1、Designation: D 4689 99 (Reapproved 2005)Standard Specification forAdhesive, Casein-Type1This standard is issued under the fixed designation D 4689; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A number
2、 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 casein and other protein-blendadh
3、esives for use adhering wood to wood. The adhesive typecovered by this specification is a dry powder or granularproduct comprising a mixture of casein, or casein and otherprotein source, with the necessary dry chemicals to effectsolution when the mixture is added to water.NOTE 1Although the term cas
4、ein adhesive is used throughout thisspecification, historically, the adhesive subclass described in 1.1 has beenknown as casein glue. See Terminology D 907, adhesive types.1.2 LimitationsCooked casein adhesives are not coveredby this specification.1.3 The values stated in inch-pound units are to be
5、regardedas standard. The values given in parentheses are mathematicalconversions to SI units that are provided for information onlyand are not considered standard.1.4 The following safety hazards caveat pertains only to thetest method portion, Sections 8 through 16, of this specifica-tion: This stan
6、dard does not purport to address all of the safetyconcerns, if any, associated with its use. It is the responsibilityof 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
7、Standards:2D 899 Practice for Applied Weight per Unit Area of LiquidAdhesiveD 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 Adh
8、esivesD 1084 Test Methods for Viscosity of AdhesivesD 2556 Test Method for Apparent Viscosity of AdhesivesHaving Shear-Rate-Dependent Flow PropertiesD 5266 Practice for Estimating the Percentage of WoodFailure in Adhesive Bonded JointsE 104 Practice for Maintaining Constant Relative Humidityby Means
9、 of Aqueous Solutions2.2 Other Standards:3MIL-STD-129Marking for Shipment and StorageFED-STD-123Marking for ShipmentPPP-C-96Cans, Metal, 28 Gage and LighterPPP-D-723Drums, FiberPPP-D-729Drums, Shipping and Storage, Steel, 55 Gal(208 L)3. Terminology3.1 DefinitionsMany terms in this specification are
10、 de-fined in Terminology D 907.3.2 Definitions of Terms Specific to This Standard:3.2.1 adhesive designation, nan 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 is identified by
11、 a specific name,number, or alphanumeric designation.3.2.2 lot, nadhesive manufactured at one place from thesame batch or blends of raw materials subjected to the sameoperation and conditions.NOTE 2In this specification, the maple block lamination in TestMethod D 905 and the birch plywood constructi
12、on in Test Method D 906are described as assemblies.4. Significance and Use4.1 This specification provides testing procedures and speci-fies requirements to differentiate the physical, adhesive, anddurability properties of commercially available casein andcasein-protein adhesives. The two classes are
13、 defined by waterresistance. Selection of class is left to the choice of the productmanufacturer and the consumer, based on measures used byeach to protect the bond line from moisture degradation.NOTE 3Because of strict EPA requirements as to disposal of waste1This specification is under the jurisdi
14、ction of ASTM Committee D14 onAdhesives and is the direct responsibility of Subcommittee D14.30 on WoodAdhesives.Current edition approved April 1, 2005. Published May 2005. Originallyapproved in 1987. Last previous edition approved in 1999 as D 4689 99.2For referenced ASTM standards, visit the ASTM
15、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.3Available from Standardization Documents Order Desk, DODSSP, Bldg. 4,Section D, 700 Robbins Ave., Philadelp
16、hia, PA 19111-5098.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.from manufacturing and production facilities, it has become necessary formore than a decade to remove biocides from casein adhesives. Paint,varnish, and restrictive e
17、xposure conditions are protective measurescommonly employed to protect the bond line against degradation due tomold and moisture.4.2 The stress calculated by this specification should not beused to predict failure, nor should it be used directly for designstress in joints with different geometry or
18、with loading direc-tion different from the test geometry.5. Classification5.1 For purposes of this specification, adhesives are classi-fied on the basis of water resistance at two performance levels:5.1.1 Class B, Water ResistantAn adhesive passing ClassB test requirements, as listed in Table 1, is
19、capable ofproducing sufficient adhesive-joint strength and durability andhas sufficient water resistance to make the bonded productsserviceable under conditions in which there will be occasionalintermittent exposure to wet conditions or high humidity.5.1.2 Class C, Dry UseAn adhesive passing Class C
20、 testrequirements, as listed in Table 1, has sufficient adhesive-jointstrength and durability under normal interior service conditionswhere the relative humidity is not high and does not fluctuatebetween wide limits.6. Test Requirements6.1 The test adhesives, when tested in accordance withSection 11
21、, shall remain in the viscosity range of 3000 to15 000 cP for a working life of at least 5 h, minimum.NOTE 4The viscosity requirement covers a 5-h span, although the“end-of-working-life” adhesive bond strength test is run at 4 h. Thisapparent conflict is necessary in order to assure that the mixed c
22、aseinadhesive is not in a rapidly rising viscosity pattern at the end of theworking life.6.1.1 The working life shall be timed from the addition ofthe adhesive powder to the water.6.1.2 The viscosity requirements shall not apply until thecasein has dissolved and the adhesive is ready for use.NOTE 5U
23、nless the manufacturer instructs otherwise, 20 min is thetypical time period required, after the adhesive powder is added to thewater, before the adhesive is ready for use.6.2 To meet the adhesive bond requirements of the specifi-cation, the test adhesive shall be subjected to the tests de-scribed i
24、n Section 12 and shall meet the requirements listed onTable 1.6.2.1 Two sets of adhesive bond tests are required, one to beinitiated 1 h after mixing the adhesive with water, and one 4 hafter mixing.6.3 To meet the storage-life requirements, an initial lot ofthe adhesive shall be tested following th
25、e manufacturerscertified storage life, and shall pass all test requirements for theapplicable adhesive classification. Following this initial test,certification for this requirement shall be based on submissionfrom the manufacturer.7. Retest and Rejection7.1 When a specimen fails at a load less than
26、 that specifiedand the wood failure is at least 50 %, 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 t
27、herequirements prescribed in this specification, that test shall berepeated on an additional set of specimens made from the samelot of adhesive, each of which shall conform to the require-ments specified. If this set of specimens fails to meet therequirements, the lot shall be rejected.TEST METHODS8
28、. Significance and Use8.1 This specification provides testing procedures to differ-entiate the physical, adhesive, and durability properties ofcommercially available casein and casein-protein adhesives.9. Apparatus9.1 Mechanical Stirrer or Mixer, capable of speed in air of5000 r/min for the preparat
29、ion of the adhesive mix.49.2 Other apparatus required to conduct tests are covered inPractice D 899, and Test Methods D 905, D 906, D 1084 andD 2556.10. Sampling10.1 Take a 5-lb (2.3-kg) representative sample of theadhesive from the lot to be tested. Store samples in airtight4Satisfactory mixing may
30、 be obtained using the intermediate speed of theThomas Three-Speed Stirrer No. 8585-M10 used with the stirring 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 loca-tions. Many other
31、laboratory supply houses can provide this same mixer or itsequivalent.TABLE 1 Test RequirementsTest Section NumberMinimum TestRequirementTest RequiredClass B Class CWorking life 6.1 5 h yes yesViscosity at 77 6 0.5F(256 0.25C)6.1 3000 to 15 000 cp yes yesBlock shear (compression)Dry at 1 and 4 h 12.
32、1 2800 psi (19 306 kPa) yes yesPlywood (tension) 12.2 340 psi (2344 kPa) yes yesDryat1and4hA12.2.3.1Soak, 48-h at 1 and 4 hA12.2.3.2 140 psi (965 kPa) yes noStorage life 14.Byes yesAOne and four hours refers to age of adhesive after mix. See 6.2.1.BA lot of the designated adhesive shall be tested fo
33、r 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.D 4689 99 (2005)2containers and seal. For the initial testing of storage life only(6.4), divide the s
34、ample into two equal portions, packed asdirected above. Use one portion for immediate testing andreserve the other for testing at the end of storage life.11. Working Life11.1 Prepare the adhesive for use in accordance with themanufacturers instructions. Measure the time from the intro-duction of the
35、 powder into the water, and determine viscosityin a 400-mL beaker at 20 min and at 1, 2, 3, 4, and 5 h, inaccordance with Test Methods D 1084, Method B, with thefollowing modifications:11.1.1 Keep the adhesive at 77 6 1F (25 6 0.5C) for theduration of the test for working life.11.1.2 Stir the adhesi
36、ve with a mechanical stirrer for 1 minimmediately before measuring the viscosity.11.1.3 Allow the viscometer spindle to rotate for 30 s beforerecording the dial reading.11.1.4 Using standard procedure for mixing a casein adhe-sive for testing, introduce the powder into the water withmechanical agita
37、tion, and continue the agitation for 1 min afterthe powder is dispersed. Turn off the mixer for approximately15 to 20 min, depending on the manufacturers instructions.Before the viscosity reading is taken, turn the mixer on againfor 1 min. Then take the reading promptly.11.1.5 Other temperatures may
38、 be used upon agreementbetween the contracting parties, but the 61F (60.5C)tolerance must be observed.NOTE 6Casein adhesives develop an exothermic reaction when addedto water, so the water temperature must be 5 to 10F (2.8 to 5.5C) lowerthan the desired temperature of the liquid adhesive.NOTE 7Altho
39、ugh casein adhesives and especially casein-soy blendadhesives have somewhat shear-rate-dependent flow properties, TestMethods D 1084, Method B, is referenced for viscosity determinationsrather than Test Method D 2556. The 1-min mixing time prior to readinga viscosity serves to break down the apparen
40、t viscosity build-up as theglue mix rests between readings. When more information is needed on theshear-rate-dependent flow properties of the adhesive, test the mix by TestMethod D 2556.12. Tests for Adhesive Bond12.1 Block Shear Strength (Compression):12.1.1 Prepare the specimens in accordance with
41、 TestMethod D 905, using the adhesive manufacturers instructions.12.1.1.1 In the absence of specific instructions, use a spreadrate of 60 lb/1000 ft2(0.19 g/in.2) of bond line (see PracticeD 899). The mixed metric/English system has been deliber-ately used, since it is a standard in the industry for
42、 spread rate.Use 1 to 2-min open assembly (time required to applyadhesive), 15-min closed assembly, 200 psi (1379 kPa) pres-sure, 2-h press time, and a 1-week conditioning period.12.1.2 Number of SpecimensTest 20 specimens represent-ing at least four assemblies.12.1.3 Dry TestFollowing the prescribe
43、d conditioningperiod for the adhesive being tested, bring one test group of 20specimens to 10 to 12 % moisture content and test in accor-dance with the instructions in Test Method D 905. Apply theload through a self-aligning seal to ensure uniform lateraldistribution of the load. Apply the load with
44、 a continuousmotion of the movable loading head at a rate of 0.5 in. (12.7mm)/min (610 %).NOTE 8To obtain the desired moisture content refer to Table 34 onpage 37 of the Wood Handbook.5Additional information is available inPractice E 104. Constant temperature and relative humidity cabinets areavaila
45、ble from laboratory supply companies.12.1.4 CalculationCalculate the shear stress at failure inpounds per square inch or kilopascals, based on the specimensbreaking load and tested bond-line area, measured to thenearest 0.10 in.2(6.5 mm2).12.2 Plywood Shear Tests:12.2.1 Prepare the specimens in acco
46、rdance with TestMethod D 906, using the adhesive manufacturers instructions.12.2.1.1 In the absence of specific instructions, use a spreadrate of 60 lb/1000 ft2(0.19 g/in.2) of bond line. The mixedmetric-English system has been deliberately used since it is astandard in the industry for spread rate
47、(see Practice D 899).Use 4 to 5 min open assembly time, 10 to 15 min closedassembly time, 2 h press time at 200 psi (1379 kPa), and a1-week conditioning period.12.2.2 Number of Specimens:12.2.2.1 Class B TestsPrepare 30 specimens, 10 fromeach of three assemblies. Separate the specimens randomlyinto
48、2 groups of 15 specimens each. Use one group for the drytest (12.2.3.1) and one group for the soak test (12.2.3.2).12.2.2.2 Class C TestsPrepare 20 specimens, 10 fromeach of two assemblies.12.2.3 Exposure Conditions and Treatments:12.2.3.1 Dry Test at 75F (24C)Following the prescribedaging period an
49、d cutting of the test specimens, bring specimens(15 specimens for Class B, and 20 specimens for Class C) to86 1 % moisture content and 75 6 2F (24 6 1C) and test inaccordance with Test Method D 906.12.2.3.2 Soak, 48-hFollowing the prescribed conditioningperiod and cutting of the test specimens, immerse the speci-mens in water at 75 6 2F (24 6 1C) and soak for 48 h, 615min. Remove from water and test immediately as specified inTest Method D 906, conducting the test in the wet state. Reportindividual and average test values. Dry the broke
