ASTM_D_1615_-_60_1995e1.pdf

Designation:D 1615 60(Reapproved 1995)e1Standard Test Methods forGlycerol,Ethylene Glycol,and Pentaerythritol in Alkyd Resins1This standard is issued under the fixed designation D 1615;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.e1NOTEKeywords were added editorially and editorial changes made throughout in May 1995.1.Scope1.1 These test methods cover the determination of glycerol,ethylene glycol,and pentaerythritol in alkyd resins and resinsolutions.Other polyhydric alcohols that can be oxidized byperiodic acid to formaldehyde or formic acid,or both,willinterfere with the determination of glycerol and ethylene glycol(see Test Methods D 2456 or D 2998).Urea,melamine,orphenolic resins interfere and render this procedure inappli-cable.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 563 Test Method for Phthalic Anhydride Content ofAlkyd Resins and Resin Solutions2D 1193 Specification for Reagent Water3D 1398 Test Method for Fatty Acid Content of AlkydResins and Alkyd Resin Solutions2D 2456 Test Method for Identification of Polyhydric Alco-hols in Alkyd Resins2D 2998 Test Method for Polyhydric Alcohols in AlkydResins23.Purity of Reagents3.1 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.4Other 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.3.2 Unless otherwise indicated,references to water shall beunderstood to mean reagent water conforming to SpecificationD 1193.3NOTE1The reagents and samples used in these methods may,undersome conditions,be hazardous.Refer to the manufacturers MaterialSafety Data Sheets for specific handling and safety precautions.Safelaboratory handling procedures and all applicable OSHAregulations are tobe followed.GLYCEROL AND ETHYLENE GLYCOL4.Summary of Test Method4.1 The primary hydroxyl groups of ethylene glycol andglycerol are oxidized to formaldehyde by periodic acid;thesecondary hydroxyl group of glycerol is oxidized to formicacid.By acidimetric and iodometric titration,the proportions offormic acid and formaldehyde can be determined respectively,and calculated to glycerol and ethylene glycol by algebraicequations.The equations for the oxidation of the polyhydricalcohols are as follows:1These test methods are under the jurisdiction ofASTM Committee D-1 on Paintand Related Coatings,Materials,and Applications and are the direct responsibilityof Subcommittee D01.33 on Polymers and Resins.Current edition approved Sept.19,1960.Originally issued 1958.ReplacesD 1615 58 T.2Annual Book of ASTM Standards,Vol 06.03.3Annual Book of ASTM Standards,Vol 11.01.4Reagent 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.Pharmaceutical Convention,Inc.(USPC),Rockville,MD.1AMERICAN SOCIETY FOR TESTING AND MATERIALS100 Barr Harbor Dr.,West Conshohocken,PA 19428Reprinted from the Annual Book of ASTM Standards.Copyright ASTMC3H8O3+2H5I06glycerolperiodicacid2HCHO+HCOOH+2HIO3+5H2Oformal-formiciodicwaterdehydeacidacidC2H6O2+H5I06ethyleneperiodicglycolacid2HCHO+HIO3+3H2Oformal-iodicwaterdehydeacidWith pentaerythritol,there is no reaction.5.Apparatus5.1 Burets,50 and 100-mL capacity.5.2 Pipets,20 and 50-mL capacity.5.3 Beakers,two of 400-mL capacity.5.4 Erlenmeyer Flasks,four of 1000-mL capacity,glass-stoppered.5.5 Volumetric Flasks,two of 100-mL capacity.5.6 Graduated Cylinder,10-mL capacity.5.7 Filter Paper,fast,qualitative grade.5.8 Watch Glass.6.Reagents6.1 Methyl Purple Indicator Solution.56.2 Periodic Acid(11 g/L)Dissolve 11 g of periodic acid(HIO4)in water and dilute to 1 L.Prepare fresh daily and storein a brown bottle.6.3 Potassium Iodide Solution(200 g/L)Dissolve 200 g ofpotassium iodide(KI)in water and dilute to 1 L.6.4 Sodium Hydroxide,Standard Solution(0.1 N)Prepareand standardize a 0.1 N aqueous sodium hydroxide(NaOH)solution.6.5 Sodium Thiosulfate,Standard Solution(0.2 N)Prepare and standardize a 0.2 N aqueous sodium thiosulfate(Na2S2O3)solution.6.6 Starch Indicator SolutionDissolve 5 g of solublestarc