ASTM_D_1013_-_93_1998.pdf

Designation:D 1013 93(Reapproved 1998)Standard Test Method forDetermining Total Nitrogen in Resins and Plastics1This standard is issued under the fixed designation D 1013;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 standard has been approved for use by agencies of the Department of Defense.1.Scope1.1 This test method covers the determination of totalnitrogen in nitrogen-containing plastics,resins,and resinsolutions.This test method is not applicable for use onmaterials containing nitro-groups.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.Significance and Use3.1 Total nitrogen content gives an indication of the level orpurity of a nitrogen-containing material such as an amine resin.It is important for the quality control of amine resins and isoften used to determine whether the proper amounts of manytypes of nitrogen-containing materials are present in formu-lated products.4.Apparatus4.1 Kjeldahl Flasks,for digestion and distillation,800-mLcapacity,moderately heavy wall,and made of hard glass.4.2 Connecting Bulbs,of the Davisson type,or a bulbequally effective in preventing mechanical carry-over of thecontents of the distillation flask to the condenser.4.3 Digestion and Distillation EquipmentA suitableKjeldahl digestion and distillation apparatus,such as any of thewell-known commercial units for multiple work.The unitsmay be heated either electrically or by gas burner.4.4 Connecting Tubes made of moderately heavy-wall glasstubing,6 to 8 in.(150 to 200 mm)in length,for conducting thedistillate from the condenser to the receiver.4.5 Weighing Tube(for Liquid Resins)Any convenientdevice for weighing a few grams of sample in a matter suchthat no loss of volatile constituents will be sustained during theweighing operation.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,referenceto water shall be understood to mean reagent water conformingto Type II of Specification D 1193.5.3 Hydrochloric or Sulfuric Acid,(standard 0.5 N)Dilute43 mL of HCl(sp gr 1.19)or 14 mL of H2SO4(sp gr 1.84)to1 L with water.Standardize against the 0.5 N NaOH solution(3.7),using the same indicator as will be used in titration of thespecimen(4.4).5.4 Metallic Mercury or Mercuric Oxide.5.5 Methyl Purple Indicator Solution.NOTE1Methyl purple has recently met with considerable favor,andis to be recommended because of the abruptness of its color change in thepresence of ammonium salts.This indicator may be purchased in solutionform ready for use.5.6 Methyl Red Indicator SolutionDissolve 0.2 g of me-thyl red in 100 mL of methanol,ethanol,or isopropanol.5.7 Potassium Sulfate.5.8 Sodium Hydroxide Solution(760 g/L)Dissolve 1000 gof technical grade NaOH in 1 L of water.5.9 Sodium Hydroxide,Standard Solution(0.5 N)Preparea 0.5 N NaOH solution free of carbonates,using reagent gradeNaOH,and standardize against the National Bureau of Stan-dards standard reference material No.84 of potassium acid1This test method is under the jurisdiction of ASTM Committee D-1 on Paintand Related Coatings,Materials,and Applications and is the direct responsibility ofSubcommittee D01.33 on Polymers and Resins.Current edition approved April 15,1993.Published June 1993.Originallypublished as D 1013 49.Last previous edition D 1013 88.2Annual 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.phthalate,using phenolphthalein indicator.Protect the solutionagainst CO2absorption.5.10 Sulfide or Thiosulfate SolutionDissolve 40 g of K2Sor Na2S,or 80 g of Na2S2O35H2O,in water and dilute to 1 L.5.11 Sulfuric Acid(sp gr 1.