ASTM_D_2358_-_89_2009.pdf

Designation:D235889(Reapproved 2009)Standard Test Method forSeparation of Active Ingredient from Surfactant and SyndetCompositions1This standard is issued under the fixed designation D2358;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 procedure for the separationand purification of active ingredient from surfactants andsyndet compositions.The separated active ingredient may beused for qualitative examinations.This test method alsopermits the estimation of total active ingredient level present inthe sample under test.1.2 This test method yields the active ingredient togetherwith other alcohol-soluble materials and therefore is usefulonly in estimating the actual active ingredient level.Correctionfor the amount of the most common contaminant,sodiumchloride,is shown by a separate determination.1.3 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.4 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.Material SafetyData Sheets are available for reagents and materials.Reviewthem for hazards prior to usage.2.Referenced Documents2.1 ASTM Standards:2D1681 Test Method for Synthetic Anionic Active Ingredientin Detergents by Cationic Titration Procedure3.Summary of Test Method3.1 The test method involves the extraction of the activeingredient with alcohol.Reprecipitation of the insolubles isspecified to remove the last traces of active ingredient.Dilutionof the alcoholic extract to a known volume and the evaporationof a suitable aliquot permits measurement of total alcohol-soluble matter.An estimation of sodium chloride content ismade so that a corrected total active ingredient level may beobtained.Provision is made for purification of the activeingredients in Section 14.4.Reagents4.1 Purity of Reagents:4.1.1 Reagent grade chemicals shall be used in all tests.Unless otherwise indicated,it is intended that all reagents shallconform to the specifications of the Committee on AnalyticalReagents of the American Chemical Society,where suchspecifications are available.3Other grades may be used,pro-vided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.4.2 Unless otherwise indicated,references to water shall beunderstood to mean distilled water or water of equal purity.SEPARATION OF TOTAL ALCOHOL-SOLUBLEMATTER5.Reagents5.1 Ethyl Alcohol(95 percent)Freshly boiled ethyl alcoholconforming to Formula No.3A or No.30 of the U.S.Bureauof Internal Revenue.The alcohol should not be neutralized.Redistilled alcohol shall be used if alkali absorption is morethan 0.2 mL of 0.1 N NaOH solution/100 mL of alcohol.5.2 Ethyl Alcohol(Absolute)Freshly boiled 200-proofethyl alcohol conforming to either Formulas No.3A or No.30of the U.S.Bureau of Internal Revenue.5.3 Phenolphthalein Indicator Solution(10 g/L)Dissolve1 g of phenolphthalein in 50 mL of ethyl alcohol(95%)andthen mix with 50 mL of water.1This test method is under the jurisdiction of ASTM Committee D12 on Soapsand Other Detergents and is the direct responsibility of Subcommittee D12.12 onAnalysis and Specifications of Soaps,Synthetics,Detergents and their Components.Current edition approved Oct.1,2009.Published December 2009.Originallyapproved in 1965 as D2358 65 T.Last previous edition approved in 2003 asD2358 89(2003).DOI:10.1520/D2358-89R09.2For 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.3Reagent Chemicals,American Chemical Society Specifications,AmericanChemical Society,Washington,DC.For suggestions on the testing of reagents notlisted by the American Chemical Society,see Analar Standards for LaboratoryChemicals,BDH Ltd.,Poole,Dorset,U.K.,and the United States Pharmacopeiaand National Formulary,U.S.Pharmacopeial Convention,Inc.(USPC),Rockville,MD.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 5.4 Sulfuric Acid(1+100)Add 1 mL of concentratedsulfuric acid(H2SO4,sp gr 1.84)to 100 mL of water.6.Safety Precautions6.1 Formulas No.3A and No.30 ethyl alcohols are dena-tured alcohols.They are health hazards and flammable liquids.See manufacturers label warning as to use,safe handling,anddisposal.6.2 Sulfuric acid is corrosive.Use proper protective equip-ment including adequate eye prot