ASTM_D_3271_-_87_2012.pdf

Designation:D327187(Reapproved 2012)Standard Practice forDirect Injection of Solvent-Reducible Paints Into a GasChromatograph for Solvent Analysis1This standard is issued under the fixed designation D3271;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 This practice describes the techniques used to injectwhole paint samples directly into a gas chromatograph toobtain a chromatogram from which the solvent compositionmay be established.2,31.2 This practice is not designed to be quantitative.1.3 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.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.A specific hazardstatement is given in 6.1.2.Referenced Documents2.1 ASTM Standards:4E260 Practice for Packed Column Gas Chromatography3.Summary of Practice3.1 Asuitable aliquot of whole paint is injected,by means ofa syringe,into a gas chromatographic column in order toseparate the solvents.4.Significance and Use4.1 Gas chromatographic separation of solvents present inwhole paints is the preferred first step for identifying andquantitating solvent compositions,using auxiliary proceduresand techniques.5.Apparatus5.1 Gas ChromatographAny instrument with temperatureprogramming capability may be used.It should be equippedwith either a thermal conductivity or flame ionization detector(see Practice E260).5.2 RecorderA 1 to 10-mV recorder with a full-scaleresponse time of 2 s or less and a maximum noise of 60.03%of full scale.5.3 ColumnThe resolution of the column must be suchthat under the operating conditions selected the distance fromthe base line to the depression between two adjacent peaksmust be not more than 50%of the smaller peak.Columns maybe either packed or capillary.6.Reagents and Materials6.1 Carrier GasHelium or hydrogen for use with thermalconductivity detector units;and nitrogen,helium or argon foruse with flame ionization detector units.6.1.1 Warning:When hydrogen is used,special precautionsshould be taken to prevent gas leakage from causing a possibleexplosion.56.2 Column Packing Material,meeting requirements in 5.3.The following materials have been used satisfactorily:6.2.1 Polyethylene glycol,molecular weight 20 000,anddiisodecyl phthalate as liquid phases on a solid support of 60 to80 mesh(250 to 175 m)diatomaceous earth.6.2.2 Porous beads of ethylvinylbenzene and divinylben-zene copolymer,60 to 80-mesh(250 to 177-m)have also beensuccessfully used as column material.6.3 Liquid Charging Devices,such as micro syringes.Dis-posable type is preferred.1This practice is under the jurisdiction of ASTM Committee D01 on Paint andRelated Coatings,Materials,and Applications and is the direct responsibility ofSubcommittee D01.21 on Chemical Analysis of Paints and Paint Materials.Current edition approved June 1,2012.Published July 2012.Originally approvedin 1973.Last previous edition approved in 2006 as D3271 87(2006).DOI:10.1520/D3271-87R12.2New York Society for Paint Technology,Technical Committee 76,“TheApplication of Gas Chromatography to the Analysis of Coating Solvents,”Journalof Paint Technology,Vol 40,No.516,January 1968,pp.3348.3Esposito,G.G.,and Swann,M.H.,“Direct Analysis of Solvents in Lacquer byProgrammed Temperature Gas Chromatography,”Offcial Digest Federation SocietyPaint Technology,Vol 33,No.440,September 1961,pp.1122 1131.4For 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.5Consult Pamphlet G-5,available from the Compressed Gas Association,Inc.,500 5th Ave.,New York,NY 10036.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 6.4 Septum Sample Vials,PTFE-fluorocarbon-faced.7.Procedure7.1 Protect the injection port from the nonvolatile portion ofthe paint by using a borosilicate glass injection port sleeve(Note 1),glass wool plug,or by any other suitable means.If thewhole paint sample is of sufficiently low viscosity,draw analiquot directly into the syringe.When the whole paint sampleis too viscous,dilute with a suitable solvent(Note 2)that willnot interfere with the analysis.In order to minimize solventlosses due to evaporation,the whole paint sample should beplaced in a PTFE-fluorocarbon-faced septum sample bottleprior to being drawn into th