ASTM_D_2075_-_92_1998.pdf

Designation:D 2075 92(Reapproved 1998)Standard Test Method forIodine Value of Fatty Amines,Amidoamines,and Diamines1This standard is issued under the fixed designation D 2075;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(e)indicates an editorial change since the last revision or reapproval.This method was prepared jointly by the American Society for Testing and Materials and the American Oil Chemists Society.1.Scope1.1 This test method(Note 1)covers the determination ofthe iodine value of fatty amines,diamines,and amidoaminesby the Wijs procedure.NOTE1This test method is essentially equivalent to Test MethodsD 2078 and D 1959.Use of mercuric acetate permits reduced reactiontime compared to Test Methods D 2078(30 min)and D 1959(1 h).1.2 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:D 1193 Specification for Reagent Water2D 1541 Test Method for Total Iodine Value of Drying Oilsand Their Derivatives3D 1959 Test Method for Iodine Value of Drying Oils andFatty Acids3D 2078 Test Method for Iodine Value of Fatty QuaternaryAmmonium Chlorides33.Terminology3.1 Definition:3.1.1 iodine valuea measure of the unsaturation of thealkyl group or groups,expressed in terms of percent iodineabsorbed.4.Significance and Use4.1 This test method measures the unsaturation of the alkylgroups as iodine value by addition of an iodine/chlorinereagent.4.2 Where no conjugated double bonds are present,theiodine value obtained is a measure of the total unsaturation,and the values obtained are useful for comparative purposes.4.3 If conjugated unsaturation is known to be present,useTest Method D 1541.5.Apparatus5.1 BottlesGlass-stoppered bottles or wide-mouth Erlen-meyer flasks of 500-mL capacity.NOTE2Wide-mouth bottles or flasks are essential if stirring is doneby mechanical means.5.2 Pipets,20 and 25-mL capacity.6.Reagents6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests.Unless otherwise indicated,it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.4Other grades may beused,provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.6.2 Purity of WaterUnless otherwise indicated,referencesto water shall be understood to mean reagent water conformingto Type II of Specification D 1193.6.3 Acetic Acid(Glacial)Verify the absence of sub-stances reducing permanganate as follows:Dilute 2 mL of theacid with 10 mL of water and add 0.1 mL of 0.1 N potassiumpermanganate(KMnO4)solution.The pink color should not beentirely discharged at the end of 2 h.56.4 Chlorine(99.8%Cl)Commercial grades of chlorineavailable in cylinders may be used,provided the gas is dried by1This method is under the jurisdiction of ASTM Committee D-1 on Paint andRelated Coatings,Materials,and Applications and is the direct responsibility ofSubcommittee D01.32 on Drying Oils.Current edition approved March 15,1992.Published May 1992.Originallypublished as D 2075 62.Last previous edition D 2075 89.2Annual Book of ASTM Standards,Vol 11.01.3Annual Book of ASTM Standards,Vol 06.03.4Reagent 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.5“Analytical reagents,ACS Specifications,”Am.Chemical Soc.,Washington,DC,1950.1Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959,United States.passing through concentrated sulfuric acid(H2SO4,sp gr 1.84)before passing it into the iodine solution(see 6.10).Alterna-tively,the chlorine may be prepared by allowing concentratedhydrochloric acid(HCl,sp gr 1.19)to drop onto potassiumpermanganate(KMnO4)or onto a mixture of KMnO4andmanganese dioxide(MnO2).Dry the gas thus generated bypassing it through H2SO4(sp gr 1.84).6.5 Chloroform.6.6 Mercuric Acetate SolutionDissolve 2.5 g of mercuricacetate(Hg(C2H3O2)2)in glacial acetic acid(CH3COOH)andmake up to 100 mL.6.7 Potassium Iodide Solution(150 g/L)Dissolve 150 g ofpotassium iodide(KI)in water and dilute to 1 L.6.8 Sodium Thiosulfate,Standard Solution(0.1 N)Dissolve 24.8 g of sodium thiosulfate(Na2S2O35H2O)inwater and dilute to 1 L.Standardize against potassium dichro-mate(K2Cr2O7)6as follo