ASTM_D_2764_-_99_2015e1.pdf

Designation:D276499(Reapproved 2015)1Standard Test Method forDimethylformamide-Insoluble(DMF-I)Content of Tar andPitch1This standard is issued under the fixed designation D2764;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.1NOTESI units formatting was corrected editorially in May 2015.1.Scope1.1 This test method covers the determination of thedimethylformamide-insoluble matter(DMF-I)in tar and pitch.1.2 Since this test method is empirical,strict adherence toall details of the procedure is necessary.1.3 The values stated in inch-pound units are to be regardedas standard.The values given in parentheses are mathematicalconversions to SI units that are provided for information onlyand are not considered standard.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 hazardinformation,see Sections 6 and 7.2.Referenced Documents2.1 ASTM Standards:2D329 Specification for AcetoneD370 Practice for Dehydration of Oil-Type PreservativesD4072 Test Method for Toluene-Insoluble(TI)Content ofTar and PitchD4296 Practice for Sampling PitchE11 Specification for Woven Wire Test Sieve Cloth and TestSieves3.Summary of Test Method3.1 A sample is digested in hot DMF and filtered.Anyinsoluble matter is washed,dried,and weighed.4.Significance and Use4.1 This test method is useful in evaluating and character-izing tars and pitches and as one element in establishing theuniformity of shipments or sources of supply.It is a rapid andreasonably accurate measure of the toluene insoluble(TI)content of tar and pitch Test Method D4072.5.Apparatus5.1 Filtering Crucible,porcelain,with fine-porosity bottom,30 mL to 40 mL capacity,high form,maximum pore diameter7 m.5.2 Filter ApparatusFilter flask and tube with crucibleadapter.5.3 Sieves,U.S.Standard 600 m(No.30)and 250 m(No.60),conforming to Specification E11.5.4 Water Bath,maintained at 203 F to 212 F(95 C to100 C).6.Reagents and Materials6.1 Dimethylformamide,reagent grade,boiling range 4 F(2 C)including 307 F(153 C).Store over a suitable desic-cant.Decant immediately before use.If necessary,filterthrough a plug of glass wool or absorbent cotton until opticallyclear.6.2 Acetone,meeting Specification D329.(WarningFlammable.Health hazard.)6.3 Concentrated Hydrochloric Acid.6.4 Celite Analytical Filter Aid(CAFA)Dry to constantmass at 22 F(105 C)and store in tightly stoppered container.NOTE1Do not use any other grade of filtering medium becauseporosities differ.7.Hazards7.1 Fumes of the solvents should be removed by means ofproper hoods from all working areas.The working area shouldbe kept free of sparks and flames.DMF fumes should not beinhaled,and prolonged contact of DMF with the skin should beavoided.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products,Liquid Fuels,and Lubricants and is the direct responsibility ofSubcommittee D02.05 on Properties of Fuels,Petroleum Coke and Carbon Material.Current edition approved April 1,2015.Published May 2015.Originallyapproved in 1968.Last previous edition approved in 2009 as D2764 99(2009).DOI:10.1520/D2764-99R15E01.2For 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.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 7.2 Observe proper laboratory procedures for handling anddiluting hydrochloric acid.8.Bulk Sampling8.1 Samples from shipments shall be taken in accordancewith Practice D4296 and shall be free of foreign substances.The sample shall be thoroughly mixed immediately beforeremoving a representative portion for the determination or fordehydration.9.Dehydration of Sample9.1 Hard PitchIf the solid bulk sample contains freewater,air-dry a representative portion in a forced draft oven at50 C.9.2 Soft PitchIf the presence of water is indicated bysurface foam on heating,maintain a representative portion ofthe bulk sample at a temperature between 257 F and 302 F(125 C and 150 C)in an open container until the surface isfree of foam.Take care not to overheat,and remove heat sourceimmediately when foam subsides.9.3 TarDehydrate a representative portion of the bulksample in accordance with Test Method D370,but stop thedistillation when the temperature reaches 338 F(170 C).Separate any oil from the water that has distilled over(ifcrystals are present,warm sufficiently to ensure their solution),and thoroughly mi