ASTM_D_5564_-_95_2011.pdf

Designation:D556495(Reapproved 2011)Standard Test Method forDetermination of the Total Ammonia Contained inSulfonated or Sulfated Oils1This standard is issued under the fixed designation D5564;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 determination of the totalammonia contained in sulfonated or sulfated oils.1.2 The values stated in SI units are to be regarded as thestandard.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 A3.Significance and Use3.1 This test method of analysis is intended to determine thetotal ammonia in a sample of sulfonated or sulfated oil,or both,by boiling a water solution of the sample with excess alkali anddetermining by titration the loss in alkali after the boiling.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 FlaskAn Erlenmeyer flask(Fig.1)made of a boro-silicate glass,having a capacity of approximately 300 mL andprovided with a glass stopper.4.1.2 Condenser,consisting of a glass tube,915 mm(36 in.)in length and 8 mm(516in.)in outside diameter.The lower endof the tube shall be flared and ground to fit the mouth of theErlenmeyer flask.4.1.3 Glass BeadsPerforated 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 a 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 mg of KOH per mL;1 mL of 1 N NaOH solutionis 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 mg of KOH per mL;1mL of 0.5 N NaOH solution is equivalent to 28.05 mg 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 mg of KOH per mL;1 mL of 0.5 NH2SO4is equivalent to 28.05 mg of KOH.5.7 Sulfuric Acid(1+19)Carefully mix 1 volume of con-centrated sulfuric acid(H2SO4,sp gr 1.84)into 19 volumes ofwater while stirring.6.Procedure6.1 The procedure consists of two determinations:namely,(1)the total alkalinity,and(2)the loss in alkalinity after boilingwith excess NaOH.6.1.1 Total AlkalinityDetermine the total alkalinity asdescribed in the determination of organically combined sulfu-ric anhydride,Test Method D5350;Procedure.6.1.2 Alkalinity After BoilingDissolve 10 g of the samplein 100 mL of water in a 500-mL beaker,add 25 mL of 0.5 N1This 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 49-1957).Current edition approved Jan.1,2011.Published March 2011.Originallyapproved in 1994.Last previous edition approved in 2006 as D5564 95(2006).DOI:10.1520/D5564-95R11.2For 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 NaOH solution,and boil the mixture for 30 min or until all theammonia is expelled as indicated by moistened red litmuspaper.Cool the contents of the beaker,add methyl orangeindicator solution(0.1%),and titrate to an approximate endpoint.Transfer the mixture to a 250-mL glass-stoppered flaskand complete the titration(with the addition of salt and ether)as described in the determination of organically combinedsulfuric anhydride,Test Method D5350;Procedure.7.Calculation7.1 Calculate the total ammonia,%,as follows:T 5 A1$B 3D!2C 3E!#/W%(1)ortotal ammonia5 0.0303 T(2)where:T=total ammonia,mg of KOH/g,A=total alkalinity,mg of KOH/g,B=mL of NaOH s