1、Designation: D 3271 87 (Reapproved 2006)Standard Practice forDirect Injection of Solvent-Reducible Paints Into a GasChromatograph for Solvent Analysis1This standard is issued under the fixed designation D 3271; the number immediately following the designation indicates the year oforiginal adoption o
2、r, 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.This standard has been approved for use by agencies of the Department of Defense.1. Scope
3、1.1 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 ass
4、tandard. 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 a
5、pplica-bility of regulatory limitations prior to use. A specific hazardstatement is given in 6.1.2. Referenced Documents2.1 ASTM Standards:4E 260 Practice for Packed Column Gas Chromatography3. Summary of Practice3.1 Asuitable aliquot of whole paint is injected, by means ofa syringe, into a gas chro
6、matographic 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 Chromatograp
7、hAny instrument with temperatureprogramming capability may be used. It should be equippedwith either a thermal conductivity or flame ionization detector(see Practice E 260).5.2 RecorderA 1 to 10-mV recorder with a full-scaleresponse time of2sorless and a maximum noise of 60.03 %of full scale.5.3 Col
8、umnThe 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
9、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
10、 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 cop
11、olymer, 60 to 80-mesh (250 to 177-m) have also beensuccessfully used as column material.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 P
12、aint Materials.Current edition approved June 1, 2006. Published June 2006. Originallyapproved in 1973. Last previous edition approved in 2001 as D 3271 87 (2001).2New York Society for Paint Technology, Technical Committee 76, “TheApplication of Gas Chromatography to the Analysis of Coating Solvents,
13、” 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. 11221131.4For refere
14、nced 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, In
15、c.,500 5th Ave., New York, NY 10036.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6.3 Liquid Charging Devices, such as micro syringes. Dis-posable type is preferred.6.4 Septum Sample Vials, PTFE-fluorocarbon-faced.7. Procedure7.1 P
16、rotect 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 s
17、ampleis 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 the syringe. Proceed with no
18、rmaltechniques to obtain a chromatogram of the solvent or solventspresent in the sample.NOTE 1Consult manufacturer of particular instrument used.NOTE 2Ethyl ether and methylene chloride have been found satisfac-tory for most sample types.8. Keywords8.1 chromotography, direct injection techniques; ch
19、romo-tography, gas; chromotography, solvent compositionASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent
20、rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either
21、for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hear
22、ing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).D 3271 87 (2006)2
