ASTM_D_2195_-_00.pdf

Designation:D 2195 00Standard Test Methods forPentaerythritol1This standard is issued under the fixed designation D 2195;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.1.Scope*1.1 These test methods cover the testing of pentaerythritolfor use in the manufacture of alkyd resins and other syntheticresins.1.2 The test procedures appear in the following sections:SectionSulfate ash5 to 10Moisture11 to 16Hydroxyl17 to 22Assay(by dibenzal)23 to 29Assay(by gas chromatography)30 to 41Phthalate ester color42 to 491.3 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 34.1.4 For hazard information and guidance,see the suppliersMaterial Safety Data Sheet.2.Referenced Documents2.1 ASTM Standards:D 1193 Specification for Reagent Water2D 1209 Test Method for Color of Clear Liquids(Platinum-Cobalt Scale)3D 1615 Test Methods for Glycerol,Ethylene Glycol,andPentaerythritol in Alkyd Resins4D 1728 Test Method for Phthalate Ester Color of High-Gravity Glycerin5D 2593 Test Method for Butadiene Purity and HydrocarbonImpurities by Gas Chromatography6E 1 Specification for ASTM Thermometers7E 180 Practice for Determining the Precision Data ofASTM Methods for Analysis and Testing of IndustrialChemicals8E 200 Practice for Preparation,Standardization,and Stor-age of Standard Solutions for Chemical Analysis8E 203 Test Method for Water Using Volumetric Karl FischerTitration8E 222 Test Methods for Hydroxyl Groups by Acetic Anhy-dride Acetylation8E 260 Practice for Packed Column Gas Chromatography93.Significance and Use3.1 These test methods provide a measurement of sulfate,ash,moisture(water),hydroxyl content,assay by dibenzal andgas chromatography,and phthalate ester color of pentaerythri-tol.The results of these measurements can be used forspecification acceptance.4.Purity of Reagents4.1 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.10Other grades may be used,provided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.4.2 Unless otherwise indicated,references to water shall beunderstood to mean Type IV of reagent water conforming toSpecification D 1193.SULFATE ASH5.Summary of Test Method5.1 The organic matter is burned off,the residue treated withsulfuric acid,ignited,and the ash weighed.6.Apparatus6.1 Crucible or DishA silica,quartz,or platinum crucible1These test methods are under the jurisdiction ofASTM Committee D-1 on Paintand Related Coatings,Materials,and Applications and are the direct responsibilityof Subcommittee D01.35 on Solvents,Plasticizers,and Chemicals Intermediates.Current edition approved Jan.10,2000.Published March 2000.Originallypublished as D 2195 63 T.Last previous edition D 2195 95.2Annual Book of ASTM Standards,Vol 11.01.3Annual Book of ASTM Standards,Vol 06.04.4Annual Book of ASTM Standards,Vol 06.03.5Discontinued,see 1991 Annual Book of ASTM Standards,Vol 06.03.6Annual Book of ASTM Standards,Vol 05.01.7Annual Book of ASTM Standards,Vol 14.03.8Annual Book of ASTM Standards,Vol 15.05.9Annual Book of ASTM Standards,Vol 14.02.10Reagent 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.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM,100 Barr Harbor Drive,West Conshohocken,PA 19428-2959,United States.or dish having a capacity of 50 to 60 mL.6.2 Bunsen Burner.6.3 Electric Muffle Furnace,maintained at 600 6 25C.7.Reagents and Materials7.1 Sulfuric Acid(1+1)Carefully mix 1 volume of con-centrated sulfuric acid(H2SO4,sp gr 1.84)with 1 volume ofwater.8.Procedure8.1 Preignite the crucible or dish at 600C,transfer to adesiccator,and when cool,weigh to 0.1 mg.Place approxi-mately 20 g of the sample in the crucible or dish and weigh to0.1 mg.Heat gently with a gas flame and ignite the specimen,allowing it to burn completely.Cool somewhat,and thenmoisten the residue with 10 to 20 drops of H2SO4(1+1).Cautiously ignite until the carbon is completely consumed.Finally,ignite in the muffle furnac