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Astm D4690 - 1 (En)
Astm D4690 - 1 (En)
This standard has been approved for use by agencies of the Department of Defense.
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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 This specification provides testing procedures and speci- 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.
4.2 Because of the diverse nature of products bonded with 7. Retest and Rejection
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 disregarded in computing the average. If more than one third of
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 requirements specified. If this set of specimens fails to meet the
use in many specifications. requirements, the lot shall be rejected.
4.3 The stress calculated by using this specification should
not be used to predict failure nor should it be used for design TEST METHODS
stress in joints with different geometry or loading direction
different from the test geometry. 8. Significance and Use
8.1 This specification provides testing procedures to differ-
5. Classification entiate between the physical and adhesive bonding properties
5.1 Urea resin adhesive shall be furnished as one of the of the many commercial urea-formaldehyde thermosetting
following types: resin and catalyst systems.
5.1.1 Type A—Powder with separate curing agent.
9. Sampling
5.1.2 Type B—Powder with incorporated curing agent.
5.1.3 Type C—Liquid with separate curing agent. 9.1 Take a representative, 2-L (2-qt) sample of adhesive
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-
tively, to prevent confusion with Type I (boil test) and Type II (cold-water container and seal tightly. Use one of the samples for tests of
soak) classifications used in existing ASTM standards for adhesives. physical and adhesive bond properties (Sections 10 and 11),
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
6.1 To meet the requirements of this specification, the urea sufficient quantity of curing agent to cure the adhesive samples
resin and adhesive mix shall be subjected to the tests listed in and place in a separate, clean, dry container. Seal all sample
Section 10. In addition, the adhesive shall meet the require- containers with well-fitting, corrosion-resistant lids.
ments of the tests described in Section 11 and as listed in Table
1. 10. Physical Properties
6.2 To meet the storage-life requirements, an initial lot of 10.1 Test the physical properties of adhesives by the fol-
the adhesive shall be tested in accordance with Sections 10 and lowing test methods:
11. It shall pass all test requirements after being stored under 10.1.1 Viscosity:
conditions and time specified by the manufacturer. Following 10.1.1.1 Measure the viscosity of the liquid urea resin or
this initial test, certification shall be based on submission from adhesive mixtures in accordance with Test Methods D 1084 or
the manufacturer. D 2556.
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)
Plywood shear (tension) curing agent, make two viscosity measurements of the test
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)
Storage life 11.2.3.3 A the addition of the curing agent. The viscosity of urea resins
A
following addition of curing agent to liquid resin is time-
A retained sample of the initial lot of the adhesive shall be tested and shall meet
the requirements of all tests listed in 6.2 for the applicable type of adhesive after dependent. Make the measurement 10 min after mixing.
the storage life time certified by the manufacturer. 10.1.2 Density:
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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:
10.1.3.1 Determine the nonvolatile content of Type A and 11. Adhesive-Bonding Properties
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 with Test 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 approximately 2 g of 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.7 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 mm2(0.01 in.2 ).
filter with at least 50 mL of 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 11⁄2 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
percentage of the nonvolatile content, is determined as follows: 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:
NOTE 3—“Filter-61” and “Celite Analytical Filter-Aid” have been 11.2.2.1 Dry Tests—Prepare 20 specimens from two assem-
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.
10.1.6 Amylaceous Matter in Type B Adhesive—Add a drop Test in accordance with 11.2.3.2.
of solution made from 5 g of iodine, 5 g of potassium iodide, 11.2.3 Exposure Conditions and Treatments:
and 100 mL of distilled water, to approximately 0.5 g of 11.2.3.1 Dry Shear at 24°C (75°F)— Condition the speci-
adhesive mix on a porcelain spot plate or watch glass. A mens to 10 to 12 % moisture content at 24 6 1°C (75 6 2°F)
darkening of the mixture denotes the presence of amylaceous and test in accordance with Test Method D 906.
matter. 11.2.3.2 Forty-Eight-Hour Soak—Immerse the test speci-
10.1.7 Mixing Properties and Working Life, Mix approxi- mens in water 24 6 1°C (75 6 2°F) and soak them for 48 h 6
mately 200 g of adhesive (in accordance with the manufactur- 15 min. Remove the specimens from the water and test them
er’s instruction) in a 400-mL beaker (Note 6) with a stirring rod immediately as specified in Test Method D 906. Report indi-
or blade. Allow the beaker to stand without a cover in air at 24 vidual and average test values.
6 2.5°C (75 6 5°F). If necessary, place in a water bath to 11.2.3.3 Storage Life, Store the 1-L sample of adhesive
obtain the proper temperature. Stir the adhesive frequently and collected in Section 9 at 24 6 1°C (756 2°F) for the period of
note the time at which the adhesive is considered no longer
spreadable. At the end of the working life, note whether the 7
“Moisture Content of Wood in Equilibrium with Dry-Bulb Temperature and
adhesive is in a homogeneous condition. In case of doubt as to Relative Humidity,” Wood Handbook, No. 72, Forest Products Laboratory, United
whether the adhesive is spreadable, test the adhesive at 24 6 States Department of Agriculture, Revised August 1974, Table 3–4, pp. 3–8.
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D 4690
time indicated by the manufacturer as the storage life of the 16.1.1 Preparation for Delivery—Packaging and packing is
adhesive. After storage, test for the requirements listed in Table Level A, B, or commercial as specified.
1. Report the length of the storage period. 16.1.2 Unless otherwise specified, when Level A or B is
specified, packaging and packing should be in accordance with
NOTE 6—The storage life of adhesives will be reduced at an unaccept-
able rate at temperatures above 27°C (80°F). the following criteria:
16.1.2.1 Metal containers conforming to PPP-C-96, Type V,
12. Report class 2 for quantities of 50 lb (22.7 kg), maximum.
12.1 Report values for the physical properties tested in 16.1.2.2 Fiber drums conforming to PPP-D-723, Type II,
Section 10. grade A or Type III, grade A for Level A, or fiber drums
12.1.1 Report the temperature at which working life and conforming to PPP-D-723, Type I, grade A for Level B, for
viscosity were measured, that is either 23°C (73°F) or 32°C quantities of 90.9 kg (200 lb), maximum.
(90°F). 16.1.2.3 Metal drums conforming to PPP-C-729, Type II or
12.2 For the adhesive-bond test, Section 11, report indi- Type IV for quantities of 181.4 kg (400 lb), maximum.
vidual and average test values, and the estimated percentages 16.2 Containers:
of wood failure for all specimens. 16.2.1 Containers should be uniform in shape and size, with
12.3 As a part of the report, include: the necessary protection required. Containers should contain
12.3.1 The manufacturer’s recommended allowable storage quantities in accordance with the applicable container spec-
period. ification. All fiber drums shall be furnished with a 0.1-mm
12.3.2 Mix-ratio used if the adhesive is a two-or-more- (0.004-in.) thick polyethylene liner, properly heat sealed.
component system. 16.2.2 Drums, as specified in PPP-D-723 or PPP-D-729,
12.3.3 Certification by the manufacturer that the adhesive will require no overpacking.
system meets the requirements of 6.3 and 6.4 as applicable. 16.3 Shipment and Delivery—Unless otherwise specified,
12.3.4 Certification by the manufacturer that the adhesive when Level C is specified, the adhesive, 113 g to 136 kg (4 oz
passes all tests at the end of the recommended allowable to 300 lb), should be packaged in containers to offer adequate
storage period. protection against corrosion, deterioration and damage during
shipment, handling and storage and should be packed to assure
13. Precision and Bias safe delivery to its destination when properly transported by
13.1 The precision and bias of the test methods measuring any common carrier in conformance to requirements by
block shear strength (compression) and plywood shear strength Uniform Freight Classification or National Motor Freight
are essentially as specified in Test Methods D 905 and D 906. Classification.
13.2 The precision and bias of Test Methods D 1084, D 16.4 Marking:
1490, D 1583, D 1875 and D 2556 are being determined and 16.4.1 Marking should be as specified in the contract or
will be available when next balloted but no later than Decem- purchase order. Interior packages and shipping containers
ber 2003. should be marked in accordance with Fed-Std-123 for civilian
agencies or in accordance with MIL-STD-129 for military
OTHER REQUIREMENTS agencies.
NOTE 7—The requirements mandated by the Department of Defense 16.4.2 Special markings when specified, in contracts, pur-
(DOD) have not been revised since publication of this specification. It is chase orders, or by the contracting officer shall include:
recommended that any manufacturer certifying to this specification 16.4.2.1 Manufacturer’s name, product code designation,
consult with DOD to determine if any regulations have been added, and batch or lot number, and the national stock number.
revised, or deleted since the original publishing date. 16.4.2.2 Date of manufacture of product and expiration
date.
14. Keywords
16.4.2.3 Special-handling instructions during product trans-
14.1 adhesives; density; insoluble matter; nonvolatile con- fer.
tent; urea formaldehyde; viscosity 16.4.2.4 Special precautions related to toxicity, flammabil-
15. Labeling ity or to any information pertinent to the proper handling and
storage of the product, for example, manufacturer’s storage
15.1 Include as part of the label, or advise consultation of, temperature range.
data sheet for the following:
15.1.1 An indication as to whether the adhesive is ready to 17. Packing and Marking Requirements for
use or if a curing agent must be added, along with any special Nongovernmental Users
instructions needed. 17.1 The following sections shall apply to nongovernmental
15.1.2 An expiration date for storage life. users of this specification, subject to the given exceptions: 16.3
(except for reference to Level C), 16.4.2 (whether or not
16. Supplemental Government Requirements specified), 16.4.2.1 (except for the national stock number),
16.1 Packaging and Packing: 16.4.2.2, 16.4.2.3 and 16.4.2.4.
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D 4690
APPENDIX
(Nonmandatory Information)
X1.1 Test Method B 417 covers the use of a standard funnel until the cup overflows. After leveling the powder in the cup,
that feeds powder into a density cup. The bottom of the funnel the density is determined. Care should be taken not to jar the
and the top of the cup are 1.0 in. apart. A standard wire can be apparatus and effect compaction by vibration.
used to assist feeding of the powder through the funnel orifice
The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted in connection
with any item mentioned in this standard. Users of this standard are expressly advised that determination of the validity of any such
patent rights, and the risk of infringement of such rights, are entirely their own responsibility.
This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM Headquarters. Your comments will receive careful consideration at a meeting of the responsible
technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should make your
views known to the ASTM Committee on Standards, 100 Barr Harbor Drive, West Conshohocken, PA 19428.