ASTM D4690-99

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D 4690 – 99
Standard Specification for
Urea-Formaldehyde Resin Adhesives
This standard is issued under the fixed designation D 4690; 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 1490 Test Method for Nonvolatile Content of Urea-
Formaldehyde Resin Solutions
1.1 This specification covers three types of urea-
D 1583 Test Method for Hydrogen Ion Concentration of
formaldehyde thermosetting resin adhesives suitable for use on
Dry Adhesive Films
wood, wood-based substrates, or plastic laminates.
D 1875 Test Method for Density of Adhesives in Fluid
1.2 The values stated in SI units are to be regarded as the
Form
standard. The values given in parentheses are provided for
D 2556 Test Method for Apparent Viscosity of Adhesives
information purposes only.
Having Shear-Rate-Dependent Flow Properties
1.3 The requirements for the adhesive are based on tests of
D 5266 Practice for Estimating the Percentage of Wood
physical properties including viscosity, density, nonvolatile
Failure in Adhesive Bonded Joints
content, pH, insoluble matter, amylaceous matter, mixing
E 70 Test Method for pH of Aqueous Solutions with the
properties, working life, and on strength properties, including
Glass Electrode
dry shear strength in lumber-type joints, dry and wet shear
E 104 Practice for Maintaining Constant Relative Humidity
strength in plywood-type joints, and all strength tests at the end
by Means of Aqueous Solutions
of the storage life certified by the manufacturer.
2.2 Federal Specifications:
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 and
2.3 Federal Standard:
health practices and determine the applicability of regulatory
FED-STD-123 Marking for Shipment
limitations prior to use.
2.4 Military Standard:
2. Referenced Documents MIL-STD-129 Marking for Shipment and Storage
2.1 ASTM Standards:
3. Terminology
B 417 Test Method for Apparent Density of Non-Free-
2 3.1 Definitions—Many terms in this specification are de-
Flowing Metal Powders
fined in Terminology D 907.
D 905 Test Method for Strength Properties of Adhesive
3 3.2 Definitions of Terms Specific to This Standard:
Bonds in Shear by Compression Loading
3.2.1 adhesive designation—an adhesive that is manufac-
D 906 Test Method for Strength Properties of Adhesives in
3 tured by a unique combination of raw materials and manufac-
Plywood Type Construction in Shear by Tension Loading
turing process that conforms to a given set of physical and
D 907 Terminology of Adhesives
3 performance properties and is identified by specific name,
D 1084 Test Methods for Viscosity of Adhesives
number, or alphanumeric designation.
D 1489 Test Method for Nonvolatile Content of Aqueous
3.2.2 lot—adhesive manufactured at one place from the
Adhesives
same batch or blends of raw materials subjected to the same
operations and conditions.
This specification is under the jurisdiction of ASTM Committee D-14 on
NOTE 1—In this specification, the maple block lamination in Test
Adhesives and is the direct responsibility of Subcommittee D14.30 on Wood
Method D 905 and the birch plywood construction in Test Method D 906
Adhesives.
Current edition approved April 10, 1999. Published June 1999. Originally
published as D 4690 – 87. Last previous edition D 4690 – 95a.
This specification is intended as a replacement for Federal Specification Annual Book of ASTM Standards, Vol 15.05.
MMM-A-188c, Adhesive; Urea Resin Type (Liquid and Powder). Annual Book of ASTM Standards, Vol 11.03.
2 6
Annual Book of ASTM Standards, Vol 02.05. Available from Standardization Documents Order Desk, Bldg. 4 Section D,
Annual Book of ASTM Standards, Vol 15.06. 700 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.
D 4690
are described as assemblies.
6.3 The curing agent for Types A and C shall readily
disperse in the adhesive mixture when used in accordance with
4. Significance and Use
the manufacturer’s recommendation.
4.1 Thisspecificationprovidestestingproceduresandspeci-
6.4 The filler shall neither dissolve nor swell excessively in
fies requirements to differentiate between the physical and
water, and shall not settle from the adhesive mixture during the
adhesive bonding properties of the many commercial urea-
working life.
formaldehyde thermosetting resin and catalyst systems.
7. Retest and Rejection
4.2 Because of the diverse nature of products bonded with
these adhesives, testing by this specification will only evaluate
7.1 When a specimen fails at a load less than that specified,
the adhesive under a given set of conditions. The physical
if the wood failure is 50 % or greater, that specimen shall be
properties of the adhesive are measured to provide information
disregardedincomputingtheaverage.Ifmorethanonethirdof
on certain handling and working properties. The adhesive-
the test specimens for any one test condition are discarded for
bonding properties are measured on maple block and birch
this reason, the test shall be repeated.
plywood specimens, prepared and tested in accordance with
7.2 If the results of any initial test do not conform to the
Test Method D 905 and Test Method D 906, respectively. The
requirements prescribed in this specification, that test shall be
certification requirements have been based on knowledge
repeated on an additional set of specimens made from the same
within the industry of values that may be expected. Test
lot of adhesive, each set of which shall conform to the
Method D 905 and Test Method D 906 have a long history of
requirementsspecified.Ifthissetofspecimensfailstomeetthe
use in many specifications.
requirements, the lot shall be rejected.
4.3 The stress calculated by using this specification should
TEST METHODS
not be used to predict failure nor should it be used for design
stress in joints with different geometry or loading direction
8. Significance and Use
different from the test geometry.
8.1 This specification provides testing procedures to differ-
5. Classification
entiate between the physical and adhesive bonding properties
of the many commercial urea-formaldehyde thermosetting
5.1 Urea resin adhesive shall be furnished as one of the
resin and catalyst systems.
following types:
5.1.1 Type A—Powder with separate curing agent.
9. Sampling
5.1.2 Type B—Powder with incorporated curing agent.
9.1 Take a representative, 2-L (2-qt) sample of adhesive
5.1.3 Type C—Liquid with separate curing agent.
from the lot to be tested. Divide the sample into two equal
NOTE 2—Type A, Type B, and Type C replace the Type I, Type II, and
portions and place each in a wide mouth, glass, 1-L (1-qt)
Type III classifications of Federal Specification MMM-A-188C, respec-
container and seal tightly. Use one of the samples for tests of
tively, to prevent confusion with Type I (boil test) and Type II (cold-water
physical and adhesive bond properties (Sections 10 and 11),
soak) classifications used in existing ASTM standards for adhesives.
and use the other for testing storage life (11.2.3.3), and for any
6. Test Requirements
retesting that may be necessary under Section 7. Also, take
sufficient quantity of curing agent to cure the adhesive samples
6.1 To meet the requirements of this specification, the urea
and place in a separate, clean, dry container. Seal all sample
resin and adhesive mix shall be subjected to the tests listed in
containers with well-fitting, corrosion-resistant lids.
Section 10. In addition, the adhesive shall meet the require-
ments of the tests described in Section 11 and as listed inTable
10. Physical Properties
1.
10.1 Test the physical properties of adhesives by the fol-
6.2 To meet the storage-life requirements, an initial lot of
lowing test methods:
the adhesive shall be tested in accordance with Sections 10 and
10.1.1 Viscosity:
11. It shall pass all test requirements after being stored under
10.1.1.1 Measure the viscosity of the liquid urea resin or
conditions and time specified by the manufacturer. Following
adhesive mixtures in accordance with Test Methods D 1084 or
this initial test, certification shall be based on submission from
D 2556.
the manufacturer.
10.1.1.2 Temperature of Test—Condition to, and maintain
the liquid urea resin or adhesive mixture at 24 6 0.5°C (75 6
TABLE 1 Test Requirements
1°F) during the viscosity reading. Other temperatures may be
Test Requirement
used upon agreement between the contracting parties, but the
Test Section Number
(Minimum)
60.5°C (61°F) tolerance must be observed.
Block shear (compression)
10.1.1.3 For Type C adhesives requiring the addition of a
Dry at 24°C (75°F) 11.1 19 306 kPa (2800 psi)
curing agent, make two viscosity measurements of the test
Plywood shear (tension)
Dry at 24°C (75°F) 11.2.3.1 2 344 kPa (340 psi)
adhesives (1) before the addition of curing agent, and (2) after
48-h soak 11.2.3.2 1 930 kPa (280 psi)
the addition of the curing agent. The viscosity of urea resins
A
Storage life 11.2.3.3
following addition of curing agent to liquid resin is time-
A
A retained sample of the initial lot of the adhesive shall be tested and shall meet
dependent. Make the measurement 10 min after mixing.
the requirements of all tests listed in 6.2 for the applicable type of adhesive after
the storage life time certified by the manufacturer. 10.1.2 Density:
D 4690
10.1.2.1 Measure the density of dry-powder adhesives or 2.5°C (75 6 5°F) using a Brookfield Viscometer. Consider the
separate curing agents in accordance with Test Method B 417, adhesive to be at the end of its working life when it reaches a
and report in grams per cubic centimetre (pounds per cubic viscosity of 600 P (0.6 Pa·s). If the temperature of the bonding
foot). (See Appendix X1.) operation is 32.2°C (90°F) or higher, the above test may be
10.1.2.2 Measure the density of Type C adhesives in accor- conducted at 32.2°C (90°F).
dance with Test Method D 1875 and report in grams per
NOTE 4—A disposable beaker or a 473-mL (16-oz) plastic cup may be
millilitre (pounds per gallon).
used.
10.1.3 Nonvolatiles:
11. Adhesive-Bonding Properties
10.1.3.1 Determine the nonvolatile content of Type A and
Type B from a 100-g mixture of adhesive and water (prepared
11.1 Block-Shear Strength (Compression) Tests:
by manufacturer’s instructions) and test in accordance with
11.1.1 Prepare and test specimens in accordance with Test
Test Method D 1490.
Method D 905. Use the adhesive manufacturer’s instructions
10.1.3.2 Determine the nonvolatile content of the uncata-
for conditions and procedures for preparing and spreading the
lyzed Type C liquid adhesive in accordance with Test Method
adhesive, and assembling, pressing, and curing of the assem-
D 1490.
bly. Use a two-week curing period unless otherwise instructed
10.1.4 pH of Cured Adhesive Film—Determine the pH of
by the adhesive manufacturer.
the cured adhesive film in accordance with Test Method
11.1.2 Number of Specimens—Test 20 specimens represent-
D 1583.
ing at least four assemblies.
10.1.5 Insoluble Matter—Determine the quantity of in-
11.1.3 Dry Shear Test—Condition one test group of 20
soluble matter in Type B adhesives, including filler and any
specimens to 10 to 12 % moisture content at 24 6 1°C (75 6
insoluble material, as a percentage of the nonvolatile constitu-
2°F) and test in accordance withTest Method D 905.Apply the
ents of the adhesive when determined as specified in 10.1.3.1.
load with a continuous motion of the movable loading head at
Weigh to the nearest milligram approximately2gof freshly
a rate of 12.7 mm (0.5 in.)/min (610 %).
mixed adhesive in a 100-mL beaker and add 50 mL of cold
NOTE 5—To obtain the desired moisture content refer to Table 3-4 on
solution of 20 parts by volume of glacial acetic acid and 80
page 3-8 of the Wood Handbook. Additional information is available in
parts by volume of distilled water. Stir the mixture thoroughly
Practice E 104. Constant temperature and relative humidity cabinets are
for 1 min and then add 0.500 6 0.001 g, acid-washed
available from laboratory supply companies.
diatomaceous earth (see Note 6). Stir the mixture for 2 min
11.1.4 Calculation—Calculate the shear stress at failure in
more and then filter through a fritted-glass crucible of medium
kilopascals per square inch by dividing the specimen’s break-
porosity with the aid of a vacuum. Transfer all residue to the
ing load by bond line area measured to the nearest 6.5
filter with a 20 % acetic acid solution. Wash the residue on the
2 2
mm (0.01 in. ).
filter with at least 50 mLof 20 % acetic acid and then with cold
11.2 Plywood Shear Tests (Tension):
distilled water to remove the acid. Dry the crucible in an oven
11.2.1 Prepare and test specimens in accordance with Test
at 124 6 3°C (255 6 5°C) for 1 to 1 ⁄2 h, cool in a desiccator,
Method D 906. Use the adhesive manufacturer’s instructions
and weigh to the nearest milligram. The insoluble content, as a
for conditions and procedures for preparing and spreading the
percentageofthenonvolatilecontent,isdeterminedasfollows:
adhesive, and for assembling, pressing, and curing of the
Percent insoluble 5 ~Weight of residue 2 0.500!
assembly. Use a two-week conditioning period unless other-
3 100/ Weight of adhesive 3 percent nonvolatile!
~
wise instructed by the adhesive manufacturer.
(1)
11.2.2 Number of Specimens:
11.2.2.1 Dry Tests—Prepare 20 specimens from two assem-
NOTE 3—“Filter-61” and “Celite Analytical Filter-Aid” have been
found satisfactory. Diatomaceous earth is prepared by acid-wash, oven
blies. Test in accordance with 11.2.3.1.
dried at 124 6 3°F (155 6 5°C) and then cooled in a desiccator.
11.2.2.2 Wet Tests—Prepare 20 specimens from two panels.
Test in accordance with 11.2.3.2.
10.1.6 Amylaceous Matter in Type B Adhesive—Add a drop
11.2.3 Exposure Conditions and Treatments:
of solution made from5gof iodine,5gof potassium iodide,
11.2.3.1 Dry Shear at 24°C (75°F)— Condition the speci-
and 100 mL of distilled water, to approximately 0.5 g of
mens
...