ASTM_D_1965_-_87_1998.pdf

Designation:D 1965 87(Reapproved 1998)Standard Test Method forUnsaponifiable Matter in Drying Oils,Fatty Acids,andPolymerized Fatty Acids1This standard is issued under the fixed designation D 1965;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 the unsa-ponifiable matter present in all natural and synthetic drying oilsand their fatty acids and any other fatty acids or polymerizedfatty acids used in protective coatings.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 460 Test Methods for Sampling and Chemical Analysisof Soaps and Soap Products2D 1193 Specification for Reagent Water3D 1466 Test Method for Sampling Liquid Oils and FattyAcids Commonly Used in Paints,Varnishes,and RelatedMaterials42.2AOSC Standard:Specification H 2-4153.Terminology3.1 Definitions:3.1.1 unsaponifiable mattersubstances frequently founddissolved in fatty acids that cannot be saponified by sodiumhydroxide or potassium hydroxide under the conditions pre-scribed but are soluble in the ordinary fat solvents.Included arethe higher aliphatic alcohols,sterols,pigments,and hydrocar-bons.4.Significance and Use4.1 The major components of drying oils and fatty acids canbe saponified by reaction with alkali and converted to water-soluble soaps.This test method determines the amount ofmaterial present that is soluble in the oil but is not saponifiable.Under conditions of this test method,this material is notconverted to a water-soluble soap and is extracted from thesaponification mixture with petroleum ether.4.2 A small amount of unsaponifiable material is character-istic of drying oils and fatty acids however a large amountindicates contamination with hydrocarbon materials such asmineral oils or hydrocarbon resins.4.3 This test method is the referee method for unsaponifi-able content.The exact amount of unsaponifiable matterobtained is governed by the partition coefficient of the matterbetween the soap solution and the solvent.Different results willbe obtained if some other solvent,such as ethyl ether,is used.NOTE1See relevant specifications for appropriate numeric ranges ofunsaponifiable matter in specific drying oils or fatty acids.5.Apparatus5.1 Glass-Stoppered Extraction Cylinder,graduated at 40,80,and 130 mL,about 300 mm in height and 35 mm indiameter.5.2 Erlenmeyer or Soxhlet Flasks,100 to 200-mL capacity.5.3 Separatory Funnels,500-mL capacity.5.4 Glass Siphon.6.Reagents6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests unless otherwise specified.Unless otherwiseindicated,it is intended that all reagents shall conform to theSpecifications of the Committee on Analytical Reagents of theAmerican Chemical Society,where such specifications areavailable.6Other grades may be used provided it is firstascertained that the reagent is of sufficiently high purity topermit its use without lessening the accuracy of the determi-nation.6.2 Purity of WaterUnless otherwise indicated,referencesto water shall be understood to mean reagent water conforming1This test method is under the jurisdiction of ASTM Committee D-1 on Paintand Related Coatings,Materials,andApplications,and is the direct responsibility ofSubcommittee D01.32 on Drying Oils.Current edition approved June 26,1987.Published August 1987.Originallypublished as D 1965 61.Last previous edition D 1965 85.2Annual Book of ASTM Standards,Vol 15.04.3Annual Book of ASTM Standards,Vol 11.01.4Annual Book of ASTM Standards,Vol 06.03.5Available from American Oil Chemists Society,508 S.Sixth St.,Champaign,IL 61820.6Reagent 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 ASTMto Type II of Specification D 1193.6.3 Ethyl Alcohol,Neutral(95%)Use 95%ethyl alcoholor neutral denatured alcohol conforming to Formula No.30 or3Aof the U.S.Bureau ofAlcohol,Tobacco and Firearms.Boiland neutralize to the phenolphthalein end point with alkali justbefore using.6.4 Ethyl Alcohol(1+9)Mix 1 volume of alcoholco