1、Designation: D4689 12 (Reapproved 2018)Standard 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 number i
2、n 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 U.S. Department of Defense.1. Scope1.1 This specification covers casein and other protein-blenda
3、dhesives 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 c
4、asein adhesive is used throughout thisspecification, historically, the adhesive subclass described in 1.1 has beenknown as casein glue. See Terminology D907, 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 13, of this specifica-tion: This sta
6、ndard 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,health, and environmental practices and determine the appli-cability of regulatory limitations prior to use.1.5 This inte
7、rnational standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT)
8、Committee.2. Referenced Documents2.1 ASTM Standards:2D899 Practice for Applied Weight Per Unit Area of LiquidAdhesiveD905 Test Method for Strength Properties of AdhesiveBonds in Shear by Compression LoadingD906 Test Method for Strength Properties of Adhesives inPlywood Type Construction in Shear by
9、Tension LoadingD907 Terminology of AdhesivesD1084 Test Methods for Viscosity of AdhesivesD2556 Test Method for Apparent Viscosity of AdhesivesHaving Shear-Rate-Dependent Flow Properties Using Ro-tational ViscometryD5266 Practice for Estimating the Percentage of WoodFailure in Adhesive Bonded JointsE
10、104 Practice for Maintaining Constant Relative Humidityby Means of Aqueous Solutions2.2 Other Standards:3MIL-STD-129 Marking for Shipment and StorageFED-STD-123 Marking for ShipmentPPP-C-96 Cans, Metal, 28 Gage and LighterPPP-D-723 Drums, FiberPPP-D-729 Drums, Shipping and Storage, Steel, 55 Gal(208
11、 L)3. Terminology3.1 DefinitionsMany terms in this specification are de-fined in Terminology D907.3.2 Definitions of Terms Specific to This Standard:3.2.1 lot, nadhesive manufactured at one place from thesame batch or blends of raw materials subjected to the sameoperation and conditions.NOTE 2In thi
12、s specification, the maple block lamination in TestMethod D905 and the birch plywood construction in Test Method D906are described as assemblies.4. Significance and Use4.1 This specification provides testing procedures and speci-fies requirements to differentiate the physical, adhesive, anddurabilit
13、y properties of commercially available casein andcasein-protein adhesives. The two classes are defined by water1This specification is under the jurisdiction of ASTM Committee D14 onAdhesives and is the direct responsibility of Subcommittee D14.30 on WoodAdhesives.Current edition approved Aug. 1, 201
14、8. Published August 2018. Originallyapproved in 1987. Last previous edition approved in 2012 as D4689 12. DOI:10.1520/D4689-12R18.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume informat
15、ion, refer to the standards Document Summary page onthe ASTM website.3Available from Standardization Documents Order Desk, DODSSP, Bldg. 4,Section D, 700 Robbins Ave., Philadelphia, PA 19111-5098, http:/dodssp.daps.dla.mil.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Consho
16、hocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Orga
17、nization Technical Barriers to Trade (TBT) Committee.1resistance. 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 wastefro
18、m manufacturing and production facilities, most if not all biocides wereremoved from casein adhesives. Paint, varnish, and restrictive exposureconditions are protective measures commonly employed now to protectthe bond line against degradation due to mold and moisture.4.2 The stress calculated by th
19、is specification should not beused to predict failure, nor should it be used directly for designstress in joints with different geometry or 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 wate
20、r resistance at two performance levels:5.1.1 Class B, Water ResistantAn adhesive passing ClassB test requirements, as listed in Table 1, is capable ofproducing sufficient adhesive-joint strength and durability andhas sufficient water resistance to make the bonded productsserviceable under conditions
21、 in which there will be occasionalintermittent exposure to wet conditions or high humidity.5.1.2 Class C, Dry UseAn adhesive passing Class C testrequirements, as listed in Table 1, has sufficient adhesive-jointstrength and durability under normal interior service conditionswhere the relative humidit
22、y is not high and does not fluctuatebetween wide limits.6. Test Requirements6.1 The test adhesives, when tested in accordance withSection 11, 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, althoug
23、h 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 caseinadhesive 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
24、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 5Unless the manufacturer instructs otherwise, 20 min is thetypical time period required, after the adhesive powder is added to thewater, before the adhesive is re
25、ady for use.6.2 To meet the adhesive bond requirements of thespecification, the test adhesive shall be subjected to the testsdescribed in Section 12 and shall meet the requirements listedon Table 1.6.2.1 Two sets of adhesive bond tests are required, one to beinitiated 1 h after mixing the adhesive w
26、ith water, and one 4 hafter mixing.6.3 To meet the storage-life requirements, an initial lot ofthe adhesive shall be tested following the manufacturerscertified storage life, and shall pass all test requirements for theapplicable adhesive classification. Following this initial test,certification for
27、 this requirement shall be based on submissionfrom the manufacturer.7. Retest and Rejection7.1 When a specimen fails at a load less than 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 an
28、y 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 this specification, that test shall berepeated on an additional set of specimens made from the samelot of adhesive, each of which shall
29、 conform to the require-ments specified. If this set of specimens fails to meet therequirements, the lot shall be rejected.TEST METHODS8. Significance and Use8.1 This specification provides testing procedures to differ-entiate the physical, adhesive, and durability properties ofcommercially availabl
30、e casein and casein-protein adhesives.TABLE 1 Test RequirementsTest Section NumberMinimum TestRequirementTest RequiredClass B Class CWorking life 6.1 5 h yes yesViscosity at 77 0.5F(25 0.25C)6.1 3000 to 15 000 cp yes yesBlock shear (compression)Dryat1and4h 12.1 2800 psi (19 306 kPa) yes yesPlywood (
31、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 14Byes yesAOne and four hours refers to age of adhesive after mix. See 6.2.1.BA lot of the designated adhesive shall be tested for all the required tests after aging for
32、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 12 (2018)29. Apparatus9.1 Mechanical Stirrer or Mixer, capable of speed in air of5000 r/min for the preparation of the adhesive mix.49.2
33、 Other apparatus required to conduct tests are covered inPractice D899, and Test Methods D905, D906, D1084 andD2556.10. Sampling10.1 Take a 5-lb (2.3-kg) representative sample of theadhesive from the lot to be tested. Store samples in airtightcontainers and seal. For the initial testing of storage l
34、ife only(6.4), divide the sample 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 fr
35、om the intro-duction of the 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 D1084, 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 l
36、ife.11.1.2 Stir the adhesive 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
37、water withmechanical agitation, 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.
38、1.5 Other temperatures may 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 l
39、iquid adhesive.NOTE 7Although casein adhesives and especially casein-soy blendadhesives have somewhat shear-rate-dependent flow properties, TestMethods D1084, Method B, is referenced for viscosity determinationsrather than Test Method D2556. The 1-min mixing time prior to readinga viscosity serves t
40、o break down the apparent 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 D2556.12. Tests for Adhesive Bond12.1 Block Shear Strength (Compression):12.1.1 Prepare the speci
41、mens in accordance with TestMethod D905, 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 PracticeD899). The mixed metric/English system has been deliberatelyused, since it is a standard
42、in the industry for spread rate. Use1 to 2-min open assembly (time required to apply adhesive),15-min closed assembly, 200 psi (1379 kPa) pressure, 2-h presstime, and a 1-week conditioning period.12.1.2 Number of SpecimensTest 20 specimens represent-ing at least four assemblies.12.1.3 Dry TestFollow
43、ing the prescribed conditioning pe-riod 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 D905. Apply theload through a self-aligning seal to ensure uniform lateraldistribution of the load. A
44、pply the load with 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 E104. Constant temperature and relative humidity c
45、abinets areavailable 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
46、specimens in accordance with TestMethod D906, 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
47、for spread rate (see Practice D899).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 from eachof three assemblies. Separate the specimen
48、s randomly into 2groups of 15 specimens each. Use one group for the dry test(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 prescribed
49、aging period and cutting of the test specimens, bring specimens(15 specimens for Class B, and 20 specimens for Class C) to 86 1 % moisture content and 75 6 2F (24 6 1C) and test inaccordance with Test Method D906.12.2.3.2 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, 6154Satisfactory mixing may be obtained using the intermediate speed of theThomas Three-Speed Stirrer No. 8585-M10 used with the stirring shaft, AHT No.8633-T10
