1、Designation: D4689 99 (Reapproved 2005) D4689 12Standard Specification forAdhesive, Casein-Type1This standard is issued under the fixed designation D4689; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A
2、 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 casein and other protein-bl
3、end adhesives for use adhering wood to wood. The adhesive typecovered by this specification is a dry powder or granular product comprising a mixture of casein, or casein and other protein source,with the necessary dry chemicals to effect solution when the mixture is added to water.NOTE 1Although the
4、 term casein adhesive is used throughout this specification, historically, the adhesive subclass described in 1.1 has been knownas casein glue. See Terminology D907, adhesive types.1.2 LimitationsCooked casein adhesives are not covered by this specification.1.3 The values stated in inch-pound units
5、are to be regarded as standard. The values given in parentheses are mathematicalconversions to SI units that are provided for information only and are not considered standard.1.4 The following safety hazards caveat pertains only to the test method portion, Sections 88 through 1316, of thisspecificat
6、ion:This standard does not purport to address all of the safety concerns, if any, associated with its use. 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 Doc
7、uments2.1 ASTM Standards:2D899 Practice for Applied Weight Per Unit Area of Liquid AdhesiveD905 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 Term
8、inology of AdhesivesD1084 Test Methods for Viscosity of AdhesivesD2556 Test Method for Apparent Viscosity of Adhesives Having Shear-Rate-Dependent Flow PropertiesD5266 Practice for Estimating the Percentage of Wood Failure in Adhesive Bonded JointsE104 Practice for Maintaining Constant Relative Humi
9、dity by Means of Aqueous Solutions2.2 Other Standards:3MIL-STD-129MarkingMIL-STD-129 Marking for Shipment and StorageFED-STD-123Marking FED-STD-123 Marking for ShipmentPPP-C-96Cans,PPP-C-96 Cans, Metal, 28 Gage and LighterPPP-D-723Drums,PPP-D-723 Drums, FiberPPP-D-729Drums,PPP-D-729 Drums, Shipping
10、and Storage, Steel, 55 Gal(208 L)3. Terminology3.1 DefinitionsMany terms in this specification are defined in Terminology D907.3.1 DefinitionsMany terms in this specification are defined in Terminology D907.1 This specification is under the jurisdiction of ASTM Committee D14 on Adhesives and is the
11、direct responsibility of Subcommittee D14.30 on Wood Adhesives.Current edition approved April 1, 2005Oct. 1, 2012. Published May 2005October 2012. Originally approved in 1987. Last previous edition approved in 19992005 asD4689 99.D4689 99 (2005). DOI: 10.1520/D4689-99R05.10.1520/D4689-12.2 For refer
12、enced 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.3 Available from Standardization Documents Order Desk, DODSSP, Bldg.
13、4, Section D, 700 Robbins Ave., Philadelphia, PA 19111-5098.19111-5098, 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 to the previous version. Becauseit may not be technically
14、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.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700
15、, West Conshohocken, PA 19428-2959. United States13.2 Definitions of Terms Specific to This Standard:3.2.1 adhesive designation, nan 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
16、 is identified by a specific name, number, oralphanumeric designation.3.2.1 lot, nadhesive manufactured at one place from the same batch or blends of raw materials subjected to the same operationand conditions.NOTE 2In this specification, the maple block lamination in Test Method D905 and the birch
17、plywood construction in Test Method D906 are describedas assemblies.4. Significance and Use4.1 This specification provides testing procedures and specifies requirements to differentiate the physical, adhesive, anddurability properties of commercially available casein and casein-protein adhesives. Th
18、e two classes are defined by waterresistance. Selection of class is left to the choice of the product manufacturer and the consumer, based on measures used by eachto protect the bond line from moisture degradation.D4689 122NOTE 3Because of strict EPA requirements as to disposal of waste from manufac
19、turing and production facilities, it has become necessary for morethan a decade to remove biocides most if not all biocides were removed from casein adhesives. Paint, varnish, and restrictive exposure conditions areprotective measures commonly employed now to protect the bond line against degradatio
20、n due to mold and moisture.4.2 The stress calculated by this specification should not be used to predict failure, nor should it be used directly for design stressin joints with different geometry or with loading direction different from the test geometry.5. Classification5.1 For purposes of this spe
21、cification, adhesives are classified on the basis of water resistance at two performance levels:5.1.1 Class B, Water ResistantAn adhesive passing Class B test requirements, as listed in Table 1, is capable of producingsufficient adhesive-joint strength and durability and has sufficient water resista
22、nce to make the bonded products serviceable underconditions in which there will be occasional intermittent exposure to wet conditions or high humidity.5.1.2 Class C, Dry UseAn adhesive passing Class C test requirements, as listed in Table 1, has sufficient adhesive-jointstrength and durability under
23、 normal interior service conditions where the relative humidity is not high and does not fluctuatebetween wide limits.6. Test Requirements6.1 The test adhesives, when tested in accordance with Section 11, shall remain in the viscosity range of 3000 to 15 000 cP fora working life of at least 5 h, min
24、imum.NOTE 4The viscosity requirement covers a 5-h span, although the “end-of-working-life” adhesive bond strength test is run at 4 h. This apparentconflict is necessary in order to assure that the mixed casein adhesive is not in a rapidly rising viscosity pattern at the end of the working life.6.1.1
25、 The working life shall be timed from the addition of the adhesive powder to the water.6.1.2 The viscosity requirements shall not apply until the casein has dissolved and the adhesive is ready for use.NOTE 5Unless the manufacturer instructs otherwise, 20 min is the typical time period required, afte
26、r the adhesive powder is added to the water, beforethe adhesive is ready for use.6.2 To meet the adhesive bond requirements of the specification, the test adhesive shall be subjected to the tests described inSection 12 and shall meet the requirements listed on Table 1.6.2.1 Two sets of adhesive bond
27、 tests are required, one to be initiated 1 h after mixing the adhesive with water, and one 4 hafter mixing.6.3 To meet the storage-life requirements, an initial lot of the adhesive shall be tested following the manufacturers certifiedstorage life, and shall pass all test requirements for the applica
28、ble adhesive classification. Following this initial test, certificationfor this requirement shall be based on submission from the manufacturer.7. Retest and Rejection7.1 When a specimen fails at a load less than that specified and the wood failure is at least 50 %, that specimen shall bedisregarded
29、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.TABLE 1 Test RequirementsTest Section Number Minimum TestRequirement Test RequiredClass B Class CWorking life 6.1 5 h yes yesWorking life 6.1 5 h
30、 yes yesViscosity at 77 0.5F(25 0.25C)6.1 3000 to 15 000 cp yes yesViscosity at 77 0.5F(25 0.25C)6.1 3000 to 15 000 cp yes yesBlock shear (compression)Dry at 1 and 4 h 12.1 2800 psi (19 306 kPa) yes yesDry at 1 and 4 h 12.1 2800 psi (19 306 kPa) yes yesPlywood (tension) 12.2 340 psi (2344 kPa) yes y
31、esPlywood (tension) 12.2 340 psi (2344 kPa) yes yesDry at 1 and 4 hA 12.2.3.1Dry at 1 and 4 hA 12.2.3.1Soak, 48-h at 1 and 4 hA 12.2.3.2 140 psi (965 kPa) yes noSoak, 48-h at 1 and 4 hA 12.2.3.2 140 psi (965 kPa) yes noStorage life 14. B yes yesStorage life 14 B yes yesA One and four hours refers to
32、 age of adhesive after mix. See 6.2.1.B A lot of the designated adhesive shall be tested for all the required tests after aging for the desired storage life time. The longest shelf life tested which passes all theminimum requirements shall be the storage life certified by the manufacturer.D4689 1237
33、.2 If the results of any initial test do not conform to the requirements prescribed in this specification, that test shall be repeatedon an additional set of specimens made from the same lot of adhesive, each of which shall conform to the requirements specified.If this set of specimens fails to meet
34、 the requirements, the lot shall be rejected.TEST METHODS8. Significance and Use8.1 This specification provides testing procedures to differentiate the physical, adhesive, and durability properties ofcommercially available casein and casein-protein adhesives.9. Apparatus9.1 Mechanical Stirrer or Mix
35、er, capable of speed in air of 5000 r/min for the preparation of the adhesive mix.49.2 Other apparatus required to conduct tests are covered in Practice D899, and Test Methods D905, D906, D1084 and D2556.10. Sampling10.1 Take a 5-lb (2.3-kg) representative sample of the adhesive from the lot to be t
36、ested. Store samples in airtight containersand seal. For the initial testing of storage life only (6.4), divide the sample into two equal portions, packed as directed above. Useone portion for immediate testing and reserve the other for testing at the end of storage life.11. Working Life11.1 Prepare
37、 the adhesive for use in accordance with the manufacturers instructions. Measure the time from the introductionof the powder into the water, and determine viscosity in a 400-mL beaker at 20 min and at 1, 2, 3, 4, and 5 h, in accordance withTest Methods D1084, Method B, with the following modificatio
38、ns:11.1.1 Keep the adhesive at 77 6 1F (25 6 0.5C) for the duration of the test for working life.11.1.2 Stir the adhesive with a mechanical stirrer for 1 min immediately before measuring the viscosity.11.1.3 Allow the viscometer spindle to rotate for 30 s before recording the dial reading.11.1.4 Usi
39、ng standard procedure for mixing a casein adhesive for testing, introduce the powder into the water with mechanicalagitation, and continue the agitation for 1 min after the powder is dispersed. Turn off the mixer for approximately 15 to 20 min,depending on the manufacturers instructions. Before the
40、viscosity reading is taken, turn the mixer on again for 1 min. Then takethe reading promptly.11.1.5 Other temperatures may be used upon agreement between the contracting parties, but the 61F (60.5C) tolerance mustbe observed.NOTE 6Casein adhesives develop an exothermic reaction when added to water,
41、so the water temperature must be 5 to 10F (2.8 to 5.5C) lower thanthe desired temperature of the liquid adhesive.NOTE 7Although casein adhesives and especially casein-soy blend adhesives have somewhat shear-rate-dependent flow properties, Test MethodsD1084, Method B, is referenced for viscosity dete
42、rminations rather than Test Method D2556. The 1-min mixing time prior to reading a viscosity servesto break down the apparent viscosity build-up as the glue mix rests between readings. When more information is needed on the shear-rate-dependent flowproperties of the adhesive, test the mix by Test Me
43、thod D2556.12. Tests for Adhesive Bond12.1 Block Shear Strength (Compression):12.1.1 Prepare the specimens in accordance with Test Method D905, using the adhesive manufacturers instructions.12.1.1.1 In the absence of specific instructions, use a spread rate of 60 lb/1000 ft2 (0.19 g/in.2) of bond li
44、ne (see Practice D899).The mixed metric/English system has been deliberately used, since it is a standard in the industry for spread rate. Use 1 to 2-minopen assembly (time required to apply adhesive), 15-min closed assembly, 200 psi (1379 kPa) pressure, 2-h press time, and a1-week conditioning peri
45、od.12.1.2 Number of SpecimensTest 20 specimens representing at least four assemblies.12.1.3 Dry TestFollowing the prescribed conditioning period for the adhesive being tested, bring one test group of 20specimens to 10 to 12 % moisture content and test in accordance with the instructions in Test Meth
46、od D905. Apply the load througha self-aligning seal to ensure uniform lateral distribution of the load. Apply the load with a continuous motion of the movableloading head at a rate of 0.5 in. (12.7 mm)/min (610 %).NOTE 8To obtain the desired moisture content refer to Table 34 on page 37 of the Wood
47、Handbook.5 Additional information is available in PracticeE104. Constant temperature and relative humidity cabinets are available from laboratory supply companies.4 Satisfactory mixing may be obtained using the intermediate speed of the Thomas Three-Speed Stirrer No. 8585-M10 used with the stirring
48、shaft, AHT No. 8633-T10,9 in. (23 cm) long, and 1.5-in. (38-mm) diameter, four-blade propeller. Available from Thomas Scientific, Swedesboro, NJ 08085-0099, and other locations. Many otherlaboratory supply houses can provide this same mixer or its equivalent.5 Wood Handbook, Wood as an Engineering M
49、aterial, FPL-GTR-113, Forest Products Laboratory, United States Dept. of Agriculture, “Moisture Content of Wood inEquilibrium with Stated Dry-Bulb Temperature and Relative Humidity,” revised 1999, Table 34, pp. 37.D4689 12412.1.4 CalculationCalculate the shear stress at failure in pounds per square inch or kilopascals, based on the specimensbreaking load and tested bond-line area, measured to the nearest 0.10 in.2 (6.5 mm2).12.2 Plywood Shear Tests:12.2.1 Prepare the specimens in accordance with Test Method D906, using the ad
