test method, report the adhesion
shall travel at the uniform rate of 50 mm (2.0 in.)/min. valve as separation rate per unit width under a stated force, as
47.1.2 Fixture—Any suitable fixture for holding the test follows:
specimen to the upper head of the machine may be used ___ mm/s. for 25-mm width under___N force
provided the direction of pull to cause separation shall be as ___in./s for 1-in. width under___lbf
nearly perpendicular as possible at all times during the test, that If a width other than 25 mm (1 in.) was used, correct the
is, making a 90° angle with the top holding fixture. The test separation by multiplying the rate by the quotient of actual
fixture shown in operation in Fig. 5 complies with the above width per desired width as follows:
and provides ease and simplicity of testing. or ___mm/25 mm

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47.1.3 Grips—Any suitable grip may be used, provided it ___in./1 in.
does not slip or rupture the rubber strip. The grip shown in Fig. Include both the rate and the actual width in the report.
5 complies and provides ease and simplicity of operation. For the machine test method, the autographic chart consti-
tutes the report, but the value of the adhesion is determined by
48. Standard Test Specimen drawing on the chart the best average line between the
maximum and minimum force values. The force so indicated,
48.1 Refer to 44.1 (same as used for static-mass test expressed in Newtons per metre (or pounds-force per inch) is
method). divided by the width measured in 10.1 for separation at the rate
used and is reported as the adhesion value, as follows:
49. Laboratory Preparation of Standard Test Pieces
N/m ~ lbf/in.! 5 force/actual width (1)
49.1 Refer to 45.1 through 45.1.4. (Same as used for
static-mass test method). Show both the force and actual width in the report.

53. Interpretation of Results

50. Procedure
53.1 In the static-mass test method, no stripping is started
50.1 Place the test specimen (Note 13) symmetrically in the
unless a certain mass is used. Small increments in mass do not
jaws attached to the fixed grip with the separating edge toward
progressively cause proportional increases in rate of separa-
the operator, as shown in Fig. 5. Place the tab in the grip and
tion. The rate initially increases slowly, but increases rapidly as
apply a steady load at the rate of 50 mm (2.0 in.)/min until
the mass increases. Rate of separation must therefore be
separation is complete. Use the autographic recorder to show
interpreted carefully. A specimen required to separate not more
graphically the adhesion values over the full length of the test
than 0.4 mm/s (1 in./min) under a force of 90 N (20 lbf) might
specimen.
be regarded as very inferior if the test result was 2 mm/s (5
NOTE 13—This specimen lends itself to the determination of the relative in./min). The same specimen might not strip at all under a force
effect of environmental conditions on possible bond deterioration. Speci- of 67 N (15 lbf) and might meet the requirement with a force
mens may be exposed unstressed or under a constant, relatively low bond
stress. It is recommended that one of the standard ASTM environmental
of 80 N (18 lbf).
exposure conditions be used. Among those applicable are the following: 53.2 The true adhesion value is not determined in the case
Test Methods D471, D572, D573, D1149, Practice G153, and Practice where the specimens repeatedly tear. The test, however, indi-
B117. If environments other than the above are used, they shall be
described completely. This should include the conditions of the exposure cates that the strength of adhesion exceeds the strength of the
such as time, temperature, etc. material, and that the adhesion value is not less than the result
obtained. In cases of tearing, the results should be so desig-
51. Precautions nated.
51.1 Tearing: 53.3 Adhesion values may differ between different plies of
51.1.1 If, during a test, one of the parts begins to tear instead the same article of plied construction and also at different
of separating from the other part of the specimen, cut the points along the same ply. The adhesion value of one ply to
material being torn with a knife up to the surface of contact another is taken as the average result of the test over a
between the two parts and start the test again. reasonable distance of separation. When possible, a distance of
51.1.2 If one of the parts repeatedly tears, instead of separation of at least 100 mm (4 in.) shall be used.
separating it from the other part, a satisfactory result may be
secured in the static-mass test method by reducing the amount 54. Report
of the mass used if this is permitted. In case of repeated tearing 54.1 The report shall include the following:
when using the machine test method, take as the result of the 54.1.1 Results of the adhesion test expressed in accordance
test the average load at which tearing occurs. with Sections 53 and 52,

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FIG. 15 Test Specimen

54.1.2 All observations and recorded data on which the instances, interfacial failure(s) and thus is a discriminatory
results are based, screening test for the agents.
54.1.3 Date of manufacture or vulcanization of rubber, if
known, 57. Adhesion Failure Terminology
54.1.4 Date of test, 57.1 Express the type of adhesion failure as determined by
54.1.5 Statement of the test method used (static-mass or examination of broken test pieces by one or more of the
machine), following symbols:
54.1.6 Temperature of test room, and
54.1.7 Dimensions of the test specimen. 57.2 R Indicates failure in the rubber (substrate failure).
57.3 RC indicates failure in the rubber-cover cement (inter-
55. Precision and Bias4 facial failure).
55.1 Precision and bias do not exist for this test method 57.4 CP indicates failure in the cover cement-prime cement
because resources necessary for round-robin testing have not (interfacial failure).
been forthcoming.
57.5 M or CM indicates failure in the prime cement-metal
interface (interfacial failure).
METHOD F—RUBBER PART ASSEMBLED NOTE 14—Example–The percentage of the various types of failure may
BETWEEN TWO PARALLEL CONVEX–SHAPED be estimated as in the following examples:
METAL PLATES R-60, RC40 means that 60 % of the bonded area showed failure in the
rubber and the other 40 % showed failure at the rubber-cover cement
56. Significance and Use interface.
R-25, RC-25, M-50 means that three types of failure are present with
56.1 Method F is used for determining the adhesive strength R indicating 25 % failure in the rubber, RC, 25 % failure between the
of rubber-to-metal bonding agents. The adhesion values are rubber and the cement(adhesive)interface, and 50 % failure at the metal-
obtained by measuring the force in an axial direction that is primer interface, 25 % in the rubber.
necessary to separate the bonded rubber from the metal
component. The metal component is composed of two parallel 58. Apparatus
metal test specimens that have a convex shape on the bonded 58.1 Testing Machine—A testing machine as described in
side. (Fig. 15). This particular geometry produces in many 6.1 of Test Methods D412 shall be used for measuring the
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FIG. 16 Test Mold and Test Specimens

strength of adhesion. The head of the machine shall travel at 60.1.2 Prepare the test face of the specified convex speci-
the uniform rate of 0.83 6 0.08 mm/s (2 6 0.2 in./min). The men in accordance with any test method for securing adhesion
machine shall be provided with a recording device to give the that may be under investigation (for example, phosphated
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force in newtons or pounds-force at the conclusion of the test. treated, mechanical blasted, etc.).
58.2 Fixture—The fixtures for holding the specimen in the 60.1.3 Coat the prepared metal surface with the adhesive
test machine shall be threaded so the threaded studs of the test system to be tested in accordance to the manufacturers recom-
specimen can be screwed into the grip. Fixtures may be mendations.
provided with ball seats, or a similar mechanism, to permit 60.1.4 Place the dry adhesive coated specimens in the mold.
proper centering of the load during the test. For compression or transfer molding, place the rubber pre-
forms in the mold cavity. For injection molding, inject the
59. Standard Test Specimen rubber into the mold.
60.1.5 Vulcanize with conditions of time, temperature, and
59.1 A standard test specimen shall consist of a rubber
pressure in accordance with the system being investigated.
compound bonded to two convex-shaped metal end pieces. The
60.1.6 After a suitable vulcanization cycle, remove the
diameter of each test specimen shall be 28.70 6 0.76 mm. The
specimens with care to avoid subjecting the adhered surfaces to
distance between the pieces shall be 25.00 6 0.76 mm, the
stress before the specimens have cooled. Store the specimens at
radius 41.3 6 0.25 mm. (see Fig. 15).
a temperature of 23 6 2°C (73 6 4°F) for at least 16 h prior
60. Laboratory Preparation of Test Specimens to testing.
60.1 The standard test specimen is formed by vulcanizing 60.2 Fig. 16 shows a photograph of a mold and inserts.
the desired type of rubber in a mold containing the adhesive
coated metal test parts. Injection molding, transfer molding, or 61. Procedure
compression molding may be used. Prepare in the laboratory in 61.1 Mount the test specimens in the threaded grips of the
accordance with 60.1.1 – 60.1.6. test machine. Apply the tension load until the rubber either
60.1.1 Machine the metal test part from rolled bar steel SAE separates from the adhesive surface or the rubber ruptures.
No. 1020 or SAE No. 1010 for standard reference pieces. Other Record the total load at the time of failure. Observe the record
rigid materials may be used if in conformity with the essential the type or types of failure and express in accordance with the
dimensions. standard adhesion failure terminology (see Section 57).

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66. Adhesion Failure Terminology
66.1 Express the type of adhesion failure as determined by
the visual examination of the of the failed area using one or
more of the following symbols:
66.2 R indicates failure in the rubber.
66.3 RC indicates failure in between the rubber and the
adhesive.
66.4 CP indicates failure between the adhesive top coat and
the primer in the case of a two coat system.
66.5 M (or CM) indicates failure between the primer (or
FIG. 17 Double Shear Test Piece adhesive in the case of a one coat system) and the substrate, for
example, metal.
NOTE 15—Example–The percentage of the various types of failure may
62. Calculation be estimated as in the following examples:
R-60, RC -40 means that 60 % of the bonded area showed failure in the
62.1 Express the adhesion value in newtons (N) or pounds- rubber and the other 40 % showed failure at the rubber-adhesive interface.
force (lbs) required to produce failure. In cases where the R-25, RC-25, M-50 means that three types of failures are present with
failure is in the rubber, the adhesion value is recognized as R indicating 25 % failure in the rubber, RC, 25 % failure between the
rubber and the cement (adhesive) interface, and 50 % failure at the
being higher than that recorded. metal-primer interface.

63. Report 67. Apparatus

63.1 The report shall include the following, preferably
67.1 Test Specimens—Fig. 17 shows a molded test speci-
reported on an Adhesion Test Data Sheet illustrated in Table 1:
men. The diameter of the substrate component (for example,
63.1.1 Type and code number of the rubber compound,
steel, aluminum, plastic, etc.) shall be 25 6 0.1 mm and the
63.1.2 Cure time and temperature,
length 20 6 0.1 mm. The rubber sections shall be 23 6 0.1 mm
63.1.3 Type of metal or rigid substrate used and surface
in diameter and 10 6 0.1 mm in length. A single- or
preparation,
multi-cavity mold can be used to make the bonded specimen,
63.1.4 Molding method used (compression, injection, etc.)
and it may be a mold for compression, transfer, or injection
63.1.5 Adhesive used, dilution, and application method,
molding.
63.1.6 The adhesion value for each test piece,
63.1.7 Type and percentage of failure, 67.2 Test Fixture—Fig. 18 shows the test fixture for holding
63.1.8 Date of vulcanization and date of test, and the bonded specimens in a strained position. The suggested
63.1.9 Temperature of test room and humidity. strain is 100 %, however, some elastomers may have an
ultimate shear strain less than 100 % and thus a fixture must be
64. Precision and Bias made to accommodate the lower shear strain value. A guideline
64.1 Precision and bias do not exist for this test method is as follows:
because resources necessary for round-robin testing have not Ultimate Shear Strain (%) Test Strain (%)
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>200 100
been forthcoming. 100 to 200 50
50 to 100 25

METHOD G—MEASURING BOND DURABILITY While the test fixture frames may be steel, acetal plastic is
FOR RUBBER-TO-METAL BONDED COMPONENTS preferred. The plastic does not corrode or otherwise contribute
WITH A DOUBLE SHEAR CYLINDRICAL SPECIMEN to bond failure. Tests have shown consistent results with acetal
frames. The positioning of the hole in the frame’s center piece
65. Significance and Use determines the percent strain.
65.1 Method G is used to determine relative bond durability 67.3 Test Apparatus—Fig. 19 shows one apparatus that may
between various adhesives. The adhesives to be compared are be used for immersing the fixtured test specimens. While the
used to bond rubber-to-metal using a double shear cylindrical exposure conditions may be varied to suit individual programs,
specimen (see Fig. 17) which is then placed in a fixture to the following have been used successfully:
impart a shear stress on the bond line. This assembly (see Fig. Media: 5 % sodium chloride solution in distilled water
18) is then placed in the prescribed test medium and the time Temperature: 35 ± 1°C
Dissolved Oxygen: 17 ± 1 mg/L
to obtain a failure depth of 5 mm at the rubber-metal bond
interface is noted. This test measures the durability of a specific
68. Laboratory Preparation of Test Specimens
adhesive as a function of changes in the rubber formation.
Different adhesives may be examined to find the best for a 68.1 Prepare the test face of the cylinders with any test
given rubber recipe. Also, different metal preparations and their method for securing adhesion that may be under investigation,
effect on bond durability may be investigated. for example, phosphate treated, mechanical blast, etc.

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FIG. 18 Test Specimen in a 100 % Strain Fixture (Frame)

FIG. 19 Test Samples in the Environmental Chamber

68.2 Coat the prepared metal surface with the adhesive 68.5 After a suitable vulcanization cycle, remove the speci-
system to be tested in accordance with the manufacturer’s mens. Store the specimens at a temperature of 23 6 2°C (73 6
recommendations, for example, film thickness, dry time. 4°F) for at least 16 h prior to testing.
68.3 Place the dry adhesive coated specimens in the mold. 69. Procedure
Fig. 20 illustrates the basic mold design for a transfer mold. For
compression or transfer molding, place the rubber preform in 69.1 Pull one testpiece of each molded batch to determine
the mold cavity or transfer pot. For injection molding, inject that 100 % adhesion, for example 100R, is obtained prior to
the rubber into the mold. immersion.
68.4 The test specimens are formed by vulcanizing the 69.2 Secure the bonded test specimens in the test fixture
desired type of rubber in a mold containing the adhesive coated with the chosen % strain.
metal cylinders. The cure conditions (temperature and time) 69.3 It is suggested that 5 samples (20 interfaces) are tested
are determined by the elastomer compound being used. for each experiment.
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FIG. 20 Basic Mold Design for Making Adhesion Test Pieces

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NOTE 1—All dimensions in mm unless otherwise noted.

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NOTE 1—Prestrains 0, 50, and 100 % (left to right)

FIG. 21 Quadruple Shear Test Pieces

69.4 Immerse these fixtured parts into the test chamber 71.9 The adhesive used, dilution, application method and
which has been prepared in terms of temperature and salt film thickness,
content. Begin the oxygen bubbling at the selected rate. At 71.10 The type and percentage of bond failure, and
various time intervals, remove the fixtured samples, and using
a short steel ruler or other calibrated scale, measure the debond 71.11 Date of vulcanization and date of failure measure-
depth. Continue the test until the debond depth of 5 mm is ment.
noted for each bond. 72. Precision and Bias
70. Calculation 72.1 Precision and bias do not exist for this test method
because resources necessary for round-robin testing have not
70.1 Measure the amount of debond in mm and the corre- been forthcoming.
sponding time.

71. Report METHOD H—MEASURING BOND DURABILITY OF

71.1 The report shall include the type and code number of RUBBER-TO-METAL BONDED COMPONENTS WITH
the rubber compound, QUADRUPLE LAP SHEAR SPECIMEN
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71.2 Cure time and temperature, 73. Significance and Use

71.3 Molding method (for example, compression, transfer, 73.1 This method has all the attributes of Method G except
injection), that no fixture for imparting the shear stress is required, only a
simple block inserted into the test piece once the pre-strain has
71.4 Type of substrate and its surface preparation, been applied. The test piece dimensions are similar to an
71.5 Test conditions (salt concentration, dissolved oxygen existing standard adhesion test piece ISO 1827: 1991 (BS903:
level, temperature, test shear strain), A14: 1992(1998)). This results in a compact test piece,
71.6 The failure criterion (for example, 5 mm of bond pre-strained to a selected pre-strain, for exposure to prescribed
failure), environments such as salt spray, elevated temperature and
humidity, boiling water, hot glycol or brine. See Fig. 21. Note
71.7 The average time required by the replicate bonds to that the use of a pre-strain of 100 %, and immersion in boiling
meet the failure criterion, along with standard deviation and water, has provided a highly accelerated test for aqueous
95 % confidence interval, bonding agents subjected to water immersion at ambient
71.8 Molding method used, temperature.

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NOTE 1—a.) Unstrained; b.) 100 % strain.
FIG. 22 Quadruple Shear Test Piece

74. Adhesion Failure Terminology shall travel at the uniform rate of 0.83 6 0.08 mm/s. (2 6 0.2
74.1 Express the type of adhesion failure as determined by in./min.). The machine shall be provided with a recording
the visual examination of the of the failed area using one or device to give the force in Newtons or pounds-force at the
more of the following symbols: conclusion of the test.
74.1.1 R indicates the failure is in the rubber. 76. Laboratory Preparation of Test Specimens
74.1.2 RC indicates the failure is at the rubber-cover cement
interface. 76.1 Masking is required to ensure that the bonding agent is
74.1.3 CP indicates the failure is at the cover cement-prime applied only to the portion of the plates where bonding is
cement interface. required. The bonding agent is applied and dried according to
74.1.4 M indicates the failure is at the metal-prime cement the manufacture’s suggestions.
interface. 76.2 The bonding shall be done using compression molding,
NOTE 16—Example-The percentage of the various types of failure may transfer molding or injection molding of the rubber into a
be estimated as in the following examples: R-60, RC -40 means that 60 % suitable mold holding the adhesive coated samples.
of the bonded area showed failure in the rubber and the other 40% showed 76.3 A minimum of two replicates (eight interfaces) shall be
failure at the rubber-adhesive interface. R-25, RC-25, M-50 means that
three types of failures are present with R indicating 25 % failure in the used for each prestrain and environmental condition, plus two
rubber, RC, 25 % failure between the rubber and the cement (adhesive) control replicates for each prestrain. In addition, one test piece
interface, and 50 % failure at the metal-primer interface. of each batch shall be prepared as a quality control for the
bonding procedure.
75. Apparatus
75.1 Test pieces. Fig. 21 shows a photo of the molded test 77. Procedure
piece. 77.1 Pull a quality control test piece from each molded
75.2 The test piece consists of four identical rubber batch to determine that 100 % adhesion (100R) is obtained
elements, 4mm6 1mm thick, 20mm 6 5mm wide and 25 mm prior to environmental exposure or laboratory storage with a
6 5mm long. The rubber is bonded to rigid plates of the same pre-strain.
width and appropriate lengths to obtain a symmetrical double- 77.2 Test pieces are pre-strained by pulling in a test machine
sandwich arrangements. The central plates may have a hole at to just above the desired pre-strain and inserting a nylon block
each protruding end to accommodate pins to fixture the of suitable dimensions (14 x 9 mm for 100 % strain) between
assembly to the test machine. See Fig. 22. the central metal plates to maintain the prescribed prestrain.
75.3 Suitable blocks (for example, nylon) to maintain the 77.3 Subject the test pieces to the chosen environmental
desired prestrain. The shape of the block shall be such that, in conditions, for example, those shown in 67.3 (Method G).
addition to setting the prescribed prestrain, there is no contact Monitor these conditions to ensure they are stable (for
between the block and the strained rubber elements (see Fig. example, for aqueous immersion, the solutions should be
22). stirred adequately and the pH and oxygen concentration should
75.4 Testing machine: To test the adhesion before/after an be checked regularly). Control test pieces are to be kept under
immersion test, a power driven test machine equipped to standard laboratory temperature and humidity.
produce a uniform rate of grip separation shall be used for 77.4 Inspect test pieces for signs of corrosion or incipient
measuring the strength of adhesion. The head of the machine bond failure at appropriate periods (for example, twice hourly

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for eight h; twice daily for 1 week; weekly for 1 month then 4 78.7 The failure criterion (for example, 5 mm bond failure
weekly). Using a short steel ruler or other calibrated scale, during environmental exposure).
measure the de-bond depth. 78.8 An estimate of the time it would take to reach the
77.5 After a predetermined period of time, pull to failure failure criterion under the prescribed environmental conditions.
each test piece which remains sufficiently intact, including Ideally this will be the average time taken by replicates to reach
those exposed to the chosen environmental conditions and the the failure criterion, but for effective bonding agents extrapo-
control test pieces, and record the peak force required to do lation may be desirable to avoid unacceptably long test times.
this. 78.9 Type and percentage of bond failure during final shear
77.6 Measure the amount of de-bond in mm and classify the test and of incipient bond failure during environmental expo-
loci of failure according to Section 74. Note that the loci may sure; shear load to failure of test pieces at the end of the
be different according to whether the failure took place during prescribed period of environmental exposure.
the environmental exposure or during the pull to failure.
78.10 Dates of vulcanisation, environmental exposure, in-
78. Report cipient failure inspections and tensile machine pull to failure.
78.1 The report shall include the type and code of the rubber 78.11 As an option, load-deflection plots for all shear tests
compound. to failure, and for the prestrain applied as in 77.2, may be
measured and reported.
78.2 Cure time and temperature.
78.3 Molding method (for example, compression, transfer, 79. Precision and Bias
or injection).
79.1 Precision and bias do not exist for this test method
78.4 Type of substrate and surface preparation. because resources necessary for round-robin testing have not
78.5 Bonding agent used, application method and film been forthcoming.
thickness.
78.6 Environmental test conditions (for example, immer- 80. Keywords
sion medium, temperature), prestrain(s) and maximum dura- 80.1 adhesion; adhesive; bond durability; double-shear test
tion of exposure. piece; elastomer; metals; rubber; rubber-to-metal bonding

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