ASTM_D_563_-_88_1996e1.pdf

Designation:D 563 88(Reapproved 1996)e1An American National StandardStandard Test Method forPhthalic Anhydride Content of Alkyd Resins and ResinSolutions1This standard is issued under the fixed designation D 563;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.e1NOTEKeywords were added editorially in October 1996.1.Scope1.1 This test method covers the determination of the ph-thalic anhydride content(Note 1)of alkyd resins and resinsolutions,including those containing styrene.NOTE1This test method is not applicable for the determination ofphthalic anhydride in alkyd resins containing other dibasic acids such asmaleic or fumaric,or modifying agents such as urea,melamine,andphenolic resins.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.2.Referenced Documents2.1 ASTM Standards:D 1193 Specification for Reagent Water23.Significance and Use3.1 The phthalic anhydride content of alkyd resins controlsthe properties of the final film.4.Apparatus4.1 Flask and CondenserA 500-mL Erlenmeyer flaskfitted with an air-cooled glass reflux condenser 30 in.(760 mm)in length.The connection between the flask and condensershall be a 24/40 standard taper ground-glass joint.4.2 Water Bath.4.3 Fritted-Glass Filter Crucible,fine or medium porosity,of 30-mL capacity.4.4 Desiccator,containing concentrated H2SO4(sp gr 1.84)as the desiccant.4.5 Filter Flasks.4.6 Crucible Holder.5.Reagents5.1 Purity of ReagentsReagent grade chemicals shall beused in all tests.Unless otherwise indicated,it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.3Other grades may beused,provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.5.2 Purity of WaterUnless otherwise indicated,referencesto water shall be understood to mean reagent water as definedby Type II of Specification D 1193.5.3 Alcohol-Benzene Wash SolutionMix one volume ofabsolute ethyl alcohol(Note 2)with three volumes of benzene.NOTE2The alcohol may be denatured,formula 2B,but must beabsolute.5.4 Benzene.5.5 EtherAnhydrous analytical reagent-grade ether.5.6 Hydrochloric Acid,Standard(0.1 N).5.7 Potassium Hydroxide,Alcoholic SolutionDissolve 66g of reagent-grade potassium hydroxide(KOH)in 1 L ofabsolute ethyl alcohol(Note 2).Filter just before use.6.Procedure6.1 Weigh by difference,from a closed container into the500-mL Erlenmeyer flask,a specimen of resin or resin solutionsufficient to yield from 0.8 to 1.2 g of potassium alcoholphthalate.Add 150 mL of benzene,warming slightly on thesteam bath if necessary,to effect solution.Add 60 mL ofalcoholic KOH solution and attach the condenser.Place theflask in a water bath to a depth approximately equal to that ofthe contents of the flask.Warm the bath,maintaining atemperature of 40C for 1 h,then gradually raise the tempera-ture until the alcoholic solution boils gently.Reflux for 112h.1This method is under the jurisdiction of ASTM Committee D-1 on Paint andRelated Coatings,Materials,and Applications and is the direct responsibility ofSubcommittee D01.33 on Polymers and Resins.Current edition approved May 27,1988.Published October 1988.Originallypublished as D 563 40 T.Last previous edition D 563 80.2Annual Book of ASTM Standards,Vol 11.01.3Reagent 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.1AMERICAN SOCIETY FOR TESTING AND MATERIALS100 Barr Harbor Dr.,West Conshohocken,PA 19428Reprinted from the Annual Book of ASTM Standards.Copyright ASTM6.2 Remove the flask from the bath and wash down theinside of the condenser with a few millilitres of alcohol-benzene wash solution.Remove the condenser,cap the flaskwith the soda-lime guard tube,and cool by means of runningwater or an ice bath.6.3 When cool,filter immediately and as rapidly as possible,through a fritted-glass crucible that previously has been tared,using the alcohol-benzene wash solution for transferring theprecipitate and washing the reaction flask.Wash the precipitatewith successive portions of alcohol-benzene wash solutio