1、Designation: D 4776 04Standard Test Method forAdhesion of Tire Cords and Other Reinforcing Cords toRubber Compounds by H-Test Procedure1This standard is issued under the fixed designation D 4776; the number immediately following the designation indicates the year oforiginal adoption or, in the case
2、of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the measurement of adhesion ofreinforcing cords that are bonded to r
3、ubber compounds. Thistest method is applicable to textile cord structures from bothnatural and manmade fibers, other than steel. For adhesiontesting of steel tire cords, refer to Test Method D 2229.1.2 This test method is primarily used to evaluate tire cords,using a suitable tire cord adhesive and
4、a suitable rubbercompound. This test method is also used to evaluate (1) tirecord adhesives, and (2) the process of adhesive reaction on thecord using one consistent form of tire cord and one consistentrubber compound. This test method may be used to evaluatecords in industrial hose and belting prod
5、ucts and other cordreinforced rubber products.1.3 This test method is written in SI units. The inch-poundunits which are provided in this test method are not necessarilyexact equivalents of the SI units. Either system may be used inthis test method.1.4 This standard does not purport to address all o
6、f thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 76 Specification for
7、Tensile Testing Machines for TextilesD 123 Terminology Relating to TextilesD 1566 Terminology Relating to RubberD 2229 Test Method for Adhesion Between Steel TireCords and RubberD 4393 Test Method for Strap Peel Adhesion of ReinforcingCords or Fabrics to Rubber CompoundsD 6477 Terminology Relating t
8、o Tire Cords, Bead Wire,Hose Reinforcing Wire, and Fabrics3. Terminology3.1 Definitions:3.1.1 For defintions of terms relating to tire cord, bead wire,hose wire, and tire cord fabrics, refer to Terminology D 6477.3.1.1.1 The following terms are relevant to this standard:adhesion, adhesion, in tire f
9、abrics, cord, curing, H-test adhe-sion, industrial yarn, reinforcing cord, rubber, rubber com-pound, as used in the manufacture of rubber articles, vulcani-zation.3.1.2 For definitions of other terms relating to rubber, referto Terminology D 1566.3.1.3 For definitions of other textile terms related
10、to textiles,refer to Terminology D 123.4. Summary of Test Method4.1 A cord specimen is sandwiched between two layers ofrubber compound test stock in a form resembling an “H,”placed in a heated mold, and cured at a specified temperatureand pressure. The test specimen sandwich is then cut to createan
11、H-test specimen consisting of a single cord with each endembedded in the center of a tab end of the rubber test block(Fig. 1). The test specimen is placed in the grips of the tensiletester, and then the grips are separated. The maximum forceobtained is the H-test adhesion force.5. Significance and U
12、se5.1 Test Method D 4776 for the determination of the H-testadhesion of reinforcing cords to rubber compounds may beused for the acceptance testing of commercial shipments ofreinforcing cords but caution is advised since informationabout between-laboratory precision is incomplete. Compara-tive tests
13、 as directed in 5.1.1 may be advisable.5.1.1 In cases of dispute arising from the differences inreported test results when using Test Method D 4776 foracceptance testing of commercial shipments, the purchaser andthe supplier should conduct comparative tests to determine ifthere is statistical bias b
14、etween their laboratories. Competentstatistical assistance is recommended for the investigation ofbias. As a minimum, the two parties should take a group of testspecimens which are as homogeneous as possible and whichare from a lot of material of the type in question. The test1This test method is un
15、der the jurisdiction of ASTM Committee D13 on Textilesand is the direct responsibility of Subcommittee D13.19 on Tire Cord and Fabrics.Current edition approved Oct. 1, 2004. Published October 2004. Originallypublished as D 4776 88. Last previous edition D 4776 02.2For referenced ASTM standards, visi
16、t the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-29
17、59, United States.specimens should then be randomly assigned in equal numbersto each laboratory for testing. The average results from the twolaboratories should be compared using Students t-test forunpaired data and an acceptable probability level chosen by thetwo parties before testing begins. If a
18、 bias is found, either itscause must be found and corrected or the purchaser and thesupplier must agree to interpret future test results in light of theknown bias.5.2 This test method is used to measure the force required toextract the cord from a rubber compound test block.5.3 This test method is d
19、esigned to test the adhesion oftextiles that are bonded to rubber compounds. Variables thatmay contribute to differences in results of this test methodinclude adhesive type, adhesive application procedure, adhe-sive cure, fiber type, construction of cords, rubber type, rubbercure, and rubber thickne
20、ss.5.3.1 The deleterious effect of ozone in combination withatmospheric moisture on the ability of adhesives to bond withrubber requires assiduous protection of cords prior to embed-ment.5.4 The expected range of values which characterize accept-able adhesion can be determined in any cord-rubber com
21、bina-tion with experience. For this reason, the purchaser normallyestablishes a minimum level of adhesion to be obtained by thesupplier in either the suppliers laboratory or the purchaserslaboratory using either the suppliers standard rubber com-pound or the purchasers rubber compound.5.5 Another pr
22、ocedure for testing adhesion of cords torubber compounds is Test Methods D 4393 . This procedurehas 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 Materials6
23、.1 Tensile Testing MachineAlthough a constant-rate-of-extension (CRE) tensile testing machine is preferred, aconstant-rate-of-traverse (CRT type, pendulum type) may beused. The specification and methods of calibration and verifi-cation of these machines shall conform to Specification D 76.The testin
24、g machine shall be equipped with an autographicrecorder (rectilinear coordinates preferred) or an interfacecomputer. There is a distinct difference between the CRE andCRT type testing machines. Consequently, they cannot be usedinterchangeably unless a mathematical correlation has beenestablished and
25、 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 moldsurface, equipped with 300 by 300 mm (12 by 12 in.) platensor larger, and capable of a platen temperature control within63C (65F) of the tempera
26、ture specified for curing therubber compound.6.3 MoldsThe design of the molds shall be as shown inFig. 2. The dimensions of the test specimen are controlled bythe specifications and tolerances of the mold. The dimensionsof the mold (6.40 mm 0.250 in. embedment) in Fig. 2a shallbe used for cords with
27、 a dtex of 1100/2 or less. The dimensionsof the mold (9.52 mm 0.375 in. embedment) in Fig. 2b shallbe used for cords with a dtex larger than 1100/2. The slot sizefor each mold shall be 1.17 mm 6 0.13 mm (0.46 in. 6 0.005in.).6.4 Specimen GripsThe design of the specimen gripsshall be as shown in Fig.
28、 3. Two grips are required.6.5 Tensioning MassesThe masses may be of the hooktype, or designed in such a manner that they can be clamped tothe cord. In any event, the total mass shall be 50 g.6.6 Sheeted Rubber Compound, (sometimes called skimstock), supported on a non hygroscopic backing, such as a
29、plasticizer-free plastic material. Polyethylene film has beenfound to be satisfactory. The thickness of the rubber stockrequired to fill the mold properly shall be determined byexperience. As a guide, the thickness of the rubber stock shouldbe not less than 8 % greater than one-half of the mold cavi
30、tydepth. In any event, the thickness is agreed upon between thepurchaser and supplier.6.6.1 Rubber stock properties are best maintained by stor-age in a cool, dry atmosphere. Excessive rubber stock moisturemay lower adhesion of some fiber/rubber composites.6.6.2 Rubber compounds exhibit wide variati
31、ons in shelflife (properties suitable for good adhesion results) dependentupon both composition and storage condition. Rubber com-pounds are usually replaced after three months; however, somemay require replacement within a few weeks. In any event,storage conditions and shelf life should be specifie
32、d by thesupplier of the rubber compound.6.7 Timers, having 60 min capacity,12 min intervals.FIG. 1 H-Test SpecimenD47760426.8 Marking Pen, silver ink for rubber.36.9 Shears, for trimming.6.10 Gloves, of temperature resistant material.6.11 Mold Release Lubricant , A suitable mold releaselubricant may
33、 be applied to the empty mold to facilitate testblock removal. Excess lubricant shall be wiped from the moldand particularly from the slots provided for the cords. Thelubricant should not be applied when exposed cord is in thearea, and should only be used when absolutely necessary. Useof mold releas
34、e lubricant should be reported on the test report.NOTE 1The use of mold release lubricant is not recommended. Themold should be covered permanently with Teflont or, preferably, with astainless stell reinforced nonstick cating such as Excaliburt.7. Sampling7.1 Lot SampleAs a lot sample for acceptance
35、 testing,take at random the number of primary sampling units directedin an applicable material specification or other agreementbetween the purchaser and the supplier. Consider shippingcases of cord to be the primary sampling units. Exercisecaution in sampling and handling so that samples receivemini
36、mum exposure to ambient atmosphere and light prior torubber embedment. This can be accomplished by storing thesample in a sealed, black plastic bag. Rayon is particularlysensitive to moisture pick-up (which negatively affects adhe-sion) and should be handled accordingly.NOTE 2A realistic specificati
37、on or other agreement between thepurchaser and the supplier requires taking into account the variabilitybetween primary shipping units and within primary shipping units so as toprovide a sampling plan with meaningful producers risk, consumers risk,acceptable quality level, and limiting quality level
38、.7.2 Laboratory SampleTake at random the number ofpackages per shipping case in the lot sample directed in anapplicable material specification or other agreement betweenthe purchaser and the supplier.7.3 Test SpecimensPrepare 15 specimens, or other num-ber as agreed upon between the purchaser and th
39、e supplier,from each sample as directed in Section 8.8. Preparation of Test Specimens8.1 Cut the rubber stock in strips 6 mm (0.25 in.) wide and150 mm (6.0 in.) long, leaving the protective film attached.This may be done with shears or with a clicker die.3Available from Fisher Pen Co., Forest Park,
40、IL.NOTE 1The mold as shown will produce 30 specimens. It may befabricated to produce a larger or smaller number, but the dimensions thatgovern the specimen size shall not be altered.NOTE 2A mold cover plate must be provided. It should be 9.5 mm(.38 in.) thick and the same outside dimensions (“K” and
41、“ L”) as the mold.NOTE 3Mold dimension tolerances are XX.X mm 6 .3 mm (XX.XXin. 6 .01 in.) or XX.XX mm 6 .13 mm (XX.XXX in. 6 .005 in.).Dimension 2a 2bmm in. mm in.A 12.70 .500 15.88 .625B 17.5 .69 17.5 .69C 6.35 .250 9.52 .375D 3.17 .125 3.17 .125E 34.9 1.38 34.9 1.38F 25.40 1.000 25.40 1.000G 25.4
42、 1.00 25.4 1.00H 1.17 1.046 1.17 .046J 6.40 .250 6.40 .250K 149.2 5.88 177.8 7.00L 9.5 .38 9.5 .38M 196.8 7.75 196.8 7.75FIG. 2 Mold for H-TestNOTE 1The important dimension is shown by an asterisk and shallnot be altered. All other dimensions are included as guides and may bealtered if desired.Dimen
43、sion mm in.A 1.6 .06B 12.5 .50C 25.0 1.00D 40.0 1.50E 7.0 .28F 14.0 .56G 4.0 .16FIG. 3 Specimen Grips for H-TestD47760438.1.1 Some laboratories have fabricated larger molds toaccommodate a greater number of test specimens. In thoselaboratories, the length of the rubber stock must be adjustedaccordin
44、gly.8.2 A mold preheated to the curing temperature is preferred.NOTE 3When a preheated mold is used, the specimens must be loadedand placed in the curing press within 3 min. The use of a preheated moldwill alter the curing conditions (time and temperature) of the rubber.8.3 Remove the protective fil
45、m from the rubber test strips,then place the individual rubber test strips in the mold cavitieswith the protective film side on top.8.4 Place the cords in the cord slots by cutting cord testspecimens allowing sufficient overhang for attaching massesand tie a knot in both ends. Take care to prevent t
46、he loss of cordtwist. The portion of the cord that is embedded in rubber mustnot be touched by the bare hand. Attach a 50 g mass on oneknotted end of the test cord. Two cords may be tied togetherand used to fill adjacent slots; a 100 g mass is used in this case(Fig. 4). Place one end of the knotted
47、test specimen so that itis snubbed firmly against the cord slots on one side of the mold.8.5 After all the cord slots are filled, remove the protectivefilm from the additional strips of rubber and place them in themold cavities on top of the cords. The side from which theprotective film was removed
48、will be down. Identify eachspecimen with a silver ink marking pen.8.6 Place the cover plat on the mold, then remove themasses and place the mold in a preheated press. Adjust thepressure to a minimum of 3.5 MPa (500 psi) with reference tothe mold surface. Vulcanize for the specified time at thespecif
49、ied pressure and temperature. Immediately remove themold assembly from the hot curing press.8.7 Remove mold cover plate then carefully remove theconstructed rubber and cord test pad from the test mold cavityand cool at room temperature. Condition prepared specimens at24 6 1C (75 6 2F) and 55 6 2% relative humidity for 4 hminimum, 4 days maximum, unless otherwise agreed betweenpurchaser and supplier. (Immediate testing is sometimes pre-ferred).8.8 Cut the cord test pad using shears, a sharp knife, orclicker die to produce individual H-test adhesion spec
