1、Designation: D4690 99 (Reapproved 2005) D4690 12Standard Specification forUrea-Formaldehyde Resin Adhesives1This standard is issued under the fixed designation D4690; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last
2、 revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () 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
3、urea-formaldehyde thermosetting resin adhesives suitable for use on wood,wood-based substrates, or plastic laminates.1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are provided for informationonly.1.3 The requirements for the adhesive are based
4、on tests of physical properties including viscosity, density, nonvolatile content,pH, insoluble matter, amylaceous matter, mixing properties, working life, and on strength properties, including dry shear strengthin lumber-type joints, dry and wet shear strength in plywood-type joints, and all streng
5、th tests at the end of the storage life certifiedby the manufacturer.1.4 The following safety hazards caveat pertains only to the test method portion, Sections 88 through 1113, of thisspecification:This standard does not purport to address all of the safety concerns, if any, associated with its use.
6、 It is theresponsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability ofregulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2B417 Test Method for Apparent Density of Non-Free-Flowing Metal Powders Using th
7、e Carney FunnelD905 Test Method for Strength Properties of Adhesive Bonds in Shear by Compression LoadingD906 Test Method for Strength Properties of Adhesives in Plywood Type Construction in Shear by Tension LoadingD907 Terminology of AdhesivesD1084 Test Methods for Viscosity of AdhesivesD1489 Test
8、Method for Nonvolatile Content of Aqueous AdhesivesD1490 Test Method for Nonvolatile Content of Urea-Formaldehyde Resin SolutionsD1583 Test Method for Hydrogen Ion Concentration of Dry Adhesive FilmsD1875 Test Method for Density of Adhesives in Fluid FormD2556 Test Method for Apparent Viscosity of A
9、dhesives Having Shear-Rate-Dependent Flow PropertiesD5266 Practice for Estimating the Percentage of Wood Failure in Adhesive Bonded JointsE70 Test Method for pH of Aqueous Solutions With the Glass ElectrodeE104 Practice for Maintaining Constant Relative Humidity by Means of Aqueous Solutions2.2 Fede
10、ral Specifications:3PPP-C-96 Cans, Metal, 28 Gage and LighterPPP-D-723 Drums, FiberPPP-D-729 Drums, Shipping and Storage, Steel, 55-gal(208-L)1 This specification is under the jurisdiction of ASTM Committee D14 on Adhesives and is the direct responsibility of Subcommittee D14.30 on Wood Adhesives.Cu
11、rrent edition approved April 1, 2005Oct. 1, 2012. Published April 2005October 2012. Originally approved in 1987. Last previous edition approved in 19992005 asD4690 99.D4690 99 (2005). DOI: 10.1520/D4690-99R05.10.1520/D4690-12.This specification is intended as a replacement for Federal Specification
12、MMM-A-188c, Adhesive; Urea Resin Type (Liquid and Powder).2 For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.
13、3 Available from Standardization Documents Order Desk, DODSSP, Bldg. 4, Section D, 700 Robbins Ave., Philadelphia, PA 19111-5098, http:/dodssp.daps.dla.mil.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made
14、to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.Copyri
15、ght ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States12.3 Federal Standard:3FED-STD-123 Marking for Shipment2.4 Military Standard:3MIL-STD-129 Marking for Shipment and Storage3. Terminology3.1 DefinitionsMany terms in this specification are defin
16、ed in Terminology D907.3.2 Definitions of Terms Specific to This Standard:3.2.1 adhesive designationan adhesive that is manufactured by a unique combination of raw materials and manufacturingprocess that conforms to a given set of physical and performance properties and is identified by specific nam
17、e, number, oralphanumeric designation.3.2.1 lotadhesive manufactured at one place from the same batch or blends of raw materials subjected to the same operationsand conditions.NOTE 1In this specification, the maple block lamination in Test Method D905 and the birch plywood construction in Test Metho
18、d D906 are describedas assemblies.4. Significance and Use4.1 This specification provides testing procedures and specifies requirements to differentiate between the physical and adhesivebonding properties of the many commercial urea-formaldehyde thermosetting resin and catalyst systems.4.2 Because of
19、 the diverse nature of products bonded with these adhesives, testing by this specification will only evaluate theadhesive under a given set of conditions. The physical properties of the adhesive are measured to provide information on certainhandling and working properties. The adhesive-bonding prope
20、rties are measured on maple block and birch plywood specimens,prepared and tested in accordance with Test Method D905 and Test Method D906, respectively. The certification requirements havebeen based on knowledge within the industry of values that may be expected. Test Method D905 and Test Method D9
21、06 have along history of use in many specifications.4.3 The stress calculated by using this specification should not be used to predict failure nor should it be used for design stressin joints with different geometry or loading direction different from the test geometry.5. Classification5.1 Urea res
22、in adhesive shall be furnished as one of the following 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 Type III classifications of Fed
23、eral Specification MMM-A-188C, respectively,to prevent confusion with Type I (boil test) and Type II (cold-water soak) classifications used in existing ASTM standards for adhesives.6. Test Requirements6.1 To meet the requirements of this specification, the urea resin and adhesive mix shall be subjec
24、ted to the tests listed in Section10. In addition, the adhesive shall meet the requirements of the tests described in Section 11 and as listed in Table 1.6.2 To meet the storage-life requirements, an initial lot of the adhesive shall be tested in accordance with Sections 10 and 11.It shall pass all
25、test requirements after being stored under conditions and time specified by the manufacturer. Following this initialtest, certification shall be based on submission from the manufacturer.TABLE 1 Test RequirementsTest Section Number Test Requirement(Minimum)Block shear (compression)Dry at 24C (75F) 1
26、1.1 19 306 kPa (2800 psi)Dry at 24C (75F) 11.1 19 306 kPa (2800 psi)Plywood shear (tension)Dry at 24C (75F) 11.2.3.1 2 344 kPa (340 psi)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)48-h soak 11.2.3.2 1 930 kPa (280 psi)Storage life 11.2.3.3 AStorage life 11.2.3.
27、3 AA A 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 type of adhesive afterthe storage life time certified by the manufacturer.D4690 1226.3 The curing agent for Types A and C shall readily disperse in t
28、he adhesive mixture when used in accordance with themanufacturers recommendation.6.4 The filler shall neither dissolve nor swell excessively in water, 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 speci
29、fied, if the wood failure is 50 % or greater, that specimen shall bedisregarded in computing the average. If more than one third of the test specimens for any one test condition are discarded for thisreason, the test shall be repeated.7.2 If the results of any initial test do not conform to the requ
30、irements prescribed in this specification, that test shall be repeatedon an additional set of specimens made from the same lot of adhesive, each set of which shall conform to the requirementsspecified. If this set of specimens fails to meet the requirements, the lot shall be rejected.TEST METHODS8.
31、Significance and Use8.1 This specification provides testing procedures to differentiate between the physical and adhesive bonding properties of themany commercial urea-formaldehyde thermosetting resin and catalyst systems.9. Sampling9.1 Take a representative, 2-L (2-qt) sample of adhesive from the l
32、ot to be tested. Divide the sample into two equal portionsand place each in a wide mouth, glass, 1-L (1-qt) container and seal tightly. Use one of the samples for tests of physical andadhesive bond properties (Sections 10 and 11), and use the other for testing storage life (11.2.3.3), and for any re
33、testing that maybe necessary under Section 7. Also, take sufficient quantity of curing agent to cure the adhesive samples and place in a separate,clean, dry container. Seal all sample containers with well-fitting, corrosion-resistant lids.10. Physical Properties10.1 Test the physical properties of a
34、dhesives by the following test methods:10.1.1 Viscosity:10.1.1.1 Measure the viscosity of the liquid urea resin or adhesive mixtures in accordance with Test Methods D1084 or D2556.10.1.1.2 Temperature of TestCondition to, and maintain the liquid urea resin or adhesive mixture at 24 6 0.5C (75 6 1F)d
35、uring the viscosity reading. Other temperatures may be used upon agreement between the contracting parties, but the 60.5C(61F) tolerance must be observed.10.1.1.3 For Type C adhesives requiring the addition of a curing agent, make two viscosity measurements of the test adhesives(1) before the additi
36、on of curing agent, and (2) after the addition of the curing agent. The viscosity of urea resins following additionof curing agent to liquid resin is time-dependent. Make the measurement 10 min after mixing.10.1.2 Density:10.1.2.1 Measure the density of dry-powder adhesives or separate curing agents
37、 in accordance with Test Method B417, andreport in grams per cubic centimetre (pounds per cubic foot). (See Appendix X1.)10.1.2.2 Measure the density of Type C adhesives in accordance with Test Method D1875 and report in grams per millilitre(pounds per gallon).10.1.3 Nonvolatiles:10.1.3.1 Determine
38、the nonvolatile content of Type A and Type B from a 100-g mixture of adhesive and water (prepared bymanufacturers instructions) and test in accordance with Test Method D1490.10.1.3.2 Determine the nonvolatile content of the uncatalyzed Type C liquid adhesive in accordance with Test Method D1490.10.1
39、.4 pH of Cured Adhesive FilmDetermine the pH of the cured adhesive film in accordance with Test Method D1583.10.1.5 Insoluble MatterDetermine the quantity of insoluble matter in Type B adhesives, including filler and any insolublematerial, as a percentage of the nonvolatile constituents of the adhes
40、ive when determined as specified in 10.1.3.1. Weigh to thenearest milligram approximately 2 g of freshly mixed adhesive in a 100-mL beaker and add 50 mL of cold solution of 20 partsby volume of glacial acetic acid and 80 parts by volume of distilled water. Stir the mixture thoroughly for 1 min and t
41、hen add 0.5006 0.001 g, acid-washed diatomaceous earth (see Note 6). Stir the mixture for 2 min more and then filter through a fritted-glasscrucible of medium porosity with the aid of a vacuum. Transfer all residue to the filter with a 20 % acetic acid solution. Wash theresidue on the filter with at
42、 least 50 mL of 20 % acetic acid and then with cold distilled water to remove the acid. Dry the cruciblein an oven at 124 6 3C (255 6 5C) for 1 to 112 h, cool in a desiccator, and weigh to the nearest milligram. The insoluble content,as a percentage of the nonvolatile content, is determined as follo
43、ws:Percent insoluble5Weight of residue20.500! (1)3100/Weight of adhesive3percent nonvolatile!D4690 123NOTE 3“Filter-61” and “Celite Analytical Filter-Aid” have been found satisfactory. Diatomaceous earth is prepared by acid-wash, oven dried at 1246 3F (155 6 5C) and then cooled in a desiccator.10.1.
44、6 Amylaceous Matter in Type B AdhesiveAdd a drop of solution made from 5 g of iodine, 5 g of potassium iodide, and100 mL of distilled water, to approximately 0.5 g of adhesive mix on a porcelain spot plate or watch glass. A darkening of themixture denotes the presence of amylaceous matter.10.1.7 Mix
45、ing Properties and Working Life, Mix approximately 200 g of adhesive (in accordance with the manufacturersinstruction) in a 400-mL beaker (Note 6) with a stirring rod or blade. Allow the beaker to stand without a cover in air at 24 6 2.5C(75 6 5F). If necessary, place in a water bath to obtain the p
46、roper temperature. Stir the adhesive frequently and note the time atwhich the adhesive is considered no longer spreadable. At the end of the working life, note whether the adhesive is in ahomogeneous condition. In case of doubt as to whether the adhesive is spreadable, test the adhesive at 24 6 2.5C
47、 (75 6 5F)using a Brookfield Viscometer. Consider the adhesive to be at the end of its working life when it reaches a viscosity of 600 P (0.6Pas). If the temperature of the bonding operation is 32.2C (90F) or higher, the above test may be conducted at 32.2C (90F).NOTE 4A disposable beaker or a 473-m
48、L (16-oz) plastic cup may be used.11. Adhesive-Bonding Properties11.1 Block-Shear Strength (Compression) Tests:11.1.1 Prepare and test specimens in accordance with Test Method D905. Use the adhesive manufacturers instructions forconditions and procedures for preparing and spreading the adhesive, and
49、 assembling, pressing, and curing of the assembly. Usea two-week curing period unless otherwise instructed by the adhesive manufacturer.11.1.2 Number of SpecimensTest 20 specimens representing at least four assemblies.11.1.3 Dry Shear TestCondition one test group of 20 specimens to 10 to 12 % moisture content at 24 6 1C (75 6 2F) andtest in accordance with Test Method D905. Apply the load with a continuous motion of the movable loading head at a rate of 12.7mm (0.5 in.)/min (610 %).NOTE 5To obtain the desired moisture conten
