1、Designation: D1259 06 (Reapproved 2018)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 U.S. Department of Defense.1. Scope1.1 These test methods cover the determinatio
3、n of 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 aree
4、ster 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
5、2.2 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
6、standard 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, health, and environmental practices and deter-mine the applicability of regulatory limitations prior to use.1.6 This
7、 international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (
8、TBT) Committee.2. Summary of Test Methods2.1 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 cal
9、culated. The test method is unique inthat it 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 Meth
10、odA.2.3 A forced-ventilation oven and a 2-h 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 t
11、hevolatile organic content.TEST METHOD ANON-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 Aluminu
12、m or Tin Foil, from 38 to 50 m (0.0015 to0.0020 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
13、 pieces about 5 mm (316 in.) thick; onepiece 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:1These test methods are un
14、der 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 PaintMaterials.Current edition approved June 1, 2018. Published June 2018. Originallyapproved in 1953. Last
15、previous edition approved in 2012 as D1259 06 (2012).DOI: 10.1520/D1259-06R18.2The bulb pipet is available from most scientific supply houses.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in
16、accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.14.4.1 Syringe, Luer, 2 or 5
17、mL capacity,4.4.2 Weighing Buret, Smith, 10-mL capacity, or4.4.3 Bulb Pipet, dropping, with 50-mL Erlenmeyer flask.4.5 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
18、 follows:4.6.1 Trays measuring 165 by 300 mm (612 by 12 in.) , foruse 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 measur
19、ing 165 by 165 mm (612 by 612 in.), foruse with (6 by 6-in.) foil, 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.Alternativ
20、ely two 150 by 150-mm (6 by 6-in.) foilsheets may be used in a similar 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 weigh
21、ing, but must be kept smooththroughout the pressing and drying operations.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 differe
22、nce a 0.9 to 1.1-gspecimen of the resin solution, to 0.1 mg. Place 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
23、specimen to spread uniformlyinto a thin film, about 75 mm (3 in.) in 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 so
24、lvent to evaporate from theweighed specimen before covering and pressing 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 c
25、arefullyremove the foil sheet from the tray. Return the dried filmsurfaces 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 f
26、ollows:C 5 A 2 B! 3100#/Swhere:A = weight of foil plus dried solids, 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
27、 two results,each the mean of duplicate determinations obtained by 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 determinat
28、ions, obtained by ana-lysts in different laboratories is normally about 0.4 %, absolute.NOTE 1Millimetre dimensions appear in section on Apparatus.FIG. 1 Tray for 150 by 300-mm (6 by 12-in.) FoilD1259 06 (2018)2Two such results should be considered suspect if they differ bymore than 1.0 %, absolute.
29、7.1.3 No bias has been determined for this test method.TEST METHOD 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
30、 apparatus is identical with thatgiven in 4.2 4.6.9. Procedure9.1 Weigh 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
31、 at 105 6 2C for 2 h. When using 150 by 150mm (612by 612-in.) trays 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-tio
32、n 6.11. Precision and Bias11.1 The following criteria should be used 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 an
33、alyst, is normally about 0.3 %, absolute. Two suchresults should be considered suspect if they differ by more than0.7 %, absolute.11.1.1.2 ReproducibilityThe difference between tworesults, each the mean of duplicate determinations obtained byanalysts in different laboratories, is normally about 0.7
34、absolute. Two such results should be considered suspect if theydiffer 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 duplicat
35、e determinations,obtained by the same analyst is normally about 0.1 %, 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.
36、2 %. Two such results should be consideredsuspect if they differ 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
37、 and Holder for 150 by 150-mm (6 by 6-in.) FoilD1259 06 (2018)3ASTM 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 the validity of any such
38、 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. Your comments are invited
39、 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 comments have not received a f
40、air 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 s
41、tandard 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). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 06 (2018)4
