ASTM_D_1439_-_03_2008e1.pdf

Designation:D143903(Reapproved 2008)1Standard Test Methods forSodium Carboxymethylcellulose1This standard is issued under the fixed designation D1439;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.1NOTEEditorial changes were made in Sections 11,12,15.5,and 31.1 in June 2008.1.Scope1.1 These test methods cover the testing of sodium car-boxymethylcellulose.1.2 The test procedures appear in the following order:SectionsMoisture4 9Degree of Etherification:Test Method AAcid Wash10 17Test Method BNonaqueous Titration10,12,18 23Viscosity24 30Purity31 38Sodium Glycolate39 47Sodium Chloride48 55Density56 621.3 The values stated in SI units are to be regarded as thestandard.The values given in parentheses are for informationonly.1.4 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 15.1 and 20.2.Referenced Documents2.1 ASTM Standards:2D1347 Test Methods for Methylcellulose(Withdrawn2003)3E1 Specification for ASTM Liquid-in-Glass Thermometers3.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 Society4,where suchspecifications are available.Other 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 distilled water.MOISTURE4.Scope4.1 This test method covers the determination of the volatilecontent of sodium carboxymethylcellulose.4.2 The results of this test are used for calculating the totalsolids in the sample;and,by common usage,all materialsvolatile at this test temperature are designated as moisture.5.Significance and Use5.1 Moisture analysis(along with purity)is used to calculatethe amount of active polymer in the material and must beconsidered when determining the amount of sodium carboxym-ethylcellulose to use in various formulations.6.Apparatus6.1 OvenGravity convection oven,capable of maintaininga temperature of 105 6 3C.6.2 Weighing Bottles,low-form,50-mm inside diameter by30-mm height,or equivalent.6.3 Analytical Balance.7.Procedure7.1 Weigh 3 to 5 g of the sample to the nearest 0.001 g in atared and covered weighing bottle.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 June 1,2008.Published June 2008.Originallyapproved in 1956.Last previous edition approved in 2003 as D1439 03.DOI:10.1520/D1439-03R08E01.2For 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.3The last approved version of this historical standard is referenced onwww.astm.org.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 7.2 Place the bottle in an oven at 105C for 2 h with thecover removed.Cool the bottle in a desiccator,replace thecover,and weigh.7.3 Replace the sample in the oven for 30 min,cool,andreweigh.7.4 Continue this procedure to a mass loss of not more than5 mg for 30 min drying time.8.Calculation8.1 Calculate the percent moisture,M,as follows:M 5A/B!3100(1)where:A=mass loss on heating,g,andB=sample used,g.9.Precision and Bias9.1 PrecisionStatistical analysis of interlaboratory repro-ducibility test results on samples containing 2 to 10%moistureindicates a precision of 60.2%absolute at the 95%confi-dence level.9.2 BiasNo justifiable statement can be made on the biasof the procedure for measuring moisture because no suitablereference material exists.DEGREE OF ETHERIFICATION10.Scope10.1 These test methods cover the determination of thedegree of etherification(D.E.)of sodium carboxymethylcellu-lose.10.2 Two test methods are included as follows:10.2.1 Test Method A(Acid Wash),for