1、Designation:D 1847 93(Reapproved 1998)Standard Test Methods forTotal Chlorine Content of Epoxy Resins1This standard is issued under the fixed designation D 1847;the number immediately following the designation indicates the year oforiginal adoption or,in the case of revision,the year of last revisio
2、n.A number in parentheses indicates the year of last reapproval.Asuperscript epsilon(e)indicates an editorial change since the last revision or reapproval.1.Scope1.1 These test methods cover the determination of the totalchlorine content,in concentrations below 1 weight percent,ofepoxy resins.Both o
3、rganic and inorganic chlorine compoundscontained in the resin are determined.Epoxy resin is defined asthe reaction product of a chlorohydrin and a di-or polyfunc-tional phenolic compound.1.2 Two alternative test methods for determining chlorideion concentration resulting from combustion of the sampl
4、e areincluded as follows:SectionsTest Method APotentiometric TitrationTest Method BGravimetric Determination6-1011-151.3 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 s
5、afety 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 The resin is oxidized by combustion in a bomb contain-ing oxygen under pressure.The chlorine
6、compounds thusliberated are absorbed in a sodium carbonate solution.In TestMethod A the amount of chlorine present is determined bypotentiometric titration with standard silver nitrate solution.InTest Method B the amount of chlorine present is determinedgravimetrically by precipitation as silver chl
7、oride.4.Significance and Use4.1 The total chlorine content of epoxy resins is an impor-tant variable in determining reactivity of epoxy resins andperformance of coatings prepared from them.These testmethods may be used to determine the total chlorine content ofmanufactured epoxy resins to confirm sp
8、ecification limits.5.Purity of Reagents5.1 Reagent grade chemicals shall be used in all tests.Unless otherwise indicated,it is intended that all reagents shallconform to the specifications of the Committee on AnalyticalReagents of the American Chemical Society,where suchspecifications are available.
9、3Other grades may be used,pro-vided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.5.2 Unless otherwise indicated,references to water shall beunderstood to mean reagent water conforming to Type II ofSpecific
10、ation D 1193.TEST METHOD APOTENTIOMETRIC TITRATION6.Apparatus6.1 Combustion ApparatusAn oxygen bomb4apparatusfor combustion of the sample.6.2 Titration ApparatusA suitable pH meter equippedwith a glass-silver electrode system and titration stand,stirrer,beakers,and 10-mL buret.7.Reagents7.1 Methyl R
11、ed Indicator(0.2%alcohol solution)Dissolve 0.2 g of methyl red in 100 mL of methanol,ethanol orisopropanol.7.2 Nitric Acid(sp gr 1.42)Concentrated nitric acid(HNO3).7.3 Oxygen,free of combustible materials and halogencompounds,available at a pressure of 40 atm.7.4 Silver Nitrate,Standard Solution(0.
12、01 N)Dissolve inwater 1.70 6 0.01 g of crystalline silver nitrate(AgNO3)which1These test methods are under the jurisdiction ofASTM Committee D-1 on Paintand Related Coatings,Materials,and Applications and are the direct responsibilityof Subcommittee D 01.33 on Polymers and Resins.Current edition app
13、roved April 15,1993.Published June 1993.Originallypublished as D 1847 61 T.Last previous edition D 1847 87.2Annual 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
14、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.4The sole source of supply of the double-valve,self-sealing oxygen bombequipped with
15、a safety-relief-type oxygen filling connection,ignition circuit,fusewire,sample cups,and water bath,known to the committee at this time is ParrInstrument Co.,209 53rd St.,Moline,IL 61265.If you are aware of alternativesuppliers,please provide this information to ASTM Headquarters.Your commentswill r
16、eceive careful consideration at a meeting of the responsible technicalcommittee,1which you may attend.1Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959,United States.previously has been pulverized,dried at 150C for 1 h,andstored in a glass-stoppered bottle,and dilute to 1 L.Standardizeagainst an accurately weighed amount of sodium chloride(NaCl)dissolved in 75 to 100 mL of water.7.5 Sodium Carbonate Solution(20 g/L)Dissolve 20 g ofsodium carbonate(Na