ASTM_D_3712_-_05_2011.pdf

Designation:D371205(Reapproved 2011)Designation:369/(95)Standard Test Method ofAnalysis of Oil-Soluble Petroleum Sulfonates by LiquidChromatography1This standard is issued under the fixed designation D3712;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 analysis of refined and crudenatural and synthetic oil-soluble sulfonate products.Resins,ifpresent,are recovered with the oil phase and carboxylates arerecovered as sulfonates.1.2 This test method covers the determination of mineraloil,sodium sulfonate,inorganic salts,water,basicity or acidity,average molecular weight,and relative density of sodiumsulfonate products.1.3 This test method covers the determination of mineraloil,sulfonate,water,base number,average molecular weight,and relative density of calcium,barium,magnesium,andammonium sulfonate products.1.4 The values stated in SI units are to be regarded as thestandard.The values given in parentheses are for informationonly.1.5 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:2D95 Test Method for Water in Petroleum Products andBituminous Materials by DistillationD2896 Test Method for Base Number of Petroleum Productsby Potentiometric Perchloric Acid Titration3.Terminology3.1 Symbols:3.1.1 Following are definitions of the symbols used inSection 17,and as noted in the sections in parentheses.A=grams of sample of calcium,barium,magnesium,or ammoniumsulfonate(8.1.1).B=volume of chloroform solution,mL(10.1).C=grams of sample of sodium sulfonate(10.1.1).D=grams of oil recovered(10.4).E=grams of sodium sulfonate recovered(10.5).F=grams of residue from chloroform blank(10.6).G=grams of residue from alcohol blank(10.6).H=grams of sodium sulfonate(11.1).I=grams of sodium sulfate ash from sodium sulfonate(11.2).J=T/KS.K=valence of cation.S=average equivalent weight of sodium sulfonate(17.1.4).T=average molecular weight of calcium,barium,magnesium,orammonium sulfonate(17.1.5).U=percentage of sodium sulfonate(17.1.2).V=percentage of calcium,barium,magnesium,or ammoniumsulfonate(17.1.3).Wc=grams of water contained in pycnometer at 25C(6.9).Ws=grams of sample contained in pycnometer at 25C(15.1).X=grams of sodium sulfonate sample for basicity(12.1).Y=volume of standard H2SO4or NaOH solution used to determinebasicity or acidity(12.1).Z=normality of standard H2SO4or NaOH solution to determine freebasicity or acidity(12.1).AA=grams of sodium sulfonate product ashed(13.1).BB=grams of sodium sulfate from inorganic salt determination(13.1).CCA=percentage of free acidity of sodium sulfonate product as H2SO4(17.1.6).CCB=percentage of free basicity of sodium sulfonate product as NaOH(17.1.6).DD=percentage of inorganic salts as sodium sulfate(17.1.7).4.Summary of Test Method4.1 The sample,except a sodium sulfonate product,isdissolved in ethyl ether and converted to sulfonic acid,usingdilute hydrochloric acid.The sulfonic acid after extraction isconverted to sodium sulfonate and the isolated sodium sul-fonate and mineral oil are dissolved in chloroform.An aliquotof the chloroform solution,or a sample of a sodium sulfonateproduct,dissolved in chloroform,is placed on a silica gelcolumn.The oil is eluted with chloroform,the sulfonate withethyl alcohol,and both are determined gravimetrically.Aver-age molecular weight is calculated from the average equivalent1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products,Liquid Fuels,and Lubricantsand is the direct responsibility ofSubcommittee D02.04.0C on Liquid Chromatography.Current edition approved Jan.1,2011.Published February 2011.Originallyapproved in 1978.Last previous edition approved in 2005 as D3712 05.DOI:10.1520/D3712-05R11.This test method was adopted as a joint ASTM-IP standard.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 weight of the sodium sulfonate,which is determined by ashinga portion of the isolated sodium sulfonate.4.2 Water is determined by Test Method D95.Base numberis determined by Test Method D2896.Relative density isdetermined by pycnometer.5.Significance and Use5.1 This test method provides a means of determiningsulfonate content and of classifying and characterizing naturaland synthetic petroleum