ASTM_D_3465_-_14.pdf

Designation:D346514Standard Test Method forPurity of Monomeric Plasticizers by Gas Chromatography1This standard is issued under the fixed designation D3465;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.1.Scope*1.1 This gas chromatographic test method covers a proce-dure for extending the range of purity determination ofmonomeric plasticizers beyond that now determined by othermethods.Due to the need to volatilize the plasticizer,onlymonomeric plasticizers having definitive boiling points and amolecular weight less than 1000 Daltons,such as dioctylphthalate,are applicable to this test method.1.2 The values in SI units are to be regarded as standard.1.3 The text of this test method references notes andfootnotes that provide explanatory material.These notes andfootnotes(excluding those in tables and figures)are not to beconsidered as requirements of this test method.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.Specific precau-tionary statements are given in Section 9NOTE1There is no known ISO equivalent to this standard.2.Referenced Documents2.1 ASTM Standards:2D883 Terminology Relating to PlasticsD1600 Terminology forAbbreviated Terms Relating to Plas-ticsD2124 Test Method for Analysis of Components in Poly(Vi-nyl Chloride)Compounds Using an Infrared Spectropho-tometric TechniqueE177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE260 Practice for Packed Column Gas ChromatographyE355 Practice for Gas Chromatography Terms and Relation-shipsE594 Practice for Testing Flame Ionization Detectors Usedin Gas or Supercritical Fluid ChromatographyE1510 Practice for Installing Fused Silica Open TubularCapillary Columns in Gas ChromatographsIEEE/ASTM SI-10 Practice for Use of the InternationalSystem of Units(SI),the Modernized Metric System3.Terminology3.1 Definitions:3.1.1 GeneralDefinitions are in accordance with Termi-nology D883 and Terminology D1600 unless otherwise indi-cated.3.1.2 All gas chromatography terms and relationships usedin this test method are consistent with,or refer to,PracticeE355.4.Summary of Test Method4.1 Atest portion of the plasticizer to be analyzed is injectedonto a gas chromatographic column and separated into itscomponents,which are sensed by the detector and quantifiedby an electronic data acquisition system(computer)or anintegrator.The purity is based on the total area response of theprincipal peak(s).All other components are impurities.5.Significance and Use5.1 Infrared techniques frequently cannot detect low-levelmaterials.Gas chromatographic methods possess highersensitivity,and are used to extend limits of detection.5.2 It is expected that this test method will be suitable forspecifications,manufacturing control,and research and devel-opment.An area percent method of determining concentrationof the components shall be used if the area percent of theplasticizer is 99.0%or higher.However,if the area percent ofthe plasticizer is less than 99.0%or if any question were toarise about the data,an internal standard shall be used.5.3 Impurities potentially found in monomeric plasticizersinclude alcohols,dibasic acids,and monoesters.6.Interferences6.1 Gas chromatography(GC)retention times are depen-dent on several variables,and it is possible to have two or more1This test method is under the jurisdiction of ASTM Committee D20 on Plasticsand is the direct responsibility of Subcommittee D20.70 on Analytical Methods(Section D20.70.02).Current edition approved March 1,2014.Published March 2014.Originallyapproved in 1975.Last previous edition approved in 2007 as D3465-00(2007)1.DOI:10.1520/D3465-14.2For 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.*A Summary of Changes section appears at the end of this standardCopyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 components with identical retention times.The analyst shalltake the necessary steps to ensure that adequate separation ofthe plasticizer components is achieved.It is possible thatanalysis by gas chromatography/mass spectrometry will iden-tify the presence of overlapping components.7.Apparatus7.1 Gas Chromatograph,equipped with a flame ionizationor thermal conductivity detector and capable of operating in therange from 250 to 350C.7.1.1 Capillary or Packed Gas Chromatographic Column,capable of operating in the