ASTM_D_4301_-_05_2013.pdf

Designation:D430105(Reapproved 2013)Standard Test Method forTotal Chlorine in Epoxy Resins and Compounds1This standard is issued under the fixed designation D4301;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.1.Scope1.1 This test method describes a procedure for the determi-nation of total chlorine in epoxy resins and glycidyl ethers.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.For specific hazardstatements,see Section 8.2.Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD6440 Terminology Relating to Hydrocarbon ResinsE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method2.2 Other Document:OSHA Regulations,29 CFR paragraphs 1910.1000 and1910.120033.Terminology3.1 Definitions:For definitions of terms used in thisstandard,See Terminology D6440.4.Summary of Test Method4.1 The material,dissolved in dimethoxyethane(DME)orother suitable inert solvent,is reacted with sodium biphenyl toconvert bound organic chlorine to the water soluble chloride.The excess reagent is decomposed with isopropyl alcohol.Thechloride ion is then titrated potentiometrically with silvernitrate.5.Significance and Use5.1 The presence of residual chlorine in epoxy resins isdeleterious to final product properties.This test method hasbeen found to be applicable to resins or ethers with chlorinecontents ranging from 50 ppm to 35%by weight.Otherhalogen compounds react with the reagent but are distin-guished from chlorine by the final potentiometric titration.Epoxy and other functional groups will consume reagent but donot affect the results.6.Apparatus6.1 Potentiograph.6.2 Beaker,of appropriate size.6.3 Buret,of appropriate size.6.4 Stirrer,magnetic or paddle.7.Reagents7.1 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.4Other 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.7.2 Purity of WaterUnless otherwise indicated,referencesto water shall be understood to mean reagent water conformingto Type II of Specification D1193.1This test method is under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings,Materials,and Applications and is the direct responsibility ofSubcommittee D01.33 on Polymers and Resins.Current edition approved Nov.1,2013.Published November 2013.Originallyapproved in 1984.Last previous edition approved in 2005 as D4301 05.DOI:10.1520/D4301-05R13.2For 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.3A suitable mechanical holder is available from the Gardner Laboratory,Inc.,5521 Landy Lane,Washington,DC,Item 660.4Reagent 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 7.3 Sodium Biphenyl Reagent5(in ether solution).NOTE1Store in a refrigerator when not in use to prevent loss ofactivity.7.4 Nitric Acid(HNO3)(1+1),aqueous solution.7.5 1,2-Dimethoxyethane.7.6 Silver Nitrate(AgNo3),0.1 and 0.01 N standardizedsolutions.7.7 Methyl Red Indicator(0.2%alcohol solution),dissolve0.2 g of methyl red in 100 mL of methanol,ethanol,orisopropanol.7.8 Isopropyl Alcohol.8.Hazards8.1 Consult current OSHA Regulations,Suppliers MaterialSafety Data Sheets,and local regulations for all materials usedin this test method.9.Procedure9.1 Pipet 5 mL of 1,2-dimethoxyethane into a clean,dry250-mL beaker.Add a weighed amount of sample.(If thematerial is anticipated to be low in total chlorine,use 0.40 g ofsample.For materials high in chlorine,weigh 0.1 to 0.2 g ofsample.)Gently swirl to dissolve.9.2 Add about 15 mL(one bottle)of sodium biphenylreagent