ASTM_D_5350_-_95_2012.pdf

Designation:D535095(Reapproved 2012)Standard Test Method forDetermination of Organically Combined Sulfuric Anhydrideby Titration,Test Method A1This standard is issued under the fixed designation D5350;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 boiling the sample with sulfuric acid anddetermining the acidity of the reaction mixture.This testmethod is applicable only to oils that split off their combinedSO3upon boiling with mineral acids and that do not containcompounds that cannot be accurately titrated in water solutionwith methyl orange as the indicator.This test method wasderived from Test Methods D500,Sections 15 through 19.1.2 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 Oils3.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,Standard(0.5 N)Accurately prepare andstandardize a 0.5 N sulfuric acid(H2SO4)solution.Express thestrength of the solution as milligrams of KOH per millilitre;1mL of 0.5 N H2SO4is equivalent to 28.05 mg of KOH.5.7 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 Oils.This testmethod was developed in cooperation with the American Leather Chemists Assn.(Method H 421957).Current edition approved April 1,2012.Published April 2012.Originallyapproved in 1993.Last previous edition approved in 2006 as D5350 95(2006).DOI:10.1520/D5350-95R12.2For 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 6.Procedure6.1 The procedure consists of two determinations:namely,(1)the alkalinity of the sample,designated as A,and(2)theincrease in acidity after boiling the sample with sulfuric acid,designated as F.6.1.1 Alkalinity,ADissolve 10 g of the sample in 100 mLof water in the 300-mL glass-stoppered Erlenmeyer flask,warming to obtain solution,if necessary.After cooling,add 30g of NaCl,25 mL of ether,and five drops of methyl orangeindicator solution;then add 0.5 N H2SO4with frequent butgentle shaking until the mixture is slightly acid.Shake thecontents of the flask vigorously,and complete the titration byadding first 0.5 N NaOH solution several drops at a time untilthe solution i