1、Designation: D1259 06 (Reapproved 2012)Standard Test Methods forNonvolatile Content of Resin Solutions1This standard is issued under the fixed designation D1259; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revi
2、sion. A number in parentheses indicates the year of last reapproval. Asuperscript 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. Scope1.1 These test methods cover the determination of
3、nonvola-tile content of solutions of resins in volatile organic solvents.1.2 Two test methods are included as follows:1.2.1 Test Method AFor solutions of non-heat-reactiveresins. These solutions contain resins that remain stable andrelease the solvent under conditions of the test. Examples areester
4、gums and alkyds.1.2.2 Test Method BFor two types of solutions:1.2.2.1 Solutions of heat-reactive resins. These solutionscontain resins that undergo condensation or other reactionsunder the influence of heat. Examples include the formalde-hyde reaction products of urea, melamine, and phenols.1.2.2.2
5、Solutions that release solvent slowly. Examplesinclude epoxy resin solutions.1.3 Test Methods A and B differ primarily in the dryingtimes and types of oven used.1.4 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.5 This stand
6、ard does not purport to address all of thesafety concerns, if any, 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. Summary of Test Methods2.1
7、 In both test methods, a weighed specimen of resinsolution is spread under pressure between two weighed sheetsof aluminum or tin foil. The coated foil sheets are separatedand then dried. The weight of residue is determined and thenonvolatile content is calculated. The test method is unique inthat it
8、 provides for drying of a very thin film of resin, thusminimizing chances for volatiles to be trapped and held duringthe heating operation.2.2 Either a gravity-convection or a forced-ventilation ovenand a 30-min heating period at 105C are used in Test MethodA.2.3 A forced-ventilation oven and a 2-h
9、heating period at105C are used in Test Method B.3. Significance and Use3.1 The nonvolatile content of resin solutions is useful tocoatings producers and users for the determination of the totalsolids available for film formation and for the estimation of thevolatile organic content.TEST METHOD ANON-
10、HEAT-REACTIVE RESINSOLUTIONS4. Apparatus4.1 Ovens:4.1.1 Gravity-convection type, maintained at 105 6 2C,with vents open.4.1.2 Forced-ventilation type, maintained at 105 6 2C. Forovens with adjustable air flow rate, set the control damper at50 %.4.2 Aluminum or Tin Foil, from 38 to 50 m (0.0015 to0.0
11、020 in.) in thickness. Either one piece 150 by 300 mm (6 by12 in.), or two 150 by 150-mm (6 by 6-in.) pieces may be used.The foil must be perfectly smooth; if it becomes wrinkledduring the initial handling, roll smooth as directed in 5.2.4.3 Plate GlassTwo pieces about 5 mm (316 in.) thick; onepiece
12、 140 by 140 mm (512 by 512 in.) and one piece 180 by 180mm (7 by 7 in.).4.4 Device for Weighing Specimens2Apparatus that willprevent loss of volatile matter during the weighing operationsuch as any of the following, or equivalent:4.4.1 Syringe, Luer, 2 or 5-mL capacity,4.4.2 Weighing Buret, Smith, 1
13、0-mL capacity, or4.4.3 Bulb Pipet, dropping, with 50-mL Erlenmeyer flask.1These test methods are under the jurisdiction of ASTM Committee D01 onPaint and Related Coatings, Materials, and Applications and are the directresponsibility of Subcommittee D01.21 on Chemical Analysis of Paints and PaintMate
14、rials.Current edition approved June 1, 2012. Published July 2012. Originally approvedin 1953. Last previous edition approved in 2006 as D1259 06. DOI: 10.1520/D1259-06R12.2The bulb pipet is available from most scientific supply houses.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700,
15、 West Conshohocken, PA 19428-2959. United States14.5 Roller, for Smoothing FoilUse a ground and polishedcylinder, preferably stainless steel, approximately 7 in. (180mm) long and 2 in. (50 mm) in diameter.4.6 Foil Trays, two types as follows:4.6.1 Trays measuring 165 by 300 mm (612 by 12 in.) , foru
16、se with (6 by 12-in.) foil, constructed from No. 22-gauge0.6mm aluminum sheet in accordance with dimensions shownin Fig. 1. Several trays may be stacked in the oven to permitrunning several specimens simultaneously.4.6.2 Trays measuring 165 by 165 mm (612 by 612 in.), foruse with (6 by 6-in.) foil,
17、with holder, shall be constructed fromNo. 22-gauge aluminum sheet, as shown in Fig. 2.5. Procedure5.1 Use the following procedure with the 150 by 300-mm (6 by 12-in. ) foil sheets and the 165 by 300-mm (612 by12-in.) trays.Alternatively two 150 by 150-mm (6 by 6-in.) foilsheets may be used in a simi
18、lar manner with the 165 by165-mm (612 by 612-in.) trays. In handling the foil, avoidwrinkling or creasing the sheets until after the specimen hasbeen dried. Sheets may be rolled for convenience of handlingand making the initial weighing, but must be kept smooththroughout the pressing and drying oper
19、ations.5.2 Weigh the foil to 0.1 mg. Open and place half the foil,with the shiny side up, on the 180 by 180-mm (7 by 7-in.) glassplate. If necessary, roll smooth with the metal roller. By meansof the weighing device, weigh by difference a 0.9 to 1.1-gspecimen of the resin solution, to 0.1 mg. Place
20、the specimenon the center of that area of the foil covering the glass plate.Place the other half of the foil on top. Cover the foil with thesecond glass plate, centering the glass on the foil, and pressdown sufficiently to cause the specimen to spread uniformlyinto a thin film, about 75 mm (3 in.) i
21、n diameter. The pressurethat must be exerted depends on the viscosity of the sample. Incase a specimen of low viscosity should extend beyond theedge of the foil, repeat the determination, allowing a fewminutes for a portion of the solvent to evaporate from theweighed specimen before covering and pre
22、ssing it.5.3 After pressing, open the foil to its full length and placeit in the foil tray. Place the tray in either a gravity-convectionor a forced-ventilation oven at 105 6 2C for 30 min.5.4 Remove the tray from the oven and then carefullyremove the foil sheet from the tray. Return the dried films
23、urfaces to the face-to-face position. While the foil is stillwarm, fold the edges together to enclose completely the driedfilm. Without undue delay, weigh to 0.1 mg.6. Calculation6.1 Calculate the percent nonvolatile content, C, as follows:C 5 A 2 B! 3100#/Swhere:A = weight of foil plus dried solids
24、, g,B = weight of foil, g, andS = weight of sample taken, g.7. Precision and Bias7.1 The following criteria should be used for judging theacceptability of results at the 95 % confidence level:7.1.1 RepeatabilityThe difference between two results,each the mean of duplicate determinations obtained by
25、thesame analyst, is normally about 0.2 %, absolute. Two suchresults should be considered suspect if they differ by more than0.5 %, absolute.7.1.2 ReproducibilityThe difference between two results,each the mean of duplicate determinations, obtained by ana-lysts in different laboratories is normally a
26、bout 0.4 %, absolute.Two such results should be considered suspect if they differ bymore than 1.0 %, absolute.7.1.3 No bias has been determined for this test method.NOTE 1Millimetre dimensions appear in section on Apparatus.FIG. 1 Tray for 150 by 300-mm (6 by 12-in.) FoilD1259 06 (2012)2TEST METHOD
27、BHEAT-REACTIVE RESINSOLUTIONS AND SOLUTIONS THAT RELEASESOLVENT SLOWLY8. Apparatus8.1 OvenForced-ventilation type, maintained at 105 62C. For ovens with adjustable air flow rate, set the controldamper at 50 %.8.2 The remainder of the apparatus is identical with thatgiven in 4.2-4.6.9. Procedure9.1 W
28、eigh the specimen of resin solution and press itbetween two sheets of foil as described in 5.1 and 5.2.9.2 After pressing, open the foil to its full length and placeit in the foil tray. Then place the tray in a forced-ventilationoven at 105 6 2C for 2 h. When using 150 by 150mm (612by 612-in.) trays
29、 and holder, place the assembly in the ovenwith the open ends perpendicular to the direction of air flow.9.3 Complete the determination as described in 5.4.10. Calculation10.1 Calculate the nonvolatile content as described in Sec-tion 6.11. Precision and Bias11.1 The following criteria should be use
30、d for judging theacceptability of results at the 95 % confidence level.11.1.1 For Heat-Reactive Resin Solutions:11.1.1.1 RepeatabilityThe difference between two results,each the mean of duplicate determinations obtained by thesame analyst, is normally about 0.3 %, absolute. Two suchresults should be
31、 considered suspect if they differ by more than0.7 %, absolute.11.1.1.2 ReproducibilityThe difference between two re-sults, each the mean of duplicate determinations obtained byanalysts in different laboratories, is normally about 0.7 %,absolute. Two such results should be considered suspect if they
32、differ by more than 1.7 %, absolute.11.1.1.3 No bias has been determined for this test method.11.1.2 For Solutions that Release Solvent Slowly:11.1.2.1 RepeatabilityThe average difference betweentwo results each the average of duplicate determinations,obtained by the same analyst is normally about 0
33、.1 %, absolute.Two such results should be considered suspect if they differ bymore than 0.3 %, absolute.11.1.2.2 ReproducibilityThe average difference betweentwo results obtained by analysts in different laboratories willapproximate 0.2 %. Two such results should be consideredsuspect if they differ
34、by more than 0.5 %, absolute.11.1.2.3 Bias cannot be determined for this method becausethere are no acceptable reference standards.12. Keywords12.1 foil method; heat-reactive; non-heat-reactive; nonvola-tile; resin solutionFIG. 2 Trays and Holder for 150 by 150-mm (6 by 6-in.) FoilD1259 06 (2012)3AS
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