ASTM_D_5354_-_95_2012.pdf

Designation:D535495(Reapproved 2012)Standard Test Method forDetermination of Total Active Ingredients in Sulfonated andSulfated Oils1This standard is issued under the fixed designation D5354;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 totalactive ingredients in a sample of sulfonated or sulfated oil,orboth,as it exists in the original sample by extracting theundecomposed sulfonated or sulfated fat and other fatty matterover an acidified concentrated salt solution.Free alkali or alkalibound as soap is not included.This test method was derivedfrom Test Methods D500.NOTE1In the case of sulfated oils only,this determination may alsobe estimated by calculation(see 6.3),as it is equivalent to the sum of thedesulfated fatty matter and neutralized organically combined sulfuricanhydride.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 of thetotal active ingredients contained in sulfonated and sulfatedoils.Free alkali and alkaline soaps are excluded.4.Reagents4.1 Ethyl Ether.4.2 Methyl Orange Indicator Solution(1 g/L)Dissolve 0.1g of methyl orange in 100 mL of water.4.3 Sodium Chloride(NaCl),solid.4.4 Sodium Sulfate(Na2SO4),anhydrous.4.5 Potassium Hydroxide,Alcoholic Standard Solution(0.5N)Accurately prepare and standardize a 0.5 N alcoholicpotassium hydroxide(KOH)solution,the strength of whichshall be expressed as milligrams of KOH per millilitre;1 mLof 0.5 N alcoholic KOH solution is equivalent to 28.05 mg ofKOH.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 weighing the purified extract.Proceed as describedin the determination of organically combined sulfuricanhydride,Test Method B,in the absence of ammonia(6.1.1),retaining the separated active ingredients in the 150-mL beakerinstead of transferring it to a crucible.Evaporate the filtrate toa total volume of about 20 mL,add exactly 2 mL of alcoholicKOH solution,mix the contents by swirling,and finallyevaporate until practically free from ether.NOTE2With highly sulfonated or sulfated oil,it may be necessary toadd 5 to 10 mL of the alcoholic KOH solution in order to stabilize theresidue.5.2 Dry the residue at 108 to 112C for 112h,cool in adesiccator,and weigh.Repeat the heating for 30-min periodsuntil constant weight is obtained.6.Calculation6.1 Correction for the Alkali AddedCalculate the correc-tion for the alkali added as follows:Correction for alkali added,g 5 0.0006791 AS(1)where:A=millilitres of KOH solution added,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 46-1957).Current edition approved April 1,2012.Published April 2012.Originallyapproved in 1993.Last previous edition approved in 2006 as D5354 95(2006).DOI:10.1520/D5354-95R12.2For 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 S=strength of KOH solution,mg of KOH/mL,and0.0006791=molecular ratio of(K H):KOH divided by1000.6.2 Total Active IngredientsCalculate the total active in-gredients as follows:Total active ingredients,%5B 2 C!/D#3100(2)where:B=weight of residue,g,C=alkali correction,andD=weight of sample,g.6.3 Total Active Ingredients Calculation Method(for Sul-fated Oils Only)Calculate the total active ingredients by thecalculation method that is applicable to sulfated oils only,asfollows:T 5 P1NaSO42/SO2!3Y#(3)orT 5 P11.48753Y(4)where:T=total active ingredients,%P=total desulfated fatty matter,%,andY=percentage of combined SO3.NOTE3The factor 1.4875 is based on the assumption that thedesulfated fatty matter becomes polymerized at the point where the SO3splits off and no hydroxyl groups are formed.If the latter are formed thefactor b