ASTM D4689-12(2018)
(Specification)Standard Specification for Adhesive, Casein-Type
Standard Specification for Adhesive, Casein-Type
ABSTRACT
This specification covers casein and other protein-based adhesives in the form of dry powder or granular product for use in adhering wood to wood. This specification provides testing procedures and specifies requirements to differentiate the physical, adhesive, and durability properties of commercially available casein and casein-protein adhesives. Adhesives are classified as class B (water resistant) and class C (dry use). Testing procedures include working life, block shear strength, plywood shear test, and storage life. The adhesive shall conform to the viscosity requirement, working life, block shear, tension, and storage life of this specification. Other requirements include instruction sheet, packing, and marking requirements.
SCOPE
1.1 This specification covers casein and other protein-blend adhesives for use adhering wood to wood. The adhesive type covered 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 1: Although the term casein adhesive is used throughout this specification, historically, the adhesive subclass described in 1.1 has been known as casein glue. See Terminology D907, adhesive types.
1.2 Limitations—Cooked casein adhesives are not covered by this specification.
1.3 The values stated in inch-pound units are to be regarded as standard. The values given in parentheses are mathematical conversions 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 8 through 13, of this specification: This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
General Information
Relations
Standards Content (Sample)
This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D4689 −12 (Reapproved 2018)
Standard Specification for
Adhesive, Casein-Type
This standard is issued under the fixed designation D4689; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript 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. Scope D899 Practice for Applied Weight Per Unit Area of Liquid
Adhesive
1.1 This specification covers casein and other protein-blend
D905 Test Method for Strength Properties of Adhesive
adhesives for use adhering wood to wood. The adhesive type
Bonds in Shear by Compression Loading
covered by this specification is a dry powder or granular
D906 Test Method for Strength Properties of Adhesives in
product comprising a mixture of casein, or casein and other
Plywood Type Construction in Shear by Tension Loading
protein source, with the necessary dry chemicals to effect
D907 Terminology of Adhesives
solution when the mixture is added to water.
D1084 Test Methods for Viscosity of Adhesives
NOTE 1—Although the term casein adhesive is used throughout this
D2556 Test Method for Apparent Viscosity of Adhesives
specification, historically, the adhesive subclass described in 1.1 has been
Having Shear-Rate-Dependent Flow Properties Using Ro-
known as casein glue. See Terminology D907, adhesive types.
tational Viscometry
1.2 Limitations—Cooked casein adhesives are not covered
D5266 Practice for Estimating the Percentage of Wood
by this specification.
Failure in Adhesive Bonded Joints
E104 Practice for Maintaining Constant Relative Humidity
1.3 The values stated in inch-pound units are to be regarded
as standard. The values given in parentheses are mathematical by Means of Aqueous Solutions
2.2 Other Standards:
conversions to SI units that are provided for information only
and are not considered standard. MIL-STD-129 Marking for Shipment and Storage
FED-STD-123 Marking for Shipment
1.4 The following safety hazards caveat pertains only to the
PPP-C-96 Cans, Metal, 28 Gage and Lighter
test method portion, Sections 8 through 13, of this specifica-
PPP-D-723 Drums, Fiber
tion: This standard does not purport to address all of the safety
PPP-D-729 Drums, Shipping and Storage, Steel, 55 Gal
concerns, if any, associated with its use. It is the responsibility
(208 L)
of the user of this standard to establish appropriate safety,
health, and environmental practices and determine the appli-
3. Terminology
cability of regulatory limitations prior to use.
3.1 Definitions—Many terms in this specification are de-
1.5 This international standard was developed in accor-
fined in Terminology D907.
dance with internationally recognized principles on standard-
3.2 Definitions of Terms Specific to This Standard:
ization established in the Decision on Principles for the
3.2.1 lot, n—adhesive manufactured at one place from the
Development of International Standards, Guides and Recom-
same batch or blends of raw materials subjected to the same
mendations issued by the World Trade Organization Technical
operation and conditions.
Barriers to Trade (TBT) Committee.
NOTE 2—In this specification, the maple block lamination in Test
2. Referenced Documents
Method D905 and the birch plywood construction in Test Method D906
are described as assemblies.
2.1 ASTM Standards:
4. Significance and Use
This specification is under the jurisdiction of ASTM Committee D14 on
4.1 Thisspecificationprovidestestingproceduresandspeci-
Adhesives and is the direct responsibility of Subcommittee D14.30 on Wood
fies requirements to differentiate the physical, adhesive, and
Adhesives.
durability properties of commercially available casein and
Current edition approved Aug. 1, 2018. Published August 2018. Originally
approved in 1987. Last previous edition approved in 2012 as D4689 – 12. DOI: casein-protein adhesives. The two classes are defined by water
10.1520/D4689-12R18.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Available from Standardization Documents Order Desk, DODSSP, Bldg. 4,
Standards volume information, refer to the standard’s Document Summary page on Section D, 700 Robbins Ave., Philadelphia, PA 19111-5098, http://
the ASTM website. dodssp.daps.dla.mil.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D4689 − 12 (2018)
resistance. Selection of class is left to the choice of the product 6.2 To meet the adhesive bond requirements of the
manufacturer and the consumer, based on measures used by specification, the test adhesive shall be subjected to the tests
each to protect the bond line from moisture degradation.
described in Section 12 and shall meet the requirements listed
on Table 1.
NOTE 3—Because of strict EPA requirements as to disposal of waste
frommanufacturingandproductionfacilities,mostifnotallbiocideswere
6.2.1 Two sets of adhesive bond tests are required, one to be
removed from casein adhesives. Paint, varnish, and restrictive exposure
initiated 1 h after mixing the adhesive with water, and one 4 h
conditions are protective measures commonly employed now to protect
after mixing.
the bond line against degradation due to mold and moisture.
4.2 The stress calculated by this specification should not be 6.3 To meet the storage-life requirements, an initial lot of
the adhesive shall be tested following the manufacturer’s
used to predict failure, nor should it be used directly for design
stress in joints with different geometry or with loading direc- certified storage life, and shall pass all test requirements for the
tion different from the test geometry. applicable adhesive classification. Following this initial test,
certification for this requirement shall be based on submission
5. Classification
from the manufacturer.
5.1 For purposes of this specification, adhesives are classi-
fied on the basis of water resistance at two performance levels:
7. Retest and Rejection
5.1.1 Class B, Water Resistant—An adhesive passing Class
7.1 When a specimen fails at a load less than that specified
B test requirements, as listed in Table 1, is capable of
and the wood failure is at least 50 %, that specimen shall be
producing sufficient adhesive-joint strength and durability and
disregardedincomputingtheaverage.Ifmorethanonethirdof
has sufficient water resistance to make the bonded products
the test specimens for any one test condition are discarded for
serviceable under conditions in which there will be occasional
this reason, the test shall be repeated.
intermittent exposure to wet conditions or high humidity.
5.1.2 Class C, Dry Use—An adhesive passing Class C test
7.2 If the results of any initial test do not conform to the
requirements, as listed in Table 1, has sufficient adhesive-joint
requirements prescribed in this specification, that test shall be
strengthanddurabilityundernormalinteriorserviceconditions
repeatedonanadditionalsetofspecimensmadefromthesame
where the relative humidity is not high and does not fluctuate
lot of adhesive, each of which shall conform to the require-
between wide limits.
ments specified. If this set of specimens fails to meet the
requirements, the lot shall be rejected.
6. Test Requirements
6.1 The test adhesives, when tested in accordance with
Section 11, shall remain in the viscosity range of 3000 to
TEST METHODS
15 000 cP for a working life of at least 5 h, minimum.
8. Significance and Use
NOTE 4—The viscosity requirement covers a 5-h span, although the
“end-of-working-life” adhesive bond strength test is run at 4 h. This
8.1 This specification provides testing procedures to differ-
apparent conflict is necessary in order to assure that the mixed casein
entiate the physical, adhesive, and durability properties of
adhesive is not in a rapidly rising viscosity pattern at the end of the
working life.
commercially available casein and casein-protein adhesives.
6.1.1 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 5—Unless the manufacturer instructs otherwise, 20 min is the
typical time period required, after the adhesive powder is added to the
water, before the adhesive is ready for use.
TABLE 1 Test Requirements
Minimum Test Test Required
Test Section Number
Requirement
Class B Class C
Working life 6.1 5 h yes yes
Viscosity at 77 ± 0.5°F 6.1 3000 to 15 000 cp yes yes
(25± 0.25°C)
Block shear (compression)
Dryat1and4h 12.1 2800 psi (19 306 kPa) yes yes
Plywood (tension) 12.2 340 psi (2344 kPa) yes yes
A
Dryat1and4h 12.2.3.1
A
Soak, 48-h at 1 and 4 h 12.2.3.2 140 psi (965 kPa) yes no
B
Storage life 14 yes yes
A
One and four hours refers to 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 the
minimum requirements shall be the storage life certified by the manufacturer.
D4689 − 12 (2018)
9. Apparatus 12.1.1 Prepare the specimens in accordance with Test
Method D905, using the adhesive manufacturer’s instructions.
9.1 Mechanical Stirrer or Mixer, capable of speed in air of
4 12.1.1.1 In the absence of specific instructions, use a spread
5000 r/min for the preparation of the adhesive mix.
2 2
rate of 60 lb/1000 ft (0.19 g/in. ) of bond line (see Practice
9.2 Other apparatus required to conduct tests are covered in
D899).The mixed metric/English system has been deliberately
Practice D899, and Test Methods D905, D906, D1084 and
used, since it is a standard in the industry for spread rate. Use
D2556.
1 to 2-min open assembly (time required to apply adhesive),
15-minclosedassembly,200psi(1379kPa)pressure,2-hpress
10. Sampling
time, and a 1-week conditioning period.
10.1 Take a 5-lb (2.3-kg) representative sample of the
12.1.2 Number of Specimens—Test 20 specimens represent-
adhesive from the lot to be tested. Store samples in airtight
ing at least four assemblies.
containers and seal. For the initial testing of storage life only
12.1.3 Dry Test—Following the prescribed conditioning pe-
(6.4), divide the sample into two equal portions, packed as
riod for the adhesive being tested, bring one test group of 20
directed above. Use one portion for immediate testing and
specimens to 10 to 12 % moisture content and t
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