ASTM_D_5352_-_95_2012.pdf

Designation:D535295(Reapproved 2012)Standard Test Method forDetermination of Organically Combined Sulfuric AnhydrideAsh-Gravimetric,Test Method C1This standard is issued under the fixed designation D5352;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 ofsulfonated or sulfated oil,or both,by extracting the undecom-posed sulfonated or sulfated fat and other fatty matter over anacidulated,concentrated salt solution,and ashing the purifiedextract.This test method is applicable to all types of sulfonatedand sulfated oils,including true sulfonic acid oils and thosecontaining sodium acetate or similar partially titratable com-pounds.This test method was derived from Test MethodsD500,Sections 25 through 28.1.2 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 for the determination oforganically combined sulfuric anhydride in sulfonated andsulfated fats and oils.4.Reagents4.1 Ethyl Ether.4.2 Hydrogen Peroxide(30%)Concentrated hydrogenperoxide(H2O2).4.3 Methyl Orange Indicator Solution(1 g/L)Dissolve 0.1g of methyl orange in 100 mL of water.4.4 Sodium Chloride(NaCl),solid.4.5 Sodium Sulfate(Na2SO4),anhydrous.5.Procedure5.1 The procedure consists of isolating and purifying thefatty matter as it exists in the original oil by dissolving thesample in a solvent,acidifying and washing with saturatedbrine,and ashing the purified extract.If the sample containsammonia,the ammonia shall first be expelled before thedetermination is made on the sample.5.1.1 In the Absence of AmmoniaProceed as described inthe separation of purified oil(6.1.1 Method B),combining theether layers in the first funnel rather than in the decompositionflask.Carefully remove any water that may settle and dehy-drate the ether layer as follows:add 5 g of anhydrous Na2SO4,shake vigorously for 5 min,and filter directly into a 150-mLbeaker placed in a bath of warm water.Wash the flask and filterwith ether until free from fat(absence of oil stains on the filterpaper after drying)and add the filtrate to the beaker.To avoidcreeping of the oil,the volume in the beaker should at no timeduring the filtering and washing exceed 50 mL(one third full).Evaporate the ether solution until the volume has been reducedto about 20 mL and transfer the residue to a tared 50-mLcrucible(high form).Immerse the crucible in a 100-mL beakercontaining warm water until practically all of the ether hasevaporated.Rinse the beaker with two 10-mL and three 5-mLportions of ether,or until all of the oil has been transferred tothe crucible;allow each portion of rinsing ether to evaporatebefore the next rinsing is made.Burn gently the solvent-freeresidue,and finally ignite at a dull red heat to constant weight.To prevent creeping of the oil and to hasten evaporation,stirthe solution with a glass rod;before the oil is burned,wipe therod clean with ashless filter paper and add the paper to thecrucible.To oxidize traces of carbon or sodium sulfide thatmight form,moisten the ash with H2O2and again carefullyignite to constant weight.Calculate the percentage of ash asfollows: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 44-1957).Current edition approved April 1,2012.Published April 2012.Originallyapproved in 1993.Last previous edition approved in 2006 as D5352 95(2006).DOI:10.1520/D5352-95R12.2For 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 Extracted ash,%5A/B!3100(1)where:A=weight of ash,g,andB=weight of sample,g.5.1.2 In the Presence of AmmoniaDissolve 5 to 8 g of thesample in 80 mL of water in a 300-mL beaker.Add 10 mL of1 N NaOH solution and boil the solution gently until wet litmuspaper no longer indicates ammonia.Cool the solution,transferto a