Designation: D4776/D4776M − 10

Standard Test Method for

Adhesion of Tire Cords and Other Reinforcing Cords to
Rubber Compounds by H-Test Procedure1
This standard is issued under the fixed designation D4776/D4776M; 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.

1. Scope D2229 Test Method for Adhesion Between Steel Tire Cords
1.1 This test method covers the measurement of adhesion of and Rubber
reinforcing cords that are bonded to rubber compounds. This D4393 Test Method for Strap Peel Adhesion of Reinforcing
test method is applicable to textile cord structures from both Cords or Fabrics to Rubber Compounds
natural and manmade fibers, other than steel. For adhesion D6477 Terminology Relating to Tire Cord, Bead Wire, Hose
testing of steel tire cords, refer to Test Method D2229. Reinforcing Wire, and Fabrics
1.2 This test method is primarily used to evaluate tire cords, 3. Terminology
using a suitable tire cord adhesive and a suitable rubber
compound. This test method is also used to evaluate (1) tire 3.1 Definitions:
cord adhesives, and (2) the process of adhesive reaction on the 3.1.1 For defintions of terms relating to tire cord, bead wire,
cord using one consistent form of tire cord and one consistent hose wire, and tire cord fabrics, refer to Terminology D6477.
rubber compound. This test method may be used to evaluate 3.1.1.1 The following terms are relevant to this standard:
cords in industrial hose and belting products and other cord adhesion, adhesion, in tire fabrics, cord, curing, H-test
reinforced rubber products. adhesion, industrial yarn, reinforcing cord, rubber, rubber
compound, as used in the manufacture of rubber articles,
1.3 The values stated in either SI units or inch-pound units vulcanization.
are to be regarded separately as standard. The values stated in 3.1.2 For definitions of other terms relating to rubber, refer
each system may not be exact equivalents; therefore, each to Terminology D1566.
system shall be used independently of the other. Combining 3.1.3 For definitions of other textile terms related to textiles,
values from the two systems may result in non-conformance refer to Terminology D123.
with the standard.
1.4 This standard does not purport to address all of the 4. Summary of Test Method
safety concerns, if any, associated with its use. It is the 4.1 A cord specimen is sandwiched between two layers of
responsibility of the user of this standard to establish appro- rubber compound test stock in a form resembling an “H,”
priate safety and health practices and determine the applica- placed in a heated mold, and cured at a specified temperature
bility of regulatory limitations prior to use. and pressure. The test specimen sandwich is then cut to create
an H-test specimen consisting of a single cord with each end
2. Referenced Documents embedded in the center of a tab end of the rubber test block
2.1 ASTM Standards:2 (Fig. 1). The test specimen is placed in the grips of the tensile
D76 Specification for Tensile Testing Machines for Textiles tester, and then the grips are separated. The maximum force
D123 Terminology Relating to Textiles obtained is the H-test adhesion force.
D1566 Terminology Relating to Rubber
5. Significance and Use
5.1 Test Method D4776 for the determination of the H-test
1
This test method is under the jurisdiction of ASTM Committee D13 on Textiles adhesion of reinforcing cords to rubber compounds may be
and is the direct responsibility of Subcommittee D13.19 on Industrial Fibers and used for the acceptance testing of commercial shipments of
Metallic Reinforcements
Current edition approved Jan. 1, 2010. Published January 2010. Originally reinforcing cords but caution is advised since information
approved in 1988. Last previous edition approved in 2004 as D4776 – 04ε1. DOI: about between-laboratory precision is incomplete. Compara-
10.1520/D4776-10.
2
tive tests as directed in 5.1.1 may be advisable.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
5.1.1 In cases of dispute arising from the differences in
contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on reported test results when using Test Method D4776 for
the ASTM website. acceptance testing of commercial shipments, the purchaser and

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

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 D4776/D4776M − 10
5.4 The expected range of values which characterize accept-
able adhesion can be determined in any cord-rubber combina-
tion with experience. For this reason, the purchaser normally
establishes a minimum level of adhesion to be obtained by the
supplier in either the supplier’s laboratory or the purchaser’s
laboratory using either the supplier’s standard rubber com-
pound or the purchaser’s rubber compound.
5.5 Another procedure for testing adhesion of cords to
rubber compounds is Test Methods D4393 . This procedure has
been used extensively in the trade for acceptance testing.
Results obtained by this method cannot be used interchange-
ably since there is no overall correlation between them.

6. Apparatus and Materials

6.1 Tensile Testing Machine—Although a constant-rate-of-
extension (CRE) tensile testing machine is preferred, a
constant-rate-of-traverse (CRT type, pendulum type) may be
used. The specification and methods of calibration and verifi-
cation of these machines shall conform to Specification D76.
The testing machine shall be equipped with an autographic
recorder (rectilinear coordinates preferred) or an interface
computer. There is a distinct difference between the CRE and
CRT type testing machines. Consequently, they cannot be used
interchangeably unless a mathematical correlation has been
established and agreed upon by the purchaser and supplier.
6.2 Curing Press, capable of maintaining a minimum pres-
sure of 3.5 MPa [500 psi] over the total area of the mold
surface, equipped with 300 by 300 mm [12 by 12 in.] platens
FIG. 1 H-Test Specimen or larger, and capable of a platen temperature control within
63°C [65°F] of the temperature specified for curing the
the supplier should conduct comparative tests to determine if rubber compound.
there is statistical bias between their laboratories. Competent 6.3 Molds—The design of the molds shall be as shown in
statistical assistance is recommended for the investigation of Fig. 2. The dimensions of the test specimen are controlled by
bias. As a minimum, the two parties should take a group of test the specifications and tolerances of the mold. The dimensions
specimens which are as homogeneous as possible and which of the mold (6.40 mm [0.250 in.] embedment) in Fig. 2a shall
are from a lot of material of the type in question. The test be used for cords with a dtex of 1100/2 [denier larger than
specimens should then be randomly assigned in equal numbers 1000/2] or less. The dimensions of the mold (9.52 mm [0.375
to each laboratory for testing. The average results from the two in.] embedment) in Fig. 2b shall be used for cords with a dtex
laboratories should be compared using Student’s t-test for larger than 1100/2 [denier larger than 1000/2]. The slot size for
unpaired data and an acceptable probability level chosen by the each mold shall be 1.17 mm 6 0.13 mm [0.046 in. 6 0.005
two parties before testing begins. If a bias is found, either its in.].
cause must be found and corrected or the purchaser and the
supplier must agree to interpret future test results in light of the 6.4 Specimen Grips—The design of the specimen grips shall
known bias. be as shown in Fig. 3. Two grips are required.
5.2 This test method is used to measure the force required to 6.5 Tensioning Masses—The masses may be of the hook
extract the cord from a rubber compound test block. type, or designed in such a manner that they can be clamped to
the cord. In any event, the total mass shall be 50 g.
5.3 This test method is designed to test the adhesion of
textiles that are bonded to rubber compounds. Variables that 6.6 Sheeted Rubber Compound, (sometimes called skim
may contribute to differences in results of this test method stock), supported on a non hygroscopic backing, such as a
include adhesive type, adhesive application procedure, adhe- plasticizer-free plastic material. Polyethylene film has been
sive cure, fiber type, construction of cords, rubber type, rubber found to be satisfactory. The thickness of the rubber stock
cure, and rubber thickness. required to fill the mold properly shall be determined by
5.3.1 The deleterious effect of ozone in combination with experience. As a guide, the thickness of the rubber stock should
atmospheric moisture on the ability of adhesives to bond with be not less than 8 % greater than one-half of the mold cavity
rubber requires assiduous protection of cords prior to embed- depth. In any event, the thickness is agreed upon between the
ment. purchaser and supplier.

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 D4776/D4776M − 10

NOTE 1—The important dimension is shown by an asterisk and shall not

be altered. All other dimensions are included as guides and may be altered
if desired.
Dimension mm [in.]
A 1.6 [.06]
B 12.5 [.50]
C 25.0 [1.00]
D 40.0 [1.50]
E 7.0 [.28]
F 14.0 [.56]
NOTE 1—The mold as shown will produce 30 specimens. It may be G 4.0 [.16]
fabricated to produce a larger or smaller number, but the dimensions that
govern the specimen size shall not be altered. FIG. 3 Specimen Grips for H-Test
NOTE 2—A mold cover plate must be provided. It should be 9.5 mm
[.38 in.] thick and the same outside dimensions (“K” and“ L”] as the mold.
NOTE 3—Mold dimension tolerances are XX.X mm 6 .3 mm [XX.XX 6.9 Shears, for trimming.
in. 6 .01 in.] or XX.XX mm 6 .13 mm [XX.XXX in. 6 .005 in.].
Dimension 2a 2b
6.10 Gloves, of temperature resistant material.
mm [in.] mm [in.[ 6.11 Mold Release Lubricant , A suitable mold release
A 12.70 [.500] 15.88 [.625]
B 17.5 [.69] 17.5 [.69] lubricant may be applied to the empty mold to facilitate test
C 6.35 [.250] 9.52 [.375] block removal. Excess lubricant shall be wiped from the mold
D 3.17 [.125] 3.17 [.125] and particularly from the slots provided for the cords. The
E 34.9 [1.38] 34.9 [1.38]
F 25.40 [1.000] 25.40 [1.000] lubricant should not be applied when exposed cord is in the
G 25.4 [1.00] 25.4 [1.00] area, and should only be used when absolutely necessary. Use
H 1.17 [0.046] 1.17 [0.046] of mold release lubricant should be reported on the test report.
J 6.40 [.250] 6.40 [.250]
K 149.2 [5.88] 177.8 [7.00] NOTE 1—The use of mold release lubricant is not recommended. The
L 9.5 [.38] 9.5 [.38] mold should be covered permanently with Teflon® or, preferably, with a
M 196.8 [7.75] 196.8 [7.75]
stainless stell reinforced nonstick cating such as Excalibur®.
FIG. 2 Mold for H-Test
7. Sampling
7.1 Lot Sample—As a lot sample for acceptance testing, take
6.6.1 Rubber stock properties are best maintained by stor-
at random the number of primary sampling units directed in an
age in a cool, dry atmosphere. Excessive rubber stock moisture
applicable material specification or other agreement between
may lower adhesion of some fiber/rubber composites.
the purchaser and the supplier. Consider shipping cases of cord
6.6.2 Rubber compounds exhibit wide variations in shelf
to be the primary sampling units. Exercise caution in sampling
life (properties suitable for good adhesion results) dependent
and handling so that samples receive minimum exposure to
upon both composition and storage condition. Rubber com-
ambient atmosphere and light prior to rubber embedment. This
pounds are usually replaced after three months; however, some
can be accomplished by storing the sample in a sealed, black
may require replacement within a few weeks. In any event,
plastic bag. Rayon is particularly sensitive to moisture pick-up
storage conditions and shelf life should be specified by the
(which negatively affects adhesion) and should be handled
supplier of the rubber compound.
accordingly.
6.7 Timers, having 60 min capacity, 1⁄2 min intervals.
NOTE 2—A realistic specification or other agreement between the
6.8 Marking Pen, silver ink for rubber.3 purchaser and the supplier requires taking into account the variability
between primary shipping units and within primary shipping units so as to
provide a sampling plan with meaningful producer’s risk, consumer’s risk,
3
Available from Fisher Pen Co., Forest Park, IL. acceptable quality level, and limiting quality level.

3
 D4776/D4776M − 10
7.2 Laboratory Sample—Take at random the number of 8.6 Place the cover plat on the mold, then remove the
packages per shipping case in the lot sample directed in an masses and place the mold in a preheated press. Adjust the
applicable material specification or other agreement between pressure to a minimum of 3.5 MPa [500 psi] with reference to
the purchaser and the supplier. the mold surface. Vulcanize for the specified time at the
7.3 Test Specimens—Prepare 15 specimens, or other number specified pressure and temperature. Immediately remove the
as agreed upon between the purchaser and the supplier, from mold assembly from the hot curing press.
each sample as directed in Section 8. 8.7 Remove mold cover plate then carefully remove the
constructed rubber and cord test pad from the test mold cavity
8. Preparation of Test Specimens and cool at room temperature. Condition prepared specimens at
8.1 Cut the rubber stock in strips 6 mm [0.25 in.] wide and 24 6 1°C [75 6 2°F] and 55 6 2% relative humidity for 4 h
150 mm [6.0 in.] long, leaving the protective film attached. minimum, 4 days maximum, unless otherwise agreed between
This may be done with shears or with a clicker die. purchaser and supplier. (Immediate testing is sometimes pre-
8.1.1 Some laboratories have fabricated larger molds to ferred).
accommodate a greater number of test specimens. In those 8.8 Cut the cord test pad using shears, a sharp knife, or
laboratories, the length of the rubber stock must be adjusted clicker die to produce individual H-test adhesion specimens
accordingly. consisting of a single cord with each end embedded in the
8.2 A mold preheated to the curing temperature is preferred. center of a rubber tab approximately 25 mm [1 in.] in length
(Fig. 1). Trim off excess rubber flash.
NOTE 3—When a preheated mold is used, the specimens must be loaded
and placed in the curing press within 3 min. The use of a preheated mold 9. Procedure
will alter the curing conditions (time and temperature) of the rubber.
8.3 Remove the protective film from the rubber test strips, 9.1 Perform test in the standard atmosphere for testing tire
then place the individual rubber test strips in the mold cavities cords, which is 24 6 1°C [75 6 2°F] and 55 6 2 % relative
with the protective film side on top. humidity.

8.4 Place the cords in the cord slots by cutting cord test 9.2 Prepare tensile tester with test grips described in Fig. 3;
specimens allowing sufficient overhang for attaching masses ensure axial alignment. Set the gage distance between the grips
and tie a knot in both ends. Take care to prevent the loss of cord to 1.5 mm [0.0625 in.]. Set the crosshead speed to 125 6 10
twist. The portion of the cord that is embedded in rubber must mm/min [5 6 0.5 in./min].
not be touched by the bare hand. Attach a 50 g mass on one 9.3 Insert the H-test adhesion specimen in the clamps,
knotted end of the test cord. Two cords may be tied together having one leg of the “H” in the upper clamp, and the other leg
and used to fill adjacent slots; a 100 g mass is used in this case in the lower grip.
(Fig. 4). Place one end of the knotted test specimen so that it 9.4 Activate the crosshead. Observe and record the cord
is snubbed firmly against the cord slots on one side of the mold. pull-out adhesion force to the nearest 0.5 N [0.1 lbf] by means
8.5 After all the cord slots are filled, remove the protective of an automatic recorder, or interfaced computer.
film from the additional strips of rubber and place them in the 9.5 Repeat, until the number of test specimens, as agreed
mold cavities on top of the cords. The side from which the upon between the purchaser and supplier, have been tested for
protective film was removed will be down. Identify each each laboratory sample.
specimen with a silver ink marking pen.
9.6 When elevated temperature testing is required, test as
directed in 9.2-9.5, except enclose the specimen grips in an
oven attached to the tensile tester. Heat the specimens in the
oven, controlled at the specified temperature for not less than
15 min and not more than 60 min total elapsed time for testing
of any one specimen.
9.6.1 As an alternate procedure, the specimens may be
heated in an oven adjacent to the tensile testing machine and
then removed, one at a time, and tested within 15 s after
removal. The technique for heating and testing the specimens
must be agreed upon by the purchaser and the supplier.

10. Report
10.1 Report the following information:
10.1.1 State that the tests were performed as directed in Test
Method D4776. Describe the products sampled and the method
of sampling used.
10.1.2 Cord identification and construction.
10.1.3 Adhesive identity, cord percent dip pick-up, and
FIG. 4 Mold Loading curing conditions (time, temperature, pressure), when known.

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 D4776/D4776M − 10
10.1.4 Test condition temperature. cords to rubber compounds by h-test procedure is being
10.1.5 Rubber stock identification and gage (thickness). determined and will be available on or before December 2003.
10.1.6 Type tensile tester used. It is not feasible to specify the precision of the procedure at this
10.1.7 Average of the number of specimen determinations time because the results of the previous round robin as reported
per sample, to the nearest 0.5 N [0.1 lbf]. in prior revisions of this test method are suspect and plans
currently underway to conduct another round robin.
11. Precision and Bias
11.1 The precision of the procedure in Test Method D4776 12. Keywords
for measuring adhesion of tire cords and other reinforcing 12.1 adhesion; reinforcements (textiles); rubber; tire cord

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