ASTM D4690-99(2005)
(Specification)Standard Specification for Urea-Formaldehyde Resin Adhesives
Standard Specification for Urea-Formaldehyde Resin Adhesives
ABSTRACT
This specification covers three types of urea-formaldehyde thermosetting resin adhesives suitable for use on wood, wood-based substrates, or plastic laminates. The requirements for the adhesive are based on tests of physical properties including viscosity, density, nonvolatile content, pH, insoluble matter, amylaceous matter, mixing properties, working life, and on strength properties, including dry shear strength in lumber-type joints, dry and wet shear strength in plywood-type joints, and all strength tests at the end of the storage life certified by the manufacturer. Testing procedures are specified to differentiate between the physical and adhesive bonding properties of the many commercial urea-formaldehyde thermosetting resin and catalyst systems. The adhesive bonding properties are measured on maple block and birch plywood specimens, prepared and tested in accordance with prescribed methods.
SCOPE
1.1 This specification covers three types of urea-formaldehyde thermosetting resin adhesives suitable for use on wood, wood-based substrates, or plastic laminates.
1.2 The values stated in SI units are to be regarded as the standard. The values given in parentheses are provided for information only.
1.3 The requirements for the adhesive are based on tests of physical properties including viscosity, density, nonvolatile content, pH, insoluble matter, amylaceous matter, mixing properties, working life, and on strength properties, including dry shear strength in lumber-type joints, dry and wet shear strength in plywood-type joints, and all strength tests at the end of the storage life certified by the manufacturer.
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 and health practices and determine the applicability of regulatory limitations prior to use.
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D4690 −99(Reapproved2005)
Standard Specification for
Urea-Formaldehyde Resin Adhesives
This standard is issued under the fixed designation D4690; 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 three types of urea-
D1489 Test Method for Nonvolatile Content of Aqueous
formaldehyde thermosetting resin adhesives suitable for use on
Adhesives
wood, wood-based substrates, or plastic laminates.
D1490 Test Method for Nonvolatile Content of Urea-
1.2 The values stated in SI units are to be regarded as the
Formaldehyde Resin Solutions
standard. The values given in parentheses are provided for
D1583 Test Method for Hydrogen Ion Concentration of Dry
information only.
Adhesive Films
1.3 The requirements for the adhesive are based on tests of D1875 Test Method for Density ofAdhesives in Fluid Form
D2556 Test Method for Apparent Viscosity of Adhesives
physical properties including viscosity, density, nonvolatile
content, pH, insoluble matter, amylaceous matter, mixing Having Shear-Rate-Dependent Flow Properties
D5266 Practice for Estimating the Percentage of Wood
properties, working life, and on strength properties, including
dry shear strength in lumber-type joints, dry and wet shear Failure in Adhesive Bonded Joints
E70 Test Method for pH of Aqueous Solutions With the
strengthinplywood-typejoints,andallstrengthtestsattheend
of the storage life certified by the manufacturer. Glass Electrode
E104 Practice for Maintaining Constant Relative Humidity
1.4 The following safety hazards caveat pertains only to the
by Means of Aqueous Solutions
test method portion, Sections 8 through 13, of this specifica-
tion: This standard does not purport to address all of the safety 2.2 Federal Specifications:
concerns, if any, associated with its use. It is the responsibility
PPP-C-96 Cans, Metal, 28 Gage and Lighter
of the user of this standard to establish appropriate safety and PPP-D-723 Drums, Fiber
health practices and determine the applicability of regulatory PPP-D-729 Drums, Shipping and Storage, Steel, 55-gal
limitations prior to use.
(208-L)
2.3 Federal Standard:
2. Referenced Documents
FED-STD-123 Marking for Shipment
2.1 ASTM Standards:
2.4 Military Standard:
B417 Test Method for Apparent Density of Non-Free-
MIL-STD-129 Marking for Shipment and Storage
Flowing Metal Powders Using the Carney Funnel
D905 Test Method for Strength Properties of Adhesive
3. Terminology
Bonds in Shear by Compression Loading
D906 Test Method for Strength Properties of Adhesives in 3.1 Definitions—Many terms in this specification are de-
Plywood Type Construction in Shear by Tension Loading
fined in Terminology D907.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 adhesive designation—an adhesive that is manufac-
This specification is under the jurisdiction of ASTM Committee D14 on
tured by a unique combination of raw materials and manufac-
Adhesives and is the direct responsibility of Subcommittee D14.30 on Wood
Adhesives.
turing process that conforms to a given set of physical and
Current edition approved April 1, 2005. Published April 2005. Originally
performance properties and is identified by specific name,
approved in 1987. Last previous edition approved in 1999 as D4690 – 99. DOI:
number, or alphanumeric designation.
10.1520/D4690-99R05.
This specification is intended as a replacement for Federal Specification
MMM-A-188c, Adhesive; Urea Resin Type (Liquid and Powder).
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,
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D4690−99(2005)
3.2.2 lot—adhesive manufactured at one place from the 6.2 To meet the storage-life requirements, an initial lot of
same batch or blends of raw materials subjected to the same the adhesive shall be tested in accordance with Sections 10 and
operations and conditions. 11. It shall pass all test requirements after being stored under
conditions and time specified by the manufacturer. Following
NOTE 1—In this specification, the maple block lamination in Test
this initial test, certification shall be based on submission from
Method D905 and the birch plywood construction in Test Method D906
the manufacturer.
are described as assemblies.
6.3 The curing agent for Types A and C shall readily
4. Significance and Use
disperse in the adhesive mixture when used in accordance with
4.1 Thisspecificationprovidestestingproceduresandspeci-
the manufacturer’s recommendation.
fies requirements to differentiate between the physical and
6.4 The filler shall neither dissolve nor swell excessively in
adhesive bonding properties of the many commercial urea-
water, and shall not settle from the adhesive mixture during the
formaldehyde thermosetting resin and catalyst systems.
working life.
4.2 Because of the diverse nature of products bonded with
these adhesives, testing by this specification will only evaluate 7. Retest and Rejection
the adhesive under a given set of conditions. The physical
7.1 When a specimen fails at a load less than that specified,
properties of the adhesive are measured to provide information
if the wood failure is 50 % or greater, that specimen shall be
on certain handling and working properties. The adhesive-
disregardedincomputingtheaverage.Ifmorethanonethirdof
bonding properties are measured on maple block and birch
the test specimens for any one test condition are discarded for
plywood specimens, prepared and tested in accordance with
this reason, the test shall be repeated.
Test Method D905 and Test Method D906, respectively. The
7.2 If the results of any initial test do not conform to the
certification requirements have been based on knowledge
requirements prescribed in this specification, that test shall be
within the industry of values that may be expected. Test
repeated on an additional set of specimens made from the same
Method D905 and Test Method D906 have a long history of
lot of adhesive, each set of which shall conform to the
use in many specifications.
requirementsspecified.Ifthissetofspecimensfailstomeetthe
4.3 The stress calculated by using this specification should
requirements, the lot shall be rejected.
not be used to predict failure nor should it be used for design
stress in joints with different geometry or loading direction
TEST METHODS
different from the test geometry.
8. Significance and Use
5. Classification
8.1 This specification provides testing procedures to differ-
5.1 Urea resin adhesive shall be furnished as one of the entiate between the physical and adhesive bonding properties
of the many commercial urea-formaldehyde thermosetting
following types:
5.1.1 Type A—Powder with separate curing agent. resin and catalyst systems.
5.1.2 Type B—Powder with incorporated curing agent.
9. Sampling
5.1.3 Type C—Liquid with separate curing agent.
9.1 Take a representative, 2-L (2-qt) sample of adhesive
NOTE 2—Type A, Type B, and Type C replace the Type I, Type II, and
from the lot to be tested. Divide the sample into two equal
Type III classifications of Federal Specification MMM-A-188C, respec-
portions and place each in a wide mouth, glass, 1-L (1-qt)
tively, to prevent confusion with Type I (boil test) and Type II (cold-water
soak) classifications used in existing ASTM standards for adhesives.
container and seal tightly. Use one of the samples for tests of
physical and adhesive bond properties (Sections 10 and 11),
6. Test Requirements
and use the other for testing storage life (11.2.3.3), and for any
6.1 To meet the requirements of this specification, the urea
retesting that may be necessary under Section 7. Also, take
resin and adhesive mix shall be subjected to the tests listed in
sufficient quantity of curing agent to cure the adhesive samples
Section 10. In addition, the adhesive shall meet the require-
and place in a separate, clean, dry container. Seal all sample
ments of the tests described in Section 11 and as listed in Table
containers with well-fitting, corrosion-resistant lids.
1.
10. Physical Properties
10.1 Test the physical properties of adhesives by the fol-
TABLE 1 Test Requirements
lowing test methods:
Test Requirement
Test Section Number
(Minimum) 10.1.1 Viscosity:
Block shear (compression)
10.1.1.1 Measure the viscosity of the liquid urea resin or
Dry at 24°C (75°F) 11.1 19 306 kPa (2800 psi)
adhesive mixtures in accordance with Test Methods D1084 or
Plywood shear (tension)
D2556.
Dry at 24°C (75°F) 11.2.3.1 2 344 kPa (340 psi)
48-h soak 11.2.3.2 1 930 kPa (280 psi)
10.1.1.2 Temperature of Test—Condition to, and maintain
A
Storage life 11.2.3.3
the liquid urea resin or adhesive mixture at 24 6 0.5°C (75 6
A
A retained sample of the initial lot of the adhesive shall be tested and shall meet
1°F) during the viscosity reading. Other temperatures may be
the requirements of all tests listed in 6.2 for the applicable type of adhesive after
used upon agreement between the contracting parties, but the
the storage life time certified by the manufacturer.
60.5°C (61°F) tolerance must be observed.
D4690−99(2005)
10.1.1.3 For Type C adhesives requiring the addition of a or blade.Allow the beaker to stand without a cover in air at 24
curing agent, make two viscosity measurements of the test 6 2.5°C (75 6 5°F). If necessary, place in a water bath to
adhesives (1) before the addition of curing agent, and (2) after obtain the proper temperature. Stir the adhesive frequently and
the addition of the curing agent. The viscosity of urea resins note the time at which the adhesive is considered no longer
following addition of curing agent to liquid resin is time- spreadable. At the end of the working life, note whether the
dependent. Make the measurement 10 min after mixing. adhesive is in a homogeneous condition. In case of doubt as to
10.1.2 Density: whether the adhesive is spreadable, test the adhesive at 24 6
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 B417, 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 D1875 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 D1490.
Method D905. 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-
D1490.
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-
D1583.
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 with Test Method D905.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 E104. 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 2
ing load by bond line area measured to the nearest 6.5 mm
filter with a 20 % acetic acid solution. Wash the residue on the 2
(0.01 in. ).
filterwithatleast50mLof20 %aceticacidandthenwithcold
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 D906. 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 (1)
~ !
assembly. Use a two-week conditioning period unless other-
wise instructed by the adhesive manufacturer.
3100/ Weight of adhesive 3percent nonvolatile
~ !
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 sat
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