ASTM_D_5553_-_95_2012.pdf

Designation:D555395(Reapproved 2012)Standard Test Method forDetermination of the Unsaponifiable Nonvolatile Matter inSulfated Oils1This standard is issued under the fixed designation D5553;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()indicates an editorial change since the last revision or reapproval.1.Scope1.1 This test method covers the determination of theunsaponifiable,nonvolatile(above 80C)matter existing in asample of sulfated oil by saponifying the desulfated fattymatter and extracting the unsaponifiable matter,and extractingthe unsaponifiable matter from the soap solution with ethylether.1.2 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.3 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:2D5350 Test Method for Determination of Organically Com-bined Sulfuric Anhydride by Titration,Test Method AD5351 Test Method for Determination of Organically Com-bined Sulfuric Anhydride by Extraction Titration,TestMethod BD5353 Test Method for Determination of Total DesulfatedFatty Matter3.Significance and Use3.1 This test method is intended for use in the determinationof the unsaponifiable,nonvolatile matter contained in sulfatedoils for the purpose of quality assurance.4.Apparatus and Reagents4.1 Saponification FlaskThe apparatus required for thesaponification consists of a glass flask provided with an aircondenser.4.2 Ethyl Ether.4.3 Potassium Hydroxide,Alcoholic Solution(28 g/L)Dissolve approximately,but not less than,28 g of KOH in ethylalcohol and dilute to 1 L.4.4 Potassium Hydroxide Aqueous Solution(28 g/L)Dissolve 28 g of potassium hydroxide(KOH)in water anddilute to 1 L.5.Procedure5.1 The procedure consists of decomposing the sample withmineral acid,extracting the desulfated fatty matter,saponifyingthe latter,and extracting the unsaponifiable matter from thesoap solution with ethyl ether.5.1.1 Desulfated Fatty MatterDetermine the desulfatedfatty matter as described in the determination of total desul-fated fatty matter.See Test Methods D5350,D5351,andD5353.5.1.2 SaponificationAccurately weigh 2 to 2.5 g of thedesulfated fatty matter in the flask,add 25 mL of the alcoholicKOH solution,and simmer the contents(without loss ofalcohol)for 1 h with occasional swirling,over an electric hotplate or other source of heat.5.1.3 ExtractionTransfer the content of the flask to a250-mL separatory funnel and wash the flask several timeswith a total of 50 mL of water,pouring it into the separatoryfunnel.Extract the solution while still warm(about 30C)with50 mL of ether(rinse the saponification flask with the etherbefore adding it to the separatory funnel),shaking vigorouslyfor about 1 min,and allow the layers to settle and clear.Drawoff the lower layer in a second 250-mL separatory funnel andextract in a similar manner with two 50-mL portions of ether.5.1.4 Preliminary Water WashingAdd 20 mL of water tothe combined ether layer,turn the separatory funnel andcontents over gently about six times,and allow the layers tosettle and clear.Draw off the lower layer and discard.Wash theether layer twice more with 20-mL portions of water,shakingvigorously after each addition.1This test method is under the jurisdiction of ASTM Committee D31 on Leatherand is the direct responsibility of Subcommittee D31.08 on Fats and Oils.This testmethod was developed in cooperation with the American Leather Chemists Assn.(Method H 471957).Current edition approved April 1,2012.Published April 2012.Originallyapproved in 1994.Last previous edition approved in 2006 as D5553 95(2006).DOI:10.1520/D5553-95R12.2For referenced ASTM standards,visit the ASTM website,www.astm.org,orcontact ASTM Customer Service at serviceastm.org.For Annual Book of ASTMStandards volume information,refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 5.1.5 Alkali and Water WashingAdd 20 mL of aqueousKOH solution to the washed ether layer,turn the separatoryfunnel and contents over gently about six times,and allow thelayers to settle and clear.Draw off the lower layer and discard.Wash the ether layer with 20 mL of water,shaking vigorously.Continue washing with 20 mLof KOH solution followed by 20mL of water,shaking vigorously after each addition,until thealkali layer upon strong acidification with HCl and settling fora few minutes is only faintly opalescent.Finally wash the etherlayer with 20-mL portions of water until the wash water is nolonger pi