ASTM D4689-99(2005)
(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 D 907, 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 16, 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 and health practices and determine the applicability of regulatory limitations prior to use.
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D4689 −99 (Reapproved2005)
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 Department of Defense.
1. Scope D907 Terminology of Adhesives
D1084 Test Methods for Viscosity of Adhesives
1.1 This specification covers casein and other protein-blend
D2556 Test Method for Apparent Viscosity of Adhesives
adhesives for use adhering wood to wood. The adhesive type
Having Shear-Rate-Dependent Flow Properties
covered by this specification is a dry powder or granular
D5266 Practice for Estimating the Percentage of Wood
product comprising a mixture of casein, or casein and other
Failure in Adhesive Bonded Joints
protein source, with the necessary dry chemicals to effect
E104 Practice for Maintaining Constant Relative Humidity
solution when the mixture is added to water.
by Means of Aqueous Solutions
NOTE 1—Although the term casein adhesive is used throughout this
2.2 Other Standards:
specification, historically, the adhesive subclass described in 1.1 has been
MIL-STD-129—Marking for Shipment and Storage
known as casein glue. See Terminology D907, adhesive types.
FED-STD-123—Marking for Shipment
1.2 Limitations—Cooked casein adhesives are not covered
PPP-C-96—Cans, Metal, 28 Gage and Lighter
by this specification.
PPP-D-723—Drums, Fiber
1.3 The values stated in inch-pound units are to be regarded
PPP-D-729—Drums, Shipping and Storage, Steel, 55 Gal
as standard. The values given in parentheses are mathematical
(208 L)
conversions to SI units that are provided for information only
and are not considered standard.
3. Terminology
1.4 The following safety hazards caveat pertains only to the
3.1 Definitions—Many terms in this specification are de-
test method portion, Sections 8 through 16, of this specifica-
fined in Terminology D907.
tion: This standard does not purport to address all of the safety
3.2 Definitions of Terms Specific to This Standard:
concerns, if any, associated with its use. It is the responsibility
3.2.1 adhesive designation, n—an adhesive that is manufac-
of the user of this standard to establish appropriate safety and
tured by a unique combination of raw materials and manufac-
health practices and determine the applicability of regulatory
turing process that conforms to a given set of physical and
limitations prior to use.
performance properties and is identified by a specific name,
number, or alphanumeric designation.
2. Referenced Documents
2 3.2.2 lot, n—adhesive manufactured at one place from the
2.1 ASTM Standards:
same batch or blends of raw materials subjected to the same
D899 Practice for Applied Weight Per Unit Area of Liquid
operation and conditions.
Adhesive
D905 Test Method for Strength Properties of Adhesive NOTE 2—In this specification, the maple block lamination in Test
Method D905 and the birch plywood construction in Test Method D906
Bonds in Shear by Compression Loading
are described as assemblies.
D906 Test Method for Strength Properties of Adhesives in
Plywood Type Construction in Shear by Tension Loading
4. Significance and Use
4.1 Thisspecificationprovidestestingproceduresandspeci-
This specification is under the jurisdiction of ASTM Committee D14 on
fies requirements to differentiate the physical, adhesive, and
Adhesives and is the direct responsibility of Subcommittee D14.30 on Wood
durability properties of commercially available casein and
Adhesives.
Current edition approved April 1, 2005. Published May 2005. Originally casein-protein adhesives. The two classes are defined by water
approved in 1987. Last previous edition approved in 1999 as D4689 – 99. DOI:
resistance. Selection of class is left to the choice of the product
10.1520/D4689-99R05.
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
Standards volume information, refer to the standard’s Document Summary page on Available from Standardization Documents Order Desk, DODSSP, Bldg. 4,
the ASTM website. Section D, 700 Robbins Ave., Philadelphia, PA 19111-5098.
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D4689 − 99 (2005)
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)
Dry at 1 and 4 h 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.
manufacturer and the consumer, based on measures used by 6.2 To meet the adhesive bond requirements of the specifi-
each to protect the bond line from moisture degradation. cation, the test adhesive shall be subjected to the tests de-
scribed in Section 12 and shall meet the requirements listed on
NOTE 3—Because of strict EPA requirements as to disposal of waste
Table 1.
from manufacturing and production facilities, it has become necessary for
6.2.1 Two sets of adhesive bond tests are required, one to be
more than a decade to remove biocides from casein adhesives. Paint,
varnish, and restrictive exposure conditions are protective measures
initiated 1 h after mixing the adhesive with water, and one 4 h
commonly employed to protect the bond line against degradation due to
after mixing.
mold and moisture.
6.3 To meet the storage-life requirements, an initial lot of
4.2 The stress calculated by this specification should not be
the adhesive shall be tested following the manufacturer’s
used to predict failure, nor should it be used directly for design
certified storage life, and shall pass all test requirements for the
stress in joints with different geometry or with loading direc-
applicable adhesive classification. Following this initial test,
tion different from the test geometry.
certification for this requirement shall be based on submission
from the manufacturer.
5. Classification
5.1 For purposes of this specification, adhesives are classi-
7. Retest and Rejection
fied on the basis of water resistance at two performance levels:
7.1 When a specimen fails at a load less than that specified
5.1.1 Class B, Water Resistant—An adhesive passing Class
and the wood failure is at least 50 %, that specimen shall be
B test requirements, as listed in Table 1, is capable of
disregardedincomputingtheaverage.Ifmorethanonethirdof
producing sufficient adhesive-joint strength and durability and
the test specimens for any one test condition are discarded for
has sufficient water resistance to make the bonded products
this reason, the test shall be repeated.
serviceable under conditions in which there will be occasional
7.2 If the results of any initial test do not conform to the
intermittent exposure to wet conditions or high humidity.
requirements prescribed in this specification, that test shall be
5.1.2 Class C, Dry Use—An adhesive passing Class C test
repeatedonanadditionalsetofspecimensmadefromthesame
requirements, as listed in Table 1, has sufficient adhesive-joint
lot of adhesive, each of which shall conform to the require-
strengthanddurabilityundernormalinteriorserviceconditions
ments specified. If this set of specimens fails to meet the
where the relative humidity is not high and does not fluctuate
requirements, the lot shall be rejected.
between wide limits.
TEST METHODS
6. Test Requirements
6.1 The test adhesives, when tested in accordance with
8. Significance and Use
Section 11, shall remain in the viscosity range of 3000 to
8.1 This specification provides testing procedures to differ-
15 000 cP for a working life of at least 5 h, minimum.
entiate the physical, adhesive, and durability properties of
NOTE 4—The viscosity requirement covers a 5-h span, although the
commercially available casein and casein-protein adhesives.
“end-of-working-life” adhesive bond strength test is run at 4 h. This
apparent conflict is necessary in order to assure that the mixed casein
9. Apparatus
adhesive is not in a rapidly rising viscosity pattern at the end of the
9.1 Mechanical Stirrer or Mixer, capable of speed in air of
working life.
5000 r/min for the preparation of the adhesive mix.
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
Satisfactory mixing may be obtained using the intermediate speed of the
Thomas Three-Speed Stirrer No. 8585-M10 used with the stirring shaft, AHT No.
casein has dissolved and the adhesive is ready for use.
8633-T10, 9 in. (23 cm) long, and 1.5-in. (38-mm) diameter, four-blade propeller.
NOTE 5—Unless the manufacturer instructs otherwise, 20 min is the
Available from Thomas Scientific, Swedesboro, NJ 08085-0099, and other loca-
typical time period required, after the adhesive powder is added to the tions. Many other laboratory supply houses can provide this same mixer or its
water, before the adhesive is ready for use. equivalent.
D4689 − 99 (2005)
9.2 Other apparatus required to conduct tests are covered in 12.1.3 Dry Test—Following the prescribed conditioning pe-
Practice D899, and Test Methods D905, D906, D1084 and riod for the adhesive being tested, bring one test group of 20
D2556. specimens to 10 to 12 % moisture content and test in accor-
dance with the instructions in Test Method D905. Apply the
10. Sampling
load through a self-aligning seal to ensure uniform lateral
distribution of the load. Apply the load with a continuous
10.1 Take a 5-lb (2.3-kg) representative sample of the
motion of the movable loading head at a rate of 0.5 in. (12.7
adhesive from the lot to be tested. Store samples in airtight
mm)/min (610 %).
containers and seal. For the initial testing of storage life only
(6.4), divide the sample into two equal portions, packed as
NOTE 8—To obtain the desired moisture content
...
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