Designation: D 4426 – 01

Standard Test Method for

Determination of Percent Nonvolatile Content of Liquid
Phenolic Resins Used for Wood Laminating1
This standard is issued under the fixed designation D 4426; 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.

1. Scope NOTE 1—A glass dish may be used if the pH of the resin is greater than
ten.
1.1 This test method covers the recommended procedure for
the determination of the nonvolatile or total solids content of 6.2 Desiccator, charged with Drierite or equivalent desic-
liquid phenolic resins used for wood laminating. cant.
1.2 The values stated in SI units are to be regarded as the 6.3 Mechanical Convection Oven.
standard. The values given in parentheses are for information 6.4 Analytical Balance, accurate to 60.1 mg (0.000002 lb).
only. 6.5 Eye Droppers, or Dropping Pipettes, 2-mL capacity.
1.3 This standard does not purport to address all of the 6.6 Anemometer.
safety concerns, if any, associated with its use. It is the 6.7 Stainless Steel Trays, fabricated 30 gage, 83 by 250 mm
responsibility of the user of this standard to establish appro- (3.25 by 9.8 in.), with 19-mm (0.75-in.) sides and open ends.
priate safety and health practices and determine the applica- 6.8 Modified Oven Shelves, fitted with fabricated 18-gage
bility of regulatory limitations prior to use. 19 by 19-mm (0.75 by 0.75-in.) stainless steel angle stop
positioned 108 mm (4.25 in.) from back edge. Shelf-stop
2. Referenced Documents ensures consistent solids dish placement and prevents place-
2.1 ASTM Standards: ment at the rear of the oven where airflow is erratic.
D 907 Terminology of Adhesives2 6.9 Laboratory Hotplate, with heating capacity to 270°C
D 1582 Test Method for Nonvolatile Content of Liquid (518°F).
Phenol, Resorcinol, and Melamine Adhesives2
7. Oven Setup and Periodic Check Specifications
3. Terminology 7.1 Specifications:
3.1 Definitions:—Many of the terms in this test method are 7.1.1 Intake Port— 6.4 mm (0.25 in.) open.
defined in Terminology D 907. 7.1.2 Exhaust Port— 6.4 mm (0.25 in.) open.
7.1.3 Internal Airflow— 91.4 6 1 m/min (300 6 3 ft/min)
4. Summary of Test Method at 40°C (104°F).
4.1 A weighed specimen is oven-dried, cooled in a desicca- 7.1.4 Temperature— 125 6 1°C (257 6 2°F).
tor, and weighed. The percent nonvolatile content is calculated, 7.2 A 6.4-mm (0.25-in.) metal spacer is a convenient tool
based on the amount remaining. for setting port openings.
7.3 Measure with Davis-type anemometer placed as close as
5. Significance and Use possible to the geometric center of the cavity with the door
5.1 This test method is intended as a fast and economical shut.
determination of the nonvolatile content of liquid phenolic 7.4 Set the oven temperature at 125°C (257°F) and record
resins used for wood laminating and is useful for general the actual temperature for a period of 2 h. The control range
comparative purposes. For greater precision and accuracy, Test shall be 6 1°C (2°F) during the check period.
Method D 1582 is recommended.
8. Sampling
6. Apparatus 8.1 Take a representative sample of the lot of resin being
6.1 Disposable Aluminum Foil Dishes, 60-mm (2.4-in.) evaluated of a sufficient quantity for the tests. While the tests
diameter by 16-mm (0.60-in.) depth. consume less than 5 g (0.01 lb) of resin, a sample of at least
250 g (0.55 lb) is recommended to ensure that it is represen-
1
This test method is under the jurisdiction of ASTM Committee D14 on tative and that rechecks can be made if desired.
Adhesives and is the direct responsibility of Subcommittee D14.30 on Wood 8.2 To ensure that surface evaporation of solvent does not
Adhesives. affect the accuracy of the results, mix the resin sample
Current edition approved March 10, 2001. Published May 2001. Originally
published as D 4426 –84. Last previous edition D 4426 – 96 . thoroughly just prior to the test.
2
Annual Book of ASTM Standards, Vol 15.06.

Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.

1
 D 4426
9. Sample Dish Preparation Nonvolatile matter, % 5 ~A/B! 3 100
9.1 Inscribe an identifying number on each dish to be used where:
in the test. (Prepare three specimens from each sample.) A = net weight of dried residue, and
9.2 Place each dish on a hotplate set at 270°C (518°F) for B = net weight of liquid resin specimen.
about 15 s to flash off a thin coating of oil. (A whitish smoke 11.2 Calculate the average of the three specimens and report
will cease to be given off when all the oil has dissipated.)
the results to the one-hundredth percent (0.01). Report all
9.3 Place the heat-treated dishes in a desiccator for at least
results. If an individual specimen result varies more than
5 min.
60.5 % from the average, rerun the test set.
10. Procedure
10.1 Adjust oven to 125 6 1°C (257 6 2°F). 12. Report
10.2 Weigh a clean, previously numbered and heat-treated, 12.1 Report the results as percent of nonvolatile content.
aluminum dish to the nearest 0.1 mg (0.000002 lb) on an
analytical balance. 13. Precision and Bias
10.3 Using an eyedropper or dropping pipette, add approxi-
mately 1 g (0.002 lb) of resin to the center of the dish. (Allow 13.1 Precision—The precision of this test method varies
resin to remain as a “button.”) with resin type, solids content and caustic level. Four resins of
10.4 Reweigh the dish and resin to the nearest 0.1 mg varying type, solids level and caustic level were evaluated in a
(0.000002 lb). Weigh rapidly to minimize loss by evaporation. series of round-robin tests to determine repeatability and
10.5 Repeat 10.2-10.4 twice more for a total of three reproducibility of this test method. The data generated by these
specimens per resin sample. round-robin tests will be available at a later date.
10.6 Place dishes on a stainless steel tray and set the tray in 13.1.1 Repeatability—The average repeatability standard
the oven. Trays are positioned with tray side against shelf-step deviation has been determined to be 0.12 % (0.08–0.15), with
and parallel with airflow. Use only the top three shelf positions, an average repeatability at 95 % of 0.34 % (0.21–.43) for four
with no more than two trays of specimens per shelf. different resins.
10.7 Dry the specimens at 125 6 1°C (257 6 2°F) for 105 13.1.2 Reproducibility—The average reproducibility stan-
6 3 min. dard deviation has been determined to be 0.20 % (0.10–0.30),
10.8 Remove the dishes with the dried specimens and place with an average reproducibility at 95 % of 0.56 % (0.28–0.83)
in a desiccator to cool for at least 5, but not more than 15 min. for four different resin samples.
10.9 When cool, weigh each specimen as rapidly as possible 13.2 Bias—No information can be presented on the bias of
to the nearest 0.1 mg (0.000002 lb). Inspect each specimen the procedure in Test Method D 4226 for measuring phenolic
visually at the time of weighing. If any of the three specimens resin nonvolatile content because no material having an ac-
obviously deviates from the other two, or from usual normal
cepted reference value is available.
appearance, discard all three specimens and rerun the test.
11. Calculation 14. Keywords
11.1 Calculate the percent of nonvolatile matter as follows: 14.1 laminating; nonvolatile content; phenolic; resins; wood

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