ASTM_D_5349_-_95_2012.pdf

Designation:D534995(Reapproved 2012)Standard Test Method forDetermination of the Moisture and Volatile Content ofSulfonated and Sulfated Oils by Hot-Plate Method1This standard is issued under the fixed designation D5349;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 per-centage of water and other compounds volatile at about 100Cexisting in a sample of sulfonated or sulfated oil,or both,byrapid evaporation.This test method is applicable only tosulfonated and sulfated oils that do not contain the following:mineral acids,free sulfonic acids or free sulfuric acid esters,ammonia,acetic acid or similar volatile acids,alkalihydroxides,carbonates,acetates or similar salts that may reactwith oleic acid at elevated temperatures liberating volatileacids,or glycerin,diethylene glycol,xylene,or other com-pounds of similar volatility.This test method was derived fromTest Methods D500,Sections 10 through 14.1.2 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.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 moistureand volatile content of fats,oils,and fatliquors used in thesoftening and stuffing of leather.4.Apparatus4.1 The apparatus required consists of a glass-stopperedweighing flask,a glass beaker,and a suitable thermometer.4.1.1 Weighing Flasks,any suitable glass-stoppered weigh-ing flask of 10 to 15-mL capacity.4.1.2 Beaker,Griffin low-form glass beaker with an approxi-mate capacity of 150 mL and a diameter of about 5 cm.4.1.3 Heat SourceThe source of heat may be either anelectric hot plate with or without asbestos paper or board cover,or an open flame under a suitable asbestos board and a wiregauze(to spread the heat).4.1.4 Thermometer,graduated from 90 to 150C,about 3 in.in length,and substantially constructed.5.Reagents5.1 Desiccating AgentAny suitable desiccating agent maybe used.NOTE1Recent investigations seem to indicate that calcium chloride isunreliable as a laboratory desiccating agent.5.2 Oleic Acid.6.Procedure6.1 Weigh approximately 5 g of oleic acid into the beakerand insert the thermometer.Heat the oleic acid gradually,whilestirring with the thermometer,until the temperature reaches130C.Place the beaker in an oven at 105 to 100C for 15 min,cool in a desiccator,and weigh.Repeat the heating over the hotplate and in the oven until two successive weighings differ byless than 1.5 mg.6.2 Place about 6 g of the sample in the weighing flask anddetermine the weight accurately.Transfer the sample to thebeaker(containing the oleic acid and the thermometer)andweigh the flask again.Heat the mixture exactly as in the taringof the beaker as described in 6.1.The loss in weight isequivalent to the moisture in the sample.7.Calculation7.1 Calculate the percentage of moisture and volatile matterin the sample as follows:Moisture and volatile matter,%5A/B!3100(1)1This test method is under the jurisdiction of ASTM Committee D31 on Leatherand is the direct responsibility of Subcommittee D31.08 on Fats and OilsThis testmethod was developed in cooperation with the American Leather Chemists Assn.(Method H 411957).Current edition approved April 1,2012.Published April 2012.Originallyapproved in 1993.Last previous edition approved in 2006 as D5349 95(2006).DOI:10.1520/D5349-95R12.2For 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 where:A=loss of weight,g,andB=weight of sample,g.8.Precision and Bias8.1 Although this test method is widely used,precision andbias information is not available at this time.9.Keywords9.1 hot plate method;leather;moisture content;sulfonatedand sulfated oils;volatile contentASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard.Users of this standard are expressly advised that determination of the validity of any such patent rights,and the riskof infringement of such rights,are entirely their own responsibility.This standard is subject to revision at any