ASTM_D_5348_-_95_2012.pdf

Designation:D534895(Reapproved 2012)Standard Test Method forDetermination of the Moisture Content of Sulfonated andSulfated Oils by Distillation with Xylene1This standard is issued under the fixed designation D5348;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 waterexisting in a sample of sulfonated or sulfated oil,or both,bydistilling the sample with a volatile solvent.The test 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.This test method wasderived from Test Methods D500,Sections 4 through 9.1.2 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 to determine the moisturecontent of fats,oils,and fatliquors used in the softening andstuffing of leather.The moisture content is measured for thepurpose of quality assurance.4.Apparatus4.1 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.1.4.1.1 Flask,500-mL,of either the short-neck,round-bottomtype or the Erlenmeyer type.4.1.2 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 control.4.1.3 Condenser,a water-cooled glass reflux condenser(Fig.1),having a jacket approximately 400 mm(1534in.)in lengthwith an inner tube 9.5 to 12.7 mm(38to12in.)in outsidediameter.The end of the condenser to be inserted in the trapshall be ground off at an angle of 30 from the vertical axis ofthe condenser.When inserted into the trap,the tip of thecondenser shall be about 7 mm(14in.)above the surface of theliquid in the trap after the distillation conditions have beenestablished.Fig.1 shows a conventional sealed-in type ofcondenser,but any other condenser fulfilling the detailedrequirements above may be used.4.1.4 Trap,a trap made of well-annealed glass constructedin accordance with Fig.1 and graduated as shown to contain 5mL at 20C.It shall be subdivided into 0.1-mL divisions,witheach 1-mL line numbered(5 mL at top).The error in anyindicated capacity may not be greater than 0.05 mL.5.Purity of Reagents5.1 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 onAnalytical Reagents of theAmerican Chemical Society.36.Reagents6.1 Oleic Acid,heated previous to use for 5 to 10 min overa free flame at a temperature of 130 to 135C.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 40-1957).Current edition approved April 1,2012.Published April 2012.Originallyapproved in 1993.Last previous edition approved in 2006 as D5348 95(2006).DOI:10.1520/D5348-95R12.2For 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.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 6.2 Xylene.7.Calibration7.1 To calibrate the apparatus add approximately 1 g ofwater to a mixture of 80 g of xyl