ASTM D4689-99

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D 4689 – 99
Standard Specification for
Adhesive, Casein-Type
This standard is issued under the fixed designation D 4689; 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 (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. Scope D 5266 Practice for Estimating the Percentage of Wood
Failure in Adhesive Bonded Joints
1.1 This specification covers casein and other protein-blend
E 104 Practice for Maintaining Constant Relative Humidity
adhesives for use adhering wood to wood. The adhesive type
by Means of Aqueous Solutions
covered by this specification is a dry powder or granular
2.2 Other Standards:
product comprising a mixture of casein, or casein and other
MIL-STD-129—Marking for Shipment and Storage
protein source, with the necessary dry chemicals to effect
FED-STD-123—Marking for Shipment
solution when the mixture is added to water.
PPP-C-96—Cans, Metal, 28 Gage and Lighter
NOTE 1—Although the term casein adhesive is used throughout this
PPP-D-723—Drums, Fiber
specification, historically, the adhesive subclass described in 1.1 has been
PPP-D-729—Drums, Shipping and Storage, Steel, 55 Gal
known as casein glue. See Terminology D 907, adhesive types.
(208 L)
1.2 Limitations—Cooked casein adhesives are not covered
3. Terminology
by this specification.
1.3 The values stated in inch-pound units are to be regarded
3.1 Definitions—Many terms in this specification are de-
as the standard.
fined in Terminology D 907.
1.4 The following safety hazards caveat pertains only to the
3.2 Definitions of Terms Specific to This Standard:
test method portion, Sections 8 through 16, of this specifica-
3.2.1 adhesive designation, n—an adhesive that is manufac-
tion: This standard does not purport to address all of the safety
tured by a unique combination of raw materials and manufac-
concerns, if any, associated with its use. It is the responsibility
turing process that conforms to a given set of physical and
of the user of this standard to establish appropriate safety and
performance properties and is identified by a specific name,
health practices and determine the applicability of regulatory
number, or alphanumeric designation.
limitations prior to use.
3.2.2 lot, n—adhesive manufactured at one place from the
same batch or blends of raw materials subjected to the same
2. Referenced Documents
operation and conditions.
2.1 ASTM Standards:
NOTE 2—In this specification, the maple block lamination in Test
D 899 Test Method for Applied Weight per Unit Area of
Method D 905 and the birch plywood construction in Test Method D 906
Liquid Adhesive
are described as assemblies.
D 905 Test Method for Strength Properties of Adhesive
Bonds in Shear by Compression Loading
4. Significance and Use
D 906 Test Method for Strength Properties of Adhesives in
4.1 Thisspecificationprovidestestingproceduresandspeci-
Plywood Type Construction in Shear by Tension Loading
fies requirements to differentiate the physical, adhesive, and
D 907 Terminology of Adhesives
durability properties of commercially available casein and
D 1084 Test Methods for Viscosity of Adhesives
casein-protein adhesives. The two classes are defined by water
D 2556 Test Method for Apparent Viscosity of Adhesives
resistance. Selection of class is left to the choice of the product
Having Shear-Rate-Dependent Flow Properties
manufacturer and the consumer, based on measures used by
each to protect the bond line from moisture degradation.
NOTE 3—Because of strict EPA requirements as to disposal of waste
This specification is under the jurisdiction of ASTM Committee D-14 on
Adhesives and is the direct responsibility of Subcommittee D 14.30 on Wood
Adhesives.
Current edition approved April 10, 1999. Published June 1999. Originally Annual Book of ASTM Standards, Vol 11.03.
published as D 4689 – 87. Last previous edition D 4689 – 95a. AvailablefromStandardizationDocumentsOrderDesk,Bldg.4SectionD,700
Annual Book of ASTM Standards, Vol 15.06. Robbins Ave., Philadelphia, PA 19111-5094, Attn: NPODS.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D4689–99
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 6 0.5°F 6.1 3000 to 15 000 cp yes yes
(256 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.
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,
initiated 1 h after mixing the adhesive with water, and one 4 h
varnish, and restrictive exposure conditions are protective measures
after mixing.
commonly employed to protect the bond line against degradation due to
6.3 To meet the storage-life requirements, an initial lot of
mold and moisture.
the adhesive shall be tested following the manufacturer’s
4.2 The stress calculated by this specification should not be
certified storage life, and shall pass all test requirements for the
used to predict failure, nor should it be used directly for design
applicable adhesive classification. Following this initial test,
stress in joints with different geometry or with loading direc-
certification for this requirement shall be based on submission
tion different from the test geometry.
from the manufacturer.
5. Classification
7. Retest and Rejection
5.1 For purposes of this specification, adhesives are classi-
7.1 When a specimen fails at a load less than that specified
fied on the basis of water resistance at two performance levels:
and the wood failure is at least 50 %, that specimen shall be
5.1.1 Class B, Water Resistant—An adhesive passing Class
disregardedincomputingtheaverage.Ifmorethanonethirdof
B test requirements, as listed in Table 1, is capable of
the test specimens for any one test condition are discarded for
producing sufficient adhesive-joint strength and durability and
this reason, the test shall be repeated.
has sufficient water resistance to make the bonded products
7.2 If the results of any initial test do not conform to the
serviceable under conditions in which there will be occasional
requirements prescribed in this specification, that test shall be
intermittent exposure to wet conditions or high humidity.
repeated on an additional set of specimens made from the same
5.1.2 Class C, Dry Use—An adhesive passing Class C test
lot of adhesive, each of which shall conform to the require-
requirements, as listed in Table 1, has sufficient adhesive-joint
ments specified. If this set of specimens fails to meet the
strengthanddurabilityundernormalinteriorserviceconditions
requirements, the lot shall be rejected.
where the relative humidity is not high and does not fluctuate
TEST METHODS
between wide limits.
8. Significance and Use
6. Test Requirements
8.1 This specification provides testing procedures to differ-
6.1 The test adhesives, when tested in accordance with
entiate the physical, adhesive, and durability properties of
Section 11, shall remain in the viscosity range of 3000 to
commercially available casein and casein-protein adhesives.
15 000 cP for a working life of at least 5 h, minimum.
9. Apparatus
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
9.1 Mechanical Stirrer or Mixer, capable of speed in air of
apparent conflict is necessary in order to assure that the mixed casein
5000 r/min for the preparation of the adhesive mix.
adhesive is not in a rapidly rising viscosity pattern at the end of the
9.2 Other apparatus required to conduct tests are covered in
working life.
Test Methods D 899, D 905, D 906, D 1084 and D 2556.
6.1.1 The working life shall be timed from the addition of
10. Sampling
the adhesive powder to the water.
6.1.2 The viscosity requirements shall not apply until the
10.1 Take a 5-lb (2.3-kg) representative sample of the
casein has dissolved and the adhesive is ready for use.
adhesive from the lot to be tested. Store samples in airtight
containers and seal. For the initial testing of storage life only
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.
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.
6.2 To meet the adhesive bond requirements of the specifi-
8633-T10, 9 in. (23 cm) long, and 1.5-in. (38-mm) diameter, four-blade propeller.
cation, the test adhesive shall be subjected to the tests de-
Available from Thomas Scientific, Swedesboro, NJ 08085-0099, and other loca-
scribed in Section 12 and shall meet the requirements listed on
tions. Many other laboratory supply houses can provide this same mixer or its
Table 1. equivalent.
D4689–99
NOTE 8—To obtain the desired moisture content refer to Table 3–4 on
(6.4), divide the sample into two equal portions, packed as
page 3–7 of the Wood Handbook. Additional information is available in
directed above. Use one portion for immediate testing and
Practice E 104. Constant temperature and relative humidity cabinets are
reserve the other for testing at the end of storage life.
available from laboratory supply companies.
11. Working Life
12.1.4 Calculation—Calculate the shear stress at failure in
11.1 Prepare the adhesive for use in accordance with the pounds per square inch or kilopascals, based on the specimen’s
m
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