ASTM_D_5351_-_93_2009.pdf

Designation:D535193(Reapproved 2009)Standard Test Method forDetermination of Organically Combined Sulfuric Anhydrideby Extraction Titration,Test Method B1This standard is issued under the fixed designation D5351;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 the organi-cally combined sulfuric anhydride existing in a sample ofsulfated oil by extracting the undecomposed sulfated fat andother fatty matter over an acidulated,concentrated saltsolution,boiling the residue with sulfuric acid after evaporat-ing the solvent,and titrating the products of reaction.This testmethod is applicable only to sulfated oils that split off theircombined SO3upon boiling with mineral acids,includingsamples containing sodium acetate or other compounds thatcannot be accurately titrated in water solution with methylorange as the indicator.This test method was derived from TestMethods D500,Sections 20 through 24,and ALCA MethodH-43.1.2 The values stated in SI units are to be regarded as thestandard.The values given in parentheses are provided forinformation only.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:2D500 Test Methods of Chemical Analysis of Sulfonated andSulfated Oils2.2 Other Document:ALCA Method H-43 Organically Combined Sulfuric Anhy-dride Extraction Titration Test(for Sulfated Oils)33.Significance and Use3.1 This test method is intended for the determination oforganically combined sulfuric anhydride in sulfated oils.4.Apparatus4.1 The apparatus required consists of a glass flask providedwith a glass stopper and an air condenser.The connectionbetween the flask and the condenser shall be a ground joint.Perforated glass beads shall be used to prevent bumping.4.1.1 Flask,an Erlenmeyer flask(Fig.1)made of borosili-cate glass,having a capacity of approximately 300 mL,andprovided with a glass stopper.4.1.2 CondenserThe condenser required consists of aglass tube,915 mm(36 in.)in length,and 8 mm(516in.)inoutside diameter.The lower end of the tube shall be flared andground to fit the mouth of the Erlenmeyer flask.4.1.3 Glass Beads,perforated glass beads,made of chemi-cally resistant glass,approximately 4 mm(532in.)in diameter.Before using,the glass beads shall be boiled thoroughly inseveral portions of water or until the wash water reacts neutralto methyl orange indicator.5.Reagents5.1 Ethyl Ether:5.2 Methyl Orange Indicator Solution(1 g/L)Dissolve 0.1g of methyl orange in 100 mL of water.5.3 Sodium Chloride(NaCl),solid.5.4 SodiumHydroxide,StandardSolution(1N)Accurately prepare and standardize a 1 N sodium hydroxide(NaOH)solution.Express the strength or concentration of thesolution as milligrams of KOH per millilitre;1 mL of 1 NNaOH solution is equivalent to 56.1 mg of KOH.5.5 Sodium Hydroxide,Standard Solution(0.5 N)Accurately prepare and standardize a 0.5 N NaOH solution.Express the strength of the solution as milligrams of KOH permillilitre;1 mL of 0.5 N NaOH solution is equivalent to 28.05mg of KOH.5.6 Sulfuric Acid(1+19)Carefully mix one volume ofconcentrated sulfuric acid(H2SO4,sp gr 1.84)into 19 volumesof water while stirring.1This test method is under the jurisdiction of ASTM Committee D31 on Leatherand is the direct responsibility of Subcommittee D31.08 on Fats and OilsCurrent edition approved April 1,2009.Published July 2009.Originallyapproved in 1993.Last previous edition approved in 2003 as D5351 93(2003).DOI:10.1520/D5351-93R09.2For 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.3Available from American Leather Chemists Assn.,Texas Tech University,P.O.Box 45300,Lubbock,TX 79409.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 5.7 Sulfuric Acid Standard(0.5 N)Accurately prepare andstandardize as 0.5 N sulfuric acid(H2SO4)solution.Expressthe strength of the solution as milligrams of KOH per millilitre;1 mL of 0.5 N H2SO4is equivalent to 28.05 mg of KOH.6.Procedure6.1 The procedure consists of isolating and purifying thefatty matter as it exists in the original oil by dissolving thesample in a solvent,acidifying and washing with saturatedbrine,and determining the increase in acidity upon boiling theisolated product with sulfuric acid.This increase in acidity isdesignated as F.6.1.1 Separation of Purified OilWeigh 5