ASTM_D_817_-_12.pdf

Designation:D81712Standard Test Methods of TestingCellulose Acetate Propionate and Cellulose AcetateButyrate1This standard is issued under the fixed designation D817;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 These test methods cover procedures for the testing ofcellulose acetate propionates and acetate butyrates.Theseesters may vary widely in composition and properties,socertain of the procedures can be used only in the ranges ofcomposition where they are suitable.1.2 The values stated in SI units are to be regarded as thestandard.The values given in parentheses are for informationonly.1.3 The test procedures appear in the following sections:SectionsAcetyl Propionyl or Butyryl Contents28 37Acetyl Content,Apparent18 27Acidity,Free12 17Ash7 10Color and Haze77 81Heat Stability57 65Hydroxyl Content38 44Hydroxyl Content,Primary46 50Intrinsic Viscosity67 71Moisture Content5-6Sulfur or Sulfate Content51 56Viscosity74-75Limiting Viscosity Number67 711.4 This standard does not purport to address the safetyconcerns,if any,associated with its use.It is the responsibilityof the user of this standard to establish appropriate safety andhealth practices and determine the applicability of regulatorylimitations prior to use.2.Referenced Documents2.1 ASTM Standards:2D618 Practice for Conditioning Plastics for TestingD1343 Test Method for Viscosity of Cellulose Derivativesby Ball-Drop MethodD2929 Test Method for Sulfur Content of Cellulosic Mate-rials by X-Ray FluorescenceD5897 Test Method for Determination of Percent Hydroxylon Cellulose Esters by Potentiometric TitrationAlternative Method3.Reagents3.1 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.4.Conditioning4.1 ConditioningCondition the test specimens at 23 62C(73.4 6 3.6F)and 50 6 5%relative humidity for not lessthan 40 h prior to test in accordance with Procedure A ofPractice D618,for those tests where conditioning is required.In cases of disagreement,the tolerances shall be 61C(61.8F)and 62%relative humidity.4.2 Test ConditionsConduct tests in the Standard Labora-tory Atmosphere of 23 6 2C(73.4 6 3.6F)and 50 6 5%relative humidity,unless otherwise specified in the test meth-ods.In cases of disagreements,the tolerances shall be 61C(61.8F)and 62%relative humidity.MOISTURE CONTENT5.Procedure5.1 Transfer about 5 g of the sample to a tared,low,wide-form weighing bottle and weigh to the nearest 0.001 g.Dry in an oven for 2 h at 105 6 3C.Remove the bottle fromthe oven,cover,cool in a desiccator,and weigh.1These test methods are under the jurisdiction of ASTM Committee D01 onPaint and Related Coatings,Materials,and Applications and are the directresponsibility of Subcommittee D01.36 on Cellulose and Cellulose Derivatives.Current edition approved Nov.1,2012.Published January 2013.Originallyapproved in 1944.Last previous edition approved in 2010 as D817 96(2010).DOI:10.1520/D0817-12.2For 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.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.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 6.Calculation6.1 Calculate the percentage of moisture as follows:Moisture,%5A/B!3100(1)where:A=weight loss on heating,g,andB=sample used,g.ASH7.Significance and Use7.1 Ash content gives an estimate of the inorganic contentof cellulose ester samples.The presence of high levels ofinorganic content(ash)can be detrimental to the melt stabilityand optical clarity of a cellulose ester in melt processing or actas a potential source of insolubles when the ester is used insolution.8.Procedure8.1 Dry the sample for 2 h at 105 6 3C and weigh 10 to 50g,to the nearest 0.01 to 0.1 g,depending on its ash content andthe accuracy desired.Burn directly over a flame in a 100-mLtared platinum crucible that has been heated to constant weightand weighed to the nearest 0.