ASTM_D_2076_-_92_1998.pdf

Designation:D 2076 92(Reapproved 1998)Standard Test Methods forAcid Value and Amine Value of Fatty Quaternary AmmoniumChlorides1This standard is issued under the fixed designation D 2076;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.These test methods were prepared jointly by ASTM and the American Oil Chemists Society.1.Scope1.1 These test methods cover the determination of acidvalue and amine value in fatty quaternary ammonium chlo-rides.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 Water23.Terminology3.1 Definitions:3.1.1 acid valuethe number of milligrams of potassiumhydroxide needed to neutralize 1 g of sample,and is usuallydue to amine hydrochloride.3.1.2 amine valuethe number of milligrams of potassiumhydroxide equivalent to the fatty amine basicity in 1 g ofsample.4.Apparatus4.1 Erlenmeyer Flasks,wide-mouth,alkali-resistant,boro-silicate glass,250-mL capacity.4.2 Micro Buret,10-mL capacity graduated to 0.02 mL.5.Reagents5.1 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.3Other 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.5.2 Purity of WaterUnless otherwise indicated,referencesto water shall be understood to mean reagent water conformingto Type II of Specification D 1193.5.3 Bromphenol Blue Indicator SolutionDissolve 0.2 g ofbromphenol blue in 100 mL of methanol,ethanol,or isopro-panol.5.4 Hydrochloric Acid,Standard Solution(0.1 N)Add 17mLof concentrated hydrochloric acid(HCl,sp gr 1.19)to 1000mL of isopropyl alcohol in a 2-L volumetric flask.Make up tovolume after cooling to room temperature.Standardize withsodium carbonate using 0.1%bromcresol green as the indica-tor.5.5 Hydrochloric Acid,Standard Solution(0.2 N)Add 34mL of concentrated HCl(sp gr 1.19)to 1000 mL of isopropylalcohol in a 2-L volumetric flask.Make up to volume aftercooling to room temperature.Standardize with sodium carbon-ate using 0.1%bromcresol green as the indicator.5.6 Isopropyl Alcohol(99%)Neutralize to the phenol-phthalein end point with 0.1 N methanolic sodium hydroxide(NaOH)just before running the acid value test.5.7 Phenolphthalein Indicator Solution(10 g/L)Dissolve1 g of phenolphthalein in 100 mL of methanol,ethanol,orisopropanol.5.8 Sodium Hydroxide,Standard Solution(0.1 N)Dissolve 4.0 g of sodium hydroxide(NaOH)in 1000 mL ofcold methyl alcohol.Allow to stand overnight in a cold room.Siphon the supernatant liquid into a clean bottle.After coming1These test methods are under the jurisdiction ofASTM Committee D-1 on Paintand Related Coatings,Materials,and Applications and are the direct responsibilityof Subcommittee D01.32 on Drying Oils.Current edition approved March 15,1992.Published May 1992.Originallypublished as D2076 62 T.Last previous edition D2076 64(1987)e1.2Annual Book of ASTM Standards,Vol 11.01.3Reagent 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.1Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959,United States.to room temperature,standardize the material with acid potas-sium phthalate using 1%phenolphthalein as the indicator.6.Procedure for Acid Value6.1 Melt the specimen,if it is not already liquid,in a waterbath,mix thoroughly,and weigh 5 to 20 g to 1 mg into a250-mL flask.Add 100 mL of neutralized alcohol and swirl todissolve.Heat if necessary.6.2 Add 1 mL of phenolphthalein indicator.If the solutionremains colorless,titrate with 0.1 N NaOH solution to theappearance of the first persistent pink color of the sameintensity as that of the neutralized alcohol before addition.Ifthe solution turns pink,the presence of free caustic material isindicated.If free caustic material is present proceed in accor-dance with Section 8.7.Procedure for Amine Value7.1 Weigh 5 to 20 g of sample to 1 mg into a 250-mL flask.Add 100 mLof alcohol and swirl to dissolve.Heat if necessary.7.2