ASTM_D_1397_-_93_1998.pdf

Designation:D 1397 93(Reapproved 1998)Standard Test Method forUnsaponifiable Matter in Alkyd Resins and Resin Solutions1This standard is issued under the fixed designation D 1397;the number immediately following the designation indicates the year oforiginal adoption 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.This standard has been approved for use by agencies of the Department of Defense.1.Scope1.1 This test method covers the determination of unsaponi-fiable matter in alkyd resins and resin solutions.This testmethod is not applicable to alkyd resins containing modifyingagents such as urea,melamine,phenols,rosin,and styrene.1.2 This 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 and health practices and determine the applica-bility of regulatory limitations prior to use.For a specifichazard statement,see Note 4.2.Referenced Documents2.1 ASTM Standards:D 1193 Specification for Reagent Water23.Significance and Use3.1 The unsaponifiable matter in alkyd resins controls theproperties of the final film.4.Apparatus4.1 Aluminum Beaker,having a capacity of 125 mL.34.2 Flask and CondenserA 200-mL Erlenmeyer flaskfitted with a water-cooled glass reflux condenser.The connec-tion between the flask and condenser shall be a standard 24/40taper ground-glass joint.4.3 Separatory FunnelsThree 500-mLcapacity fitted withstandard-taper,ground-glass stoppers and stopcocks.Stop-cocks should be lubricated sparingly with ether-insolublestopcock grease.Alternatively,funnels fitted with tetrafluoro-ethylene(TFE-fluorocarbon)stopcocks may be used.4.4 Steam Bath.4.5 Vacuum Drying OvenAsmall,laboratory-size vacuumoven,thermostatically controlled to operate at 80 6 5C.Awater aspirator vacuum source is satisfactory.5.Reagents and Materials5.1 Reagent grade chemicals shall be used in all tests.Unless otherwise indicated,it is intended that all reagents shallconform to the specifications of the Committee on AnalyticalReagents of the American Chemical Society,where suchspecifications are available.4Other grades may be used,pro-vided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.5.2 Unless otherwise indicated references to water shall beunderstood to mean reagent water as defined by Type II ofSpecification D 1193.5.3 Benzene.5.4 BenzeneAlcohol MixtureMix equal volumes of ben-zene and ethyl alcohol,add 2 drops of phenolphthaleinindicator solution,and neutralize with 0.02 N sodium hydrox-ide(NaOH)solution to a persistent faint pink color.5.5 Ethyl Alcohol(95 volume%)Pure ethyl alcohol ordenatured alcohol conforming to Formula No.2B of the U.S.Bureau of Internal Revenue.5.6 Ethyl Ether.5.7 Phenolphthalein Indicator Solution(10 g/L)Dissolve1 g of phenolphthalein in ethyl alcohol(95%)and dilute to 100mL with ethyl alcohol.5.8 pH Indicator Paper,universal type.5.9 Sodium Hydroxide Solution(50%)Dissolve sodiumhydroxide(NaOH)in an equal weight of water.1This test method is under the jurisdiction of ASTM Committee D-1 on Paintand Related Coatings,Materials,and Applications and is the direct responsibility ofSubcommittee D01.33 on Polymers and Resins.Current edition approved April 15,1993.Published June 1993.Originallypublished as D 1397 56 T.Last previous edition D 1397 88.2Annual Book of ASTM Standards,Vol 11.01.3Aluminum beakers,Catalog No.2100,manufactured by theA.H.Thomas Co.,W.Washington Square,Philadelphia,PA 19105,have been found satisfactory forthis purpose.4Reagent Chemicals,American Chemical Society Specifications,AmericanChemical Society,Washington,DC.For suggestions on the testing of reagents notlisted by the American Chemical Society,see Analar Standards for LaboratoryChemicals,BDH Ltd.,Poole,Dorset,U.K.,and the United States Pharmacopeiaand National Formulary,U.S.Pharmacopeial Convention,Inc.(USPC),Rockville,MD.1Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959,United States.5.10 Sodium Hydroxide,Standard Solution(0.02 N)Prepare and accurately standardize a 0.02 N aqueous NaOHsolution.6.Procedure6.1 Weigh by difference,from a closed container into the200-mL Erlenmeyer flask,a portion of resin or resin solutioncontaining from 0.05 to 0.2 g of unsaponifiable matter(Note 1)(8 to 10 g of resin solution usually is sufficient).NOTE1The maximum specimen size is limited to 10 g of nonvolatilematter;otherwise saponification or separation difficulties may arise.Thespecimen should be weighed to the nearest milligram.6.2 Add 10 mL of benzene,and warm to dissolve thesample.Add 50 mL of alcohol,swirl gently to mix,and thenadd slowly 5 mL of the NaOH solution(50%),whileswirlinggently.Add 5 mL of water,attach to the condenser,a