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TM_D_500_
_95_2009
Designation:D50095(Reapproved 2009)Standard Test Methods ofChemical Analysis of Sulfonated and Sulfated Oils1This standard is issued under the fixed designation D500;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 These test methods cover the chemical analysis ofsulfonated and sulfated oils.The analytical procedures appearin the following order:SectionMoisture:Test Method A.Water by Distillation with Volatile Solvent4 9Test Method B.Moisture and Volatile Matter by Hot-Plate Method10 14Organically Combined Sulfuric Anhydride:Test Method A.Titration Test15 19Test Method B.Extraction-Titration Test20 24Test Method C.Ash-Gravimetric Test(in the Presence of TrueSulfonates)25 28Total Desulfated Fatty Matter29 32Total Active Ingredients33 36Unsaponifiable Nonvolatile Matter37 41Inorganic Salts42 46Total Alkalinity47 49Total Ammonia50 52Acidity as Free Fatty Acids or Acid Number:Test Method A.In the Absence of Ammonium or TriethanolamineSoaps53 56Test Method B.In the Presence of Dark Colored Oils but in theAbsence of Ammonium or Triethanolamine Soaps(Brine Test)57 60Test Method C.In the Presence of Ammonium or TriethanolamineSoaps61 63Water-Immiscible Organic Solvents Volatile with Steam64 701.2 The values stated in inch-pound units are to be regardedas the standard.The metric equivalents of inch-pound unitsmay be approximate.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.Material SafetyData Sheets are available for reagents and materials.Reviewthem for hazards prior to usage.2.Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent Water3.Purity of Reagents3.1 Purity of ReagentsReagent grade chemicals shall beused in all tests.Unless otherwise indicated,it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.3Other grades may beused,provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.3.2 Purity of WaterUnless otherwise indicated,referencesto water shall be understood to mean reagent water conformingto Specification D1193.MOISTUREMethod A.Water by Distillation with Volatile Solvent4.Scope4.1 This test method covers the determination of waterexisting in a sample of sulfonated or sulfated oil,or both,bydistilling the sample with a volatile solvent.The method isapplicable only to sulfonated and sulfated oils that do notcontain the following:mineral acids,free sulfonic acids,or freesulfuric acid esters;or alkali hydroxides,carbonates or ac-etates;or alcohol,glycerin,diethylene glycol,acetone,or otherwater-miscible volatile compounds.1These test methods are under the jurisdiction of ASTM Committee D12 onSoaps and Other Detergents and is the direct responsibility of Subcommittee D12.12on Analysis and Specifications of Soaps,Synthetics,Detergents and their Compo-nents.Current edition approved Oct.1,2009.Published December 2009.Originallyapproved in 1937.Last previous edition approved in 2003 as D500 95(2003).DOI:10.1520/D0500-95R09.2For 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.3Reagent 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.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 5.Apparatus5.1 The apparatus required consists of a glass flask heatedby suitable means and provided with a reflux condenserdischarging into a trap and connected to the flask.Theconnections between the trap and the condenser and flask shallbe interchangeable ground joints.The trap serves to collect andmeasure the condensed water and to return the solvent to theflask.A suitable assembly of the apparatus is illustrated in Fig.1.5.1.1 Flask,500-mL,of either the short-neck,round-bottomtype or the Erlenmeyer type.5.1.2 Heat SourceThe source of heat may be either an oilbath(stearic acid,paraffin wax,etc.),or an electric heaterprovided with a sliding rheostat or other means of heat contro