ASTM_D_5040_-_90_2011.pdf

Designation:D504090(Reapproved 2011)Standard Test Methods forAsh Content of Adhesives1This standard is issued under the fixed designation D5040;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.This standard has been approved for use by agencies of the Department of Defense.1.Scope1.1 These test methods cover procedures used in determin-ing the ash content of adhesives.This standard is intended as areplacement for Method 4032.1 of Federal Test Method Stan-dard 175B,“Adhesives:Methods of Testing.”1.2 Two test methods are used:1.2.1 Test Method A is used for a starch adhesive or othertype glue,where there is no danger from the non-volatilecontent forming a rubbery mass when ignited.1.2.2 Test Method B employs nitric acid to avoid thenon-volatile residue being transformed into a viscous foamwhen ignited.1.3 These methods are not applicable to adhesives contain-ing decomposable salts such as zinc chloride.1.4 The values stated in SI units are to be regarded as thestandard.The values given in parentheses are for informationonly.1.5 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 9.2.3.2.Referenced Documents2.1 ASTM Standards:2D301 Test Methods for Soluble Cellulose Nitrate(With-drawn 2011)3D907 Terminology of AdhesivesD2415 Test Method for Ash in Coal Tar and Pitch3.Terminology3.1 DefinitionsDefinitions of terms in this standard maybe found in Terminology D907.4.Summary of Test Methods4.1 Ash content of adhesive materials is determined byheating a sample of material to remove all of the volatilecomponents.Complete oxidation and removal of all carbona-ceous material may be enhanced by the addition of concen-trated HNO3.The general method of burning the residual ashin a muffle furnace at 600 6 25C(1112 6 45F)for 8 h oruntil constant weight,is used.5.Significance and Use5.1 This test method measures the amount of inorganicmaterial in the sample.6.Apparatus6.1 Crucible,porcelain,silica or platinum with a tightlyfitting lid,having a capacity of 30 to 45 mL.6.2 Evaporating Dish,porcelain,silica,or platinum,with acapacity of 150 mL.6.2.1 Watch Glasses to cover evaporating dishes.6.3 Desiccator,equipped with drying agent and tray.6.4 Analytical Balance,sensitive to 1 mg.6.5 Steam Bath.6.6 Drying Oven,with temperature control for maintainingtemperature at 100 to 105C(212 to 221F).6.7 Electric Hotplate.6.8 Muffle Furnace,for igniting crucibles containing testspecimens.Capable of maintaining desired temperature regu-lation(6006 25C(1112 6 45F).7.Reagents7.1 Nitric Acid(HNO3),concentrated,sp gr 1.42.8.Test Specimens8.1 For each test,use 5 to 6 g of material.1These test methods are under the jurisdiction of ASTM Committee D14 onAdhesives and are the direct responsibility of Subcommittee D14.10 on WorkingProperties.Current edition approved April 1,2011.Published April 2011.Originallyapproved in 1990.Last previous edition approved in 2005 as D5040 90(2005).DOI:10.1520/D5040-90R11.2For 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.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 8.2 The specimen being tested should represent the entirelot of material.Two specimens shall be taken for testing fromeach sample unit.9.Procedure9.1 Test Method APlace a 5.0 6 0.5-g test specimen in anignited and tared crucible and evaporate to dryness on a steambath.Cool in a desiccator and weigh accurately.Heat thecrucible and its contents in a muffle furnace,gradually heatingthe furnace until the temperature reaches 600 6 25C(1112 645F).With the ignition temperature kept at 600C(1112F),allow the specimen to remain in the muffle furnace for 8 h oruntil constant weight is reached.Check weight by cooling indesiccator and weighing to constant weight.9.2 Test Method B:9.2.1 Place 5.0 6 0.5 g test specimen in a tared and igniteddish and evaporate to dryness on a steam bath.NOTE1It is necessary to evaporate all volatile solvent to avoid firehazard when subjecting material to subsequent drying operation.9.2.2 Dry the test specimen in the oven at 100 to 105C(212to 221F)for 5 h,cool in the desiccator,then reweigh to thenearest mg.Add 25 mL nitric acid to the dried material in theevaporating dish,cover with a watch glass to prevent loss bys