ASTM_D_5353_-_95_2012.pdf

Designation:D535395(Reapproved 2012)Standard Test Method forDetermination of Total Desulfated Fatty Matter1This standard is issued under the fixed designation D5353;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 totaldesulfated fatty matter in a sample of sulfated oils by decom-position with diluted mineral acids and extraction of thedecomposed fat.This test method is not applicable to samplesthat are not completely decomposed upon boiling with mineralacids.This test method was derived from Test Methods D500,Sections 29 through 32.1.2 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 OilsD5350 Test Method for Determination of Organically Com-bined Sulfuric Anhydride by Titration,Test Method AD5351 Test Method for Determination of Organically Com-bined Sulfuric Anhydride by Extraction Titration,TestMethod B3.Significance and Use3.1 This test method is intended for the determination of thetotal desulfated matter contained in sulfated oils following theirtotal decomposition with dilute mineral acid.4.Reagents4.1 Ethyl Ether.4.2 Sulfuric Acid(1+19)Carefully mix one volume ofconcentrated sulfuric acid(H2SO4,sp gr 1.84)into 19 volumesof water while stirring.5.Procedure5.1 The procedure consists of decomposing the sample withH2SO4,extracting the fatty matter with ether,evaporating thesolvent,and weighing the residue.After cooling,transfer thetitrated solution obtained after determining organically com-bined sulfuric anhydride in accordance with Test MethodD5350 or Test Method D5351(6.1.2)into a 250-mL separatoryfunnel and shake with 50 mL of ether.Draw off the water layerinto another separatory funnel and extract twice with 25-mLportions of ether.Wash the combined ether layers with 15-mLportions of water until the wash water is neutral to methylorange.Transfer the ether layer to a tared 150-mL beaker,evaporate on the water bath until practically free from solvent,dry in a hot-air oven at 105 to 110C for 30 min,cool in adesiccator,and weigh.Repeat the heating for 30-min periodsuntil constant weight is obtained.NOTE1Reserve the extracted fatty matter for the subsequent deter-mination of unsaponifiable matter(Sections 37 through 41 of TestMethods D500).6.Calculation6.1 Calculate the total desulfated fatty matter as follows:Total desulfated fatty matter,%5A/B!3100where:A=weight of residue,g,andB=weight of sample,g.7.Precision and Bias7.1 Although this test method is widely used,precision andbias information is not available at this time.8.Keywords8.1 desulfated matter;leather;sulfated fats and oils1This 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 45-1957).Current edition approved April 1,2012.Published April 2012.Originallyapproved in 1993.Last previous edition approved in 2006 as D5353 95(2006).DOI:10.1520/D5353-95R12.2For 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 ASTM 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 time by the responsible technical committee and must be reviewed every five years andif not revised,either reapproved or withdrawn.Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters.Your comments will receive careful consideration at a meeting of theresponsible technical committee,which you may attend.If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards,at the address shown below.This s