ASTM_D_2074_-_07_2013.pdf

Designation:D207407(Reapproved 2013)Standard Test Methods forTotal,Primary,Secondary,and Tertiary Amine Values ofFatty Amines by Alternative Indicator Method1This standard is issued under the fixed designation D2074;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.These test methods were prepared jointly by ASTM and the American Oil Chemists Society.1.Scope1.1 These alternative test methods cover the indicator pro-cedure for determining the total,primary,secondary,andtertiary amine values of fatty amines.These procedures are notapplicable to fatty amidoamines and fatty diamines.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:2D1193 Specification for Reagent Water3.Terminology3.1 Definitions:3.1.1 primary amine value,nthe number of milligrams ofpotassium hydroxide(KOH)equivalent to the primary aminebasicity in 1 g of sample.3.1.2 secondary amine value,nthe number of milligramsof potassium hydroxide(KOH)equivalent to the secondaryamine basicity in 1 g of sample.3.1.3 tertiary amine value,nthe number of milligrams ofpotassium hydroxide(KOH)equivalent to the tertiary aminebasicity in 1 g of sample.3.1.4 total amine value,nthe number of milligrams ofpotassium hydroxide(KOH)equivalent to the basicity in 1 g ofsample.4.Apparatus4.1 Erlenmeyer Flasks,wide-mouth,alkali-resistant,borosilicate-glass,250-mL capacity.4.2 Magnetic Stirrer,with an inert plastic-coated stirringbar.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 D1193.5.3 Bromphenol Blue Indicator SolutionDissolve 0.2 g ofbromphenol blue in 100 mL of methanol,ethanol,or isopro-panol.5.4 Bromcresol Green Indicator SolutionDissolve 0.1 g ofbromcresol green sodium salt in 100 mL of water.5.5 Chloroform(CHCl3).5.6 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 bromcresol green as the indicator.1These test methods are under the jurisdiction of ASTM Committee D01 onPaint and Related Coatings,Materials,and Applications and are the directresponsibility of Subcommittee D01.33 on Polymers and Resins.Current edition approved June 1,2013.Published June 2013.Originallyapproved in 1962.Last previous edition approved in 2007 as D2074 07.DOI:10.1520/D2074-07R13.2For 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 5.7 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 bromcresol green as the indicator.5.8 Isopropyl Alcohol(99%).5.9 Phenyl Isothiocyanate.5.10 Salicylaldehyde.6.Procedure for Total Amine Value6.1 Melt the sample,if it is not already liquid,in a waterbath.Mix thoroughly,and accurately weigh 1 to 4 g to 0.1 mginto a 250 mL flask.Add 50 mL of alcohol and boil for 1 minto drive off any free ammonia that may be present.Cool toroom temperature.6.2 Add 5 drops of bromphenol blue indicator and titrate,while swirling,with 0.2 N HCl to the yellow end point.7.Procedure for