1、Designation: D 4426 01 (Reapproved 2006)Standard Test Method forDetermination of Percent Nonvolatile Content of LiquidPhenolic Resins Used for Wood Laminating1This standard is issued under the fixed designation D 4426; the number immediately following the designation indicates the year oforiginal ad
2、option or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the recommended procedure forthe determinatio
3、n of the nonvolatile or total solids content ofliquid phenolic resins used for wood laminating.1.2 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.3 This standard does not purport to address all of thesafety concerns, if any,
4、 associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 907 Terminology of AdhesivesD 1582 Test Method for
5、 Nonvolatile Content of LiquidPhenol, Resorcinol, and Melamine Adhesives3. Terminology3.1 DefinitionsMany of the terms in this test method aredefined in Terminology D 907.4. Summary of Test Method4.1 A weighed specimen is oven-dried, cooled in a desicca-tor, and weighed. The percent nonvolatile cont
6、ent is calculated,based on the amount remaining.5. Significance and Use5.1 This test method is intended as a fast and economicaldetermination of the nonvolatile content of liquid phenolicresins used for wood laminating and is useful for generalcomparative purposes. For greater precision and accuracy
7、, TestMethod D 1582 is recommended.6. Apparatus6.1 Disposable Aluminum Foil Dishes, 60-mm (2.4-in.)diameter by 16-mm (0.60-in.) depth.NOTE 1A glass dish may be used if the pH of the resin is greater thanten.6.2 Desiccator, charged with Drierite or equivalent desic-cant.6.3 Mechanical Convection Oven
8、.6.4 Analytical Balance, accurate to 60.1 mg (0.000002 lb).6.5 Eye Droppers, or Dropping Pipettes, 2-mL capacity.6.6 Anemometer.6.7 Stainless Steel Trays, fabricated 30 gauge, 83 by 250mm (3.25 by 9.8 in.), with 19-mm (0.75-in.) sides and openends.6.8 Modified Oven Shelves, fitted with fabricated 18
9、-gauge19 by 19-mm (0.75 by 0.75-in.) stainless steel angle stoppositioned 108 mm (4.25 in.) from back edge. Shelf-stopensures consistent solids dish placement and prevents place-ment at the rear of the oven where airflow is erratic.6.9 Laboratory Hotplate, with heating capacity to 270C(518F).7. Oven
10、 Setup and Periodic Check Specifications7.1 Specifications:7.1.1 Intake Port6.4 mm (0.25 in.) open.7.1.2 Exhaust Port6.4 mm (0.25 in.) open.7.1.3 Internal Airflow91.4 6 1 m/min (300 6 3 ft/min) at40C (104F).7.1.4 Temperature125 6 1C (257 6 2F).7.2 A 6.4-mm (0.25-in.) metal spacer is a convenient too
11、lfor setting port openings.7.3 Measure with Davis-type anemometer placed as close aspossible to the geometric center of the cavity with the doorshut.7.4 Set the oven temperature at 125C (257F) and recordthe actual temperature for a period of 2 h. The control rangeshall be 61C (2F) during the check p
12、eriod.8. Sampling8.1 Take a representative sample of the lot of resin beingevaluated of a sufficient quantity for the tests. While the testsconsume less than 5 g (0.01 lb) of resin, a sample of at least1This test method is under the jurisdiction of ASTM Committee D14 onAdhesives and is the direct re
13、sponsibility of Subcommittee D14.30 on WoodAdhesives.Current edition approved Oct. 1, 2006. Published October 2006. Originallyapproved in 1984. Last previous edition approved in 2001 as D 4426 01.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at
14、 serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.250 g (0.55 lb) is recommended to ensure that it i
15、s represen-tative and that rechecks can be made if desired.8.2 To ensure that surface evaporation of solvent does notaffect the accuracy of the results, mix the resin samplethoroughly just prior to the test.9. Sample Dish Preparation9.1 Inscribe an identifying number on each dish to be usedin the te
16、st. (Prepare three specimens from each sample.)9.2 Place each dish on a hotplate set at 270C (518F) forabout 15 s to flash off a thin coating of oil. (A whitish smokewill cease to be given off when all the oil has dissipated.)9.3 Place the heat-treated dishes in a desiccator for at least5 min.10. Pr
17、ocedure10.1 Adjust oven to 125 6 1C (257 6 2F).10.2 Weigh a clean, previously numbered and heat-treated,aluminum dish to the nearest 0.1 mg (0.000002 lb) on ananalytical balance.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
18、resin to remain as a “button.”)10.4 Reweigh the dish and resin to the nearest 0.1 mg(0.000002 lb). Weigh rapidly to minimize loss by evaporation.10.5 Repeat 10.2-10.4 twice more for a total of threespecimens per resin sample.10.6 Place dishes on a stainless steel tray and set the tray inthe oven. Tr
19、ays are positioned with tray side against shelf-stepand parallel with airflow. Use only the top three shelf positions,with no more than two trays of specimens per shelf.10.7 Dry the specimens at 125 6 1C (257 6 2F) for 1056 3 min.10.8 Remove the dishes with the dried specimens and placein a desiccat
20、or to cool for at least 5, but not more than 15 min.10.9 When cool, weigh each specimen as rapidly as possibleto the nearest 0.1 mg (0.000002 lb). Inspect each specimenvisually at the time of weighing. If any of the three specimensobviously deviates from the other two, or from usual normalappearance
21、, discard all three specimens and rerun the test.11. Calculation11.1 Calculate the percent of nonvolatile matter as follows:Nonvolatile matter, % 5 A/B! 3 100where:A = net weight of dried residue, andB = net weight of liquid resin specimen.11.2 Calculate the average of the three specimens and report
22、the results to the one-hundredth percent (0.01). Report allresults. If an individual specimen result varies more than60.5 % from the average, rerun the test set.12. Report12.1 Report the results as percent of nonvolatile content.13. Precision and Bias13.1 PrecisionThe precision of this test method v
23、arieswith resin type, solids content and caustic level. Four resins ofvarying type, solids level and caustic level were evaluated in aseries of round-robin tests to determine repeatability andreproducibility of this test method. The data generated by theseround-robin tests will be available at a lat
24、er date.13.1.1 RepeatabilityThe average repeatability standarddeviation has been determined to be 0.12 % (0.080.15), withan average repeatability at 95 % of 0.34 % (0.21.43) for fourdifferent resins.13.1.2 ReproducibilityThe average reproducibility stan-dard deviation has been determined to be 0.20
25、% (0.100.30),with an average reproducibility at 95 % of 0.56 % (0.280.83)for four different resin samples.13.2 BiasNo information can be presented on the bias ofthe procedure in Test Method D 4226 for measuring phenolicresin nonvolatile content because no material having an ac-cepted reference value
26、 is available.14. Keywords14.1 laminating; nonvolatile content; phenolic; resins; woodASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of t
27、he validity of any such patent rights, and the riskof 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 andif not revised, either reapproved or withdrawn. Yo
28、ur comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comment
29、s have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).D 4426 01 (2006)2
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