ASTM_D_2363_-_79_2011.pdf

Designation:D236379(Reapproved 2011)Standard Test Methods forHydroxypropyl Methylcellulose1This standard is issued under the fixed designation D2363;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 the testing of hydroxypropylmethylcellulose.1.2 The test procedures appear in the following order:SectionsMoisture4 to 6Ash(as Sulfate)7 to 10Chlorides(as NaCl)11 to 14Alkalinity(as Na2CO3)15 to 18Iron19 to 24Heavy Metals25 to 29Methoxyl Content30 to 35Hydroxypropoxyl Content36 to 41Viscosity42 to 46pH47Solids48 to 51Density52 to 561.3 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 a specifichazard statement,see 33.5.1.2.Referenced Documents2.1 ASTM Standards:2D96 Test Method for Water and Sediment in Crude Oil byCentrifuge Method(Field Procedure)(Withdrawn 2000)3E70 Test Method for pH of Aqueous Solutions With theGlass Electrode3.Purity of Reagents3.1 Reagent grade chemicals shall be used in all tests.Unless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 distilled water.MOISTURE4.Scope4.1 This test method covers the determination of the volatilecontent of hydroxypropyl methylcellulose and,by commonusage,designated moisture.5.Procedure5.1 Transfer 2 to 5 g of the sample weighed to the nearest0.01 g to a tared dish(fitted with a lid)and dry for 2 h in anoven at 100 to 105C with lid removed.Remove the dish fromthe oven,cover with a lid,cool in a desiccator,and weigh.6.Calculation6.1 Calculate the percent of moisture as follows:Moisture,%5A/B!3100(1)where:A=mass loss on heating,andB=sample used,g.ASHAS SULFATE7.Scope7.1 This test method covers the determination of the amountof residue left from igniting a sample of hydroxypropylmethylcellulose after being moistened with sulfuric acid.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 1,2011.Published June 2011.Originallyapproved in 1965.Last previous edition approved in 2006 as D2363 79(2006).DOI:10.1520/D2363-79R11.2For 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 8.Reagents8.1 Nitric Acid(sp gr 1.42)Concentrated nitric acid(HNO3).8.2 Sulfuric Acid(sp gr 1.84)Concentrated sulfuric acid(H2SO4).9.Procedure9.1 Weigh to the nearest 0.01 g about 2 g of the sample(previously dried for12h at 105C)into a tared Coors No.1,high-form,porcelain crucible.Add 5 drops of H2SO4aroundthe inside surface of the crucible.Place the crucible inside of aloosely fitting aluminum ring(approximately 32 mm(114in.)high,with 6.4-mm(14-in.)sidewall,and 44-mm(134-in.)inside diameter,cut from a piece of aluminum pipe)on a hotplate.Loosely cover with a crucible cover.Carefully char thehydroxypropyl methylcellulose until all the volatiles are re-moved.9.2 Cool the crucible,add 1 ml of H2SO4and 2 ml of HNO3so that it completely wets the charred residue.Cautiously heatto dense white fumes on a hot plate.Place the uncoveredcrucible in a muffle furnace at 600C and ignite until all thecarbon is gone(for about 1 h).Transfer to a dessicator untilcool,then weigh.(Save the residue for the Heavy Metalsdetermination.)10.Calculation10.1 Calculate the percent o