ASTM_D_1347_-_72_1995.pdf

Designation:D 1347 72(Reapproved 1995)Standard Test Methods forMethylcellulose1This standard is issued under the fixed designation D 1347;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.Scope1.1 These test methods cover the testing of methylcellulose.1.2 The test methods appear in the following order:SectionsMoisture4 and 5Ashas Sulfate6-8Chloridesas Sodium Chloride9-11Alkalinityas Na2CO312-14Iron15-19Heavy Metals20-22Methoxyl Content23-26Viscosity:Water-Soluble Methylcellulose27-29Alkali-Soluble Methylcellulose30 and 31pH32Solids33 and 34Density35-391.3 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.For a specific hazard statement,seeNote 1.2.Referenced Documents2.1 ASTM Standards:D 96 Test Methods for Water and Sediment in Crude Oil byCentrifuge Method(Field Procedure)23.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.3Other 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.Procedure4.1 Transfer 2 to 5 g of the sample,weighed to the nearest0.01 g,to a tared dish(fitted with a lid)and dry it for 3 h in anoven at 105 6 3C.Remove the dish from the oven,cover itwith a lid,cool in a desiccator,and weigh.5.Calculation5.1 Calculate the percent moisture,M,as follows:M 5A/B!3 100(1)where:A5 mass loss on heating,g,andB5 sample used,g.ASHAS SULFATE6.Reagent6.1 Sulfuric Acid(sp gr 1.84)Concentrated sulfuric acid(H2SO4).7.Procedure7.1 Weigh,to the nearest 0.01 g,about 2 g of the sample(previously dried for12h at 105C)and transfer it to a taredplatinum crucible.Place it in a muffle furnace at 575 6 25Cfor approximately12h,to char the organic material.7.2 Cool the crucible and add 1 mL of H2SO4so that itcompletely wets the charred residue.Then cautiously heat itover a small flame to dense white fumes.Place the crucible ina muffle furnace at 575 6 25C and leave it there until all signsof carbon are gone(approximately 1 h).Transfer the specimento a desiccator until cool,then weigh.8.Calculation8.1 Calculate the percent of ash,C,as follows:C 5A/B!3 100(2)where:1These test methods are under the jurisdiction ofASTM Committee D-1 on Paintand Related Coatings,Materials,and Applications,and are the direct responsibilityof Subcommittee D01.36 on Cellulose and Cellulose Derivatives.Current edition approved Feb.9,1972.Published March 1972.Originallypublished as D 1347 54 T.Last previous edition D 1347 64.2Annual Book of ASTM Standards,Vol 05.01.3Reagent 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.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 ASTMA5 ash,g,andB5 sample used,g.CHLORIDESAS SODIUM CHLORIDE9.Reagents9.1 Ferric Alum Indicator SolutionAdd 100 g of ferricaluminum sulfate(Fe2SO4)3(NH4)2SO4 24H2O)to 250 mL ofwater.Heat it to boiling and add HNO3(sp gr 1.42)slowly untilthe red color is removed.This will usually require about 6 to 15mL of HNO3.Filter the solution and store it in a glass bottle.9.2 Potassium Thiocyanate,Solution,Standard(0.1 N)Dissolve 10 g of potassium thioagonate(KCNS)in 1 L ofwater.By means of a pipet,measure 25 mL of 0.1000 NAgNO3solution into a 400-mL beaker.Add 100 mL of water,10 mL of nitric acid(NHO3,sp gr 1.42)and 5 mL of ferricalum indicator solution.Titrate with the KCNS solution,whilestirring,until a faint persistent red color is produced.Calculatethe normality of the KCNS solution,N,as follows:N 5A/B!3 0.1(3)where:A5 0.100 N AgNO3solution added,mL,andB5 KCNS solution required for the titration,mL.9.3 Silver Nitrate,Solution,Standard(0.1 N)Grind silvernitrate(AgNO3)crystals fine enough to pass through a 850-m(No.20)sieve,and then dry for 2 h at 110C.Prepare a 0.1000N solution by dissolving 16.989 g of dry AgNO3in chloride-free water and diluting it to 1 L in a volumetric flask.10.Proced