1、Designation: D 4690 99 (Reapproved 2005)Standard Specification forUrea-Formaldehyde Resin Adhesives1This standard is issued under the fixed designation D 4690; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revisi
2、on. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1 This specification covers three types of urea-f
3、ormaldehyde thermosetting resin adhesives suitable for use onwood, wood-based substrates, or plastic laminates.1.2 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are provided forinformation only.1.3 The requirements for the adhesive are based on test
4、s ofphysical properties including viscosity, density, nonvolatilecontent, pH, insoluble matter, amylaceous matter, mixingproperties, working life, and on strength properties, includingdry shear strength in lumber-type joints, dry and wet shearstrength in plywood-type joints, and all strength tests a
5、t the endof the storage life certified by the manufacturer.1.4 The following safety hazards caveat pertains only to thetest method portion, Sections 8 through 13, of this specifica-tion: This standard does not purport to address all of the safetyconcerns, if any, associated with its use. It is the r
6、esponsibilityof the user of this standard to establish appropriate safety andhealth practices and determine the applicability of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:2B 417 Test Method for Apparent Density of Non-Free-Flowing Metal Powders Using the Carney Fun
7、nelD 905 Test Method for Strength Properties of AdhesiveBonds in Shear by Compression LoadingD 906 Test Method for Strength Properties of Adhesives inPlywood Type Construction in Shear by Tension LoadingD 907 Terminology of AdhesivesD 1084 Test Methods for Viscosity of AdhesivesD 1489 Test Method fo
8、r Nonvolatile Content of AqueousAdhesivesD 1490 Test Method for Nonvolatile Content of Urea-Formaldehyde Resin SolutionsD 1583 Test Method for Hydrogen Ion Concentration ofDry Adhesive FilmsD 1875 Test Method for Density of Adhesives in FluidFormD 2556 Test Method for Apparent Viscosity of Adhesives
9、Having Shear-Rate-Dependent Flow PropertiesD 5266 Practice for Estimating the Percentage of WoodFailure in Adhesive Bonded JointsE 70 Test Method for pH of Aqueous Solutions with theGlass ElectrodeE 104 Practice for Maintaining Constant Relative Humidityby Means of Aqueous Solutions2.2 Federal Speci
10、fications:3PPP-C-96 Cans, Metal, 28 Gage and LighterPPP-D-723 Drums, FiberPPP-D-729 Drums, Shipping and Storage, Steel, 55-gal(208-L)2.3 Federal Standard:3FED-STD-123 Marking for Shipment2.4 Military Standard:3MIL-STD-129 Marking for Shipment and Storage3. Terminology3.1 DefinitionsMany terms in thi
11、s specification are de-fined in Terminology D 907.3.2 Definitions of Terms Specific to This Standard:3.2.1 adhesive designationan adhesive that is manufac-tured by a unique combination of raw materials and manufac-turing process that conforms to a given set of physical andperformance properties and
12、is identified by specific name,number, or alphanumeric designation.3.2.2 lotadhesive manufactured at one place from thesame batch or blends of raw materials subjected to the sameoperations and conditions.NOTE 1In this specification, the maple block lamination in Test1This specification is under the
13、jurisdiction of ASTM Committee D14 onAdhesives and is the direct responsibility of Subcommittee D14.30 on WoodAdhesives.Current edition approved April 1, 2005. Published April 2005. Originallyapproved in 1987. Last previous edition approved in 1999 as D 4690 99.This specification is intended as a re
14、placement for Federal SpecificationMMM-A-188c, Adhesive; Urea Resin Type (Liquid and Powder).2For referenced ASTM standards, visit 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
15、Summary page onthe ASTM website.3Available from Standardization Documents Order Desk, DODSSP, Bldg. 4,Section D, 700 Robbins Ave., Philadelphia, PA 19111-50981Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.Method D 905 and the birch
16、plywood construction in Test Method D 906are described as assemblies.4. Significance and Use4.1 This specification provides testing procedures and speci-fies requirements to differentiate between the physical andadhesive bonding properties of the many commercial urea-formaldehyde thermosetting resin
17、 and catalyst systems.4.2 Because of the diverse nature of products bonded withthese adhesives, testing by this specification will only evaluatethe adhesive under a given set of conditions. The physicalproperties of the adhesive are measured to provide informationon certain handling and working prop
18、erties. The adhesive-bonding properties are measured on maple block and birchplywood specimens, prepared and tested in accordance withTest Method D 905 and Test Method D 906, respectively. Thecertification requirements have been based on knowledgewithin the industry of values that may be expected. T
19、estMethod D 905 and Test Method D 906 have a long history ofuse in many specifications.4.3 The stress calculated by using this specification shouldnot be used to predict failure nor should it be used for designstress in joints with different geometry or loading directiondifferent from the test geome
20、try.5. Classification5.1 Urea resin adhesive shall be furnished as one of thefollowing types:5.1.1 Type APowder with separate curing agent.5.1.2 Type BPowder with incorporated curing agent.5.1.3 Type CLiquid with separate curing agent.NOTE 2Type A, Type B, and Type C replace the Type I, Type II, and
21、Type III classifications of Federal Specification MMM-A-188C, respec-tively, to prevent confusion with Type I (boil test) and Type II (cold-watersoak) classifications used in existing ASTM standards for adhesives.6. Test Requirements6.1 To meet the requirements of this specification, the urearesin a
22、nd adhesive mix shall be subjected to the tests listed inSection 10. In addition, the adhesive shall meet the require-ments of the tests described in Section 11 and as listed in Table1.6.2 To meet the storage-life requirements, an initial lot ofthe adhesive shall be tested in accordance with Section
23、s 10 and11. It shall pass all test requirements after being stored underconditions and time specified by the manufacturer. Followingthis initial test, certification shall be based on submission fromthe manufacturer.6.3 The curing agent for Types A and C shall readilydisperse in the adhesive mixture
24、when used in accordance withthe manufacturers recommendation.6.4 The filler shall neither dissolve nor swell excessively inwater, and shall not settle from the adhesive mixture during theworking life.7. Retest and Rejection7.1 When a specimen fails at a load less than that specified,if the wood fail
25、ure is 50 % or greater, that specimen shall bedisregarded in computing the average. If more than one third ofthe test specimens for any one test condition are discarded forthis reason, the test shall be repeated.7.2 If the results of any initial test do not conform to therequirements prescribed in t
26、his specification, that test shall berepeated on an additional set of specimens made from the samelot of adhesive, each set of which shall conform to therequirements specified. If this set of specimens fails to meet therequirements, the lot shall be rejected.TEST METHODS8. Significance and Use8.1 Th
27、is specification provides testing procedures to differ-entiate between the physical and adhesive bonding propertiesof the many commercial urea-formaldehyde thermosettingresin and catalyst systems.9. Sampling9.1 Take a representative, 2-L (2-qt) sample of adhesivefrom the lot to be tested. Divide the
28、 sample into two equalportions and place each in a wide mouth, glass, 1-L (1-qt)container and seal tightly. Use one of the samples for tests ofphysical and adhesive bond properties (Sections 10 and 11),and use the other for testing storage life (11.2.3.3), and for anyretesting that may be necessary
29、under Section 7. Also, takesufficient quantity of curing agent to cure the adhesive samplesand place in a separate, clean, dry container. Seal all samplecontainers with well-fitting, corrosion-resistant lids.10. Physical Properties10.1 Test the physical properties of adhesives by the fol-lowing test
30、 methods:10.1.1 Viscosity:10.1.1.1 Measure the viscosity of the liquid urea resin oradhesive mixtures in accordance with Test Methods D 1084 orD 2556.10.1.1.2 Temperature of TestCondition to, and maintainthe liquid urea resin or adhesive mixture at 24 6 0.5C (75 61F) during the viscosity reading. Ot
31、her temperatures may beused upon agreement between the contracting parties, but the60.5C (61F) tolerance must be observed.10.1.1.3 For Type C adhesives requiring the addition of acuring agent, make two viscosity measurements of the testadhesives (1) before the addition of curing agent, and (2) after
32、the addition of the curing agent. The viscosity of urea resinsfollowing addition of curing agent to liquid resin is time-dependent. Make the measurement 10 min after mixing.10.1.2 Density:TABLE 1 Test RequirementsTest Section NumberTest Requirement(Minimum)Block shear (compression)Dry at 24C (75F) 1
33、1.1 19 306 kPa (2800 psi)Plywood shear (tension)Dry at 24C (75F) 11.2.3.1 2 344 kPa (340 psi)48-h soak 11.2.3.2 1 930 kPa (280 psi)Storage life 11.2.3.3AAA retained sample of the initial lot of the adhesive shall be tested and shall meetthe requirements of all tests listed in 6.2 for the applicable
34、type of adhesive afterthe storage life time certified by the manufacturer.D 4690 99 (2005)210.1.2.1 Measure the density of dry-powder adhesives orseparate curing agents in accordance with Test Method B 417,and report in grams per cubic centimetre (pounds per cubicfoot). (See Appendix X1.)10.1.2.2 Me
35、asure the density of Type C adhesives in accor-dance with Test Method D 1875 and report in grams permillilitre (pounds per gallon).10.1.3 Nonvolatiles:10.1.3.1 Determine the nonvolatile content of Type A andType B from a 100-g mixture of adhesive and water (preparedby manufacturers instructions) and
36、 test in accordance withTest Method D 1490.10.1.3.2 Determine the nonvolatile content of the uncata-lyzed Type C liquid adhesive in accordance with Test MethodD 1490.10.1.4 pH of Cured Adhesive FilmDetermine the pH ofthe cured adhesive film in accordance with Test MethodD 1583.10.1.5 Insoluble Matte
37、rDetermine the quantity of in-soluble matter in Type B adhesives, including filler and anyinsoluble material, as a percentage of the nonvolatile constitu-ents of the adhesive when determined as specified in 10.1.3.1.Weigh to the nearest milligram approximately2goffreshlymixed adhesive in a 100-mL be
38、aker and add 50 mL of coldsolution of 20 parts by volume of glacial acetic acid and 80parts by volume of distilled water. Stir the mixture thoroughlyfor 1 min and then add 0.500 6 0.001 g, acid-washeddiatomaceous earth (see Note 6). Stir the mixture for 2 minmore and then filter through a fritted-gl
39、ass crucible of mediumporosity with the aid of a vacuum. Transfer all residue to thefilter with a 20 % acetic acid solution. Wash the residue on thefilter with at least 50 mL of 20 % acetic acid and then with colddistilled water to remove the acid. Dry the crucible in an ovenat 124 6 3C (255 6 5C) f
40、or 1 to 112 h, cool in a desiccator,and weigh to the nearest milligram. The insoluble content, as apercentage of the nonvolatile content, is determined as follows:Percent insoluble 5 Weight of residue 2 0.500!3 100/Weight of adhesive 3 percent nonvolatile!(1)NOTE 3“Filter-61” and “Celite Analytical
41、Filter-Aid” have beenfound satisfactory. Diatomaceous earth is prepared by acid-wash, ovendried at 124 6 3F (155 6 5C) and then cooled in a desiccator.10.1.6 Amylaceous Matter in Type B AdhesiveAdd a dropof solution made from5gofiodine,5gofpotassium iodide,and 100 mL of distilled water, to approxima
42、tely 0.5 g ofadhesive mix on a porcelain spot plate or watch glass. Adarkening of the mixture denotes the presence of amylaceousmatter.10.1.7 Mixing Properties and Working Life, Mix approxi-mately 200 g of adhesive (in accordance with the manufactur-ers instruction) in a 400-mLbeaker (Note 6) with a
43、 stirring rodor blade. Allow the beaker to stand without a cover in air at 246 2.5C (75 6 5F). If necessary, place in a water bath toobtain the proper temperature. Stir the adhesive frequently andnote the time at which the adhesive is considered no longerspreadable. At the end of the working life, n
44、ote whether theadhesive is in a homogeneous condition. In case of doubt as towhether the adhesive is spreadable, test the adhesive at 24 62.5C (75 6 5F) using a Brookfield Viscometer. Consider theadhesive to be at the end of its working life when it reaches aviscosity of 600 P (0.6 Pas). If the temp
45、erature of the bondingoperation is 32.2C (90F) or higher, the above test may beconducted at 32.2C (90F).NOTE 4A disposable beaker or a 473-mL (16-oz) plastic cup may beused.11. Adhesive-Bonding Properties11.1 Block-Shear Strength (Compression) Tests:11.1.1 Prepare and test specimens in accordance wi
46、th TestMethod D 905. Use the adhesive manufacturers instructionsfor conditions and procedures for preparing and spreading theadhesive, and assembling, pressing, and curing of the assem-bly. Use a two-week curing period unless otherwise instructedby the adhesive manufacturer.11.1.2 Number of Specimen
47、sTest 20 specimens represent-ing at least four assemblies.11.1.3 Dry Shear TestCondition one test group of 20specimens to 10 to 12 % moisture content at 24 6 1C (75 62F) and test in accordance with Test Method D 905.Apply theload with a continuous motion of the movable loading head ata rate of 12.7
48、mm (0.5 in.)/min (610 %).NOTE 5To obtain the desired moisture content refer to Table 3-4 onpage 3-8 of the Wood Handbook.4Additional information is available inPractice E 104. Constant temperature and relative humidity cabinets areavailable from laboratory supply companies.11.1.4 CalculationCalculat
49、e the shear stress at failure inkilopascals per square inch by dividing the specimens break-ing load by bond line area measured to the nearest 6.5mm2(0.01 in.2).11.2 Plywood Shear Tests (Tension):11.2.1 Prepare and test specimens in accordance with TestMethod D 906. Use the adhesive manufacturers instructionsfor conditions and procedures for preparing and spreading theadhesive, and for assembling, pressing, and curing of theassembly. Use a two-week conditioning period unless other-wise instructed by the adhesive manufacturer.11.2.2 Nu
