ASTM_D_2073_-_92_1998e1.pdf

Designation:D 2073 92(Reapproved 1998)e1Standard Test Methods forTotal,Primary,Secondary,and Tertiary Amine Values ofFatty Amines,Amidoamines,and Diamines by RefereePotentiometric Method1This standard is issued under the fixed designation D 2073;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 methods were prepared jointly by ASTM and the American Oil Chemists Society.e1NOTEFormer Footnote 6 was deleted editorially in May 1998.1.Scope1.1 These referee test methods cover the potentiometricdetermination of the total,primary,secondary,and tertiaryamine values of fatty amines and diamines,and the total aminevalue of fatty amidoamines.Test methods for primary,second-ary,and tertiary amine values are not applicable to fattyamidoamines.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.Specific hazardstatements are given in Note 1 and Note 2 and Note 6.1.2.Referenced Documents2.1 ASTM Standards:D 1193 Specification for Reagent Water2D 2080 Test Method forAverage Molecular Weight of FattyQuaternary Ammonium Chlorides3E 70 Test Method for pH of Aqueous Solutions with theGlass Electrode43.Terminology3.1 Definitions:3.1.1 total amine valuethe number of milligrams of po-tassium hydroxide(KOH)equivalent to the basicity in 1 g ofspecimen.3.1.2 primary amine valuethe number of milligrams ofpotassium hydroxide(KOH)equivalent to the primary aminebasicity in 1 g of specimen.3.1.3 secondary amine valuethe number of milligrams ofpotassium hydroxide(KOH)equivalent to the secondary aminebasicity in 1 g of specimen.3.1.4 tertiary amine valuethe number of milligrams ofpotassium hydroxide(KOH)equivalent to the tertiary aminebasicity in 1 g of specimen.4.Apparatus4.1 Air Condenser,minimum length 650 mm.4.2 ErlenmeyerFlask,wide-mouth,alkali-resistant,borosilicate-glass,250-mL capacity.4.3 Glass Electrode pH Meter,conforming to the require-ments of Test Method E 70 or similar potentiometric titrator.4.4 Hot Plate,with variable heat control.4.5 Magnetic Stirrer,with inert plastic-coated stirring bar.4.6 Microburet,graduated to 0.02 mL and having a capacityof 10 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.5Other 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 Acetic Acid,Glacial(CH3COOH).(WarningSeeNote 1).1These 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 D 2073 62.Last previous edition D 2073 66(1987)e1.2Annual Book of ASTM Standards,Vol 11.01.3Annual Book of ASTM Standards,Vol 06.03.4Annual Book of ASTM Standards,Vol 15.05.5Reagent 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.5.4 Acetic Anhydride.5.5 Chloroform(CHCl3).(WarningSee Note 2).5.6 Hydrochloric Acid,Standard Solution(0.5 N)Add 85mLof concentrated hydrochloric acid(HCl,sp gr 1.19)to 1000mL of isopropyl alcohol in a 2-L volumetric flask.Dilute tovolume and mix.Standardize with sodium carbonate to a pH of3.5.5.7 Isopropanol(1+19)Add 5 mL of water to 95 mL ofisopropyl alcohol(99%).5.8 Perchloric Acid,Standard Solution(0.1 N)Prepareand standardize in accordance with Test Method D 2080.5.9 Salicylaldehyde.6.Hazards6.1 Fatty amines and diamines can sensitize and irritate.Wash from clothing and body surfaces immediately on contact.NOTE1Warning:Glacial acetic acid,concentrated hydrochloricacid,70 to 72%perchloric acid,and acetic anhydride can cause burns ofskin and eyes;the vapor of each is irritating to mucous membranes.Usecare in handling these acidic substa