ASTM_D_2082_-_92_1998.pdf

Designation:D 2082 92(Reapproved l998)Standard Test Method forPercent of Non-Amines in Fatty Nitrogen Compounds1This standard is issued under the fixed designation D 2082;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.1.1Scope1.1 This method covers the determination of the percentageof non-amine components in fatty amines and diamines.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.Summary of Test Method3.1 Aspecimen of the fatty amine compound is dissolved inalcohol and passed through an ion exchange column.Theamine components of the specimen are retained on the columnand the nonamine components pass through the column and arecollected and weighed.A correction factor is applied to correctfor any amine components that pass through the column.4.Apparatus4.1 Chromatographic Columns,made by attaching 500-mLbulbs with 24/40 joints to chromatographic tubes and withattached fritted-glass disks inside a 19/22 joint(Fig.1).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 onAnalytical Reagents of theAmerican Chemical Society3,where such specifications are available.Other 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(0.2N)Add 34mLof concentrated HCl(sp gr 1.19)to 1000 mLof isopropanolin a 2-L volumetric flask.Make up to volume after cooling toroom temperature.Standardize against sodium carbonate usingbromcresol green as the indicator.5.5 Methanol,Ethanol,or Isopropanol(99%).5.6 Resin,Cationic,Ion-Exchange,500 to 100 mesh.1This 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 2082 65 T.Last previous edition D 2082 82(1987).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.FIG.1 Diagram of Chromatographic Columns1AMERICAN SOCIETY FOR TESTING AND MATERIALS100 Barr Harbor Dr.,West Conshohocken,PA 19428Reprinted from the Annual Book of ASTM Standards.Copyright ASTM6.Preparation of Chromatographic Columns6.1 Place the resin in a 250-mL beaker,pour 100 mL ofmethanol,ethanol,or isopropanol on the resin,and stir.6.2 Filter with suction through a 350-mL coarse sintered-glass funnel.Repeat until there is no residue left uponevaporation of the alcohol used to wash the resin.Transfer thewashed resin to a bottle and add enough isopropyl alcohol tojust cover the resin.6.3 To fill the chromatographic column first placeapproximately 10 mm of glass wool on top of the fritted-glassdisk then pour a slurry of resin in methanol,ethanol,orisopropanol on top of the glass wool.For fatty amines use a200-mm column and pour in enough resin to just fill thecolumn after the resin has settled.For fatty diamines a 500-mmcolumn should be packed with 450 mm of resin.Once the resinhas been placed in the column,keep it covered with alcohol atall times.NOTE1Blanks should be run on each new batch of resin.Use 80 g ofresin for duplicate determinations of fatty amines using 200-mm columnsand 200 g of resin for duplicate determinations using 500-mm columns forfatty diamines.Experience has shown that the total quantity of methanol,ethanol,or isopropanol required for washing the resin is 400 mL for 80-gbatches and 900 mL for 200-g batches of resin.7.Procedure7.1 Accurately weigh into a 150-mLbeaker approximately 5g of the sample for fatty amines or 2.5 g of the