1、Designation: D 3465 00 (Reapproved 2007)e1Standard Test Method forPurity of Monomeric Plasticizers by Gas Chromatography1This standard is issued under the fixed designation D 3465; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, th
2、e 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.1. Scope*1.1 This gas chromatographic test method covers a proce-dure for extending the range of purity determination o
3、fmonomeric 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
4、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
5、 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 Sec
6、tion 9NOTE 1There is no known ISO equivalent for this test method.2. Referenced Documents2.1 ASTM Standards:2D 883 Terminology Relating to PlasticsD 1600 Terminology for Abbreviated Terms Relating toPlasticsD 2124 Test Method for Analysis of Components in Poly-(Vinyl Chloride) Compounds Using an Inf
7、rared Spectro-photometric TechniqueE 177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE 260 Practice for Packed Column Gas ChromatographyE 355 Practice for Gas Chromatography Terms and Rela-tionshipsE 594 Practice for Testing Flame Ionization Detectors Usedin Gas or Supercriti
8、cal Fluid ChromatographyE 1510 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
9、Termi-nology D 883 and Terminology D 1600 unless otherwise indi-cated.3.1.2 All gas chromatography terms and relationships usedin this test method are consistent with, or refer to, PracticeE 355.4. Summary of Test Method4.1 Atest portion of the plasticizer to be analyzed is injectedonto a gas chroma
10、tographic 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.
11、1 Infrared techniques frequently cannot detect low-levelmaterials. Gas chromatographic methods possess higher sensi-tivity, and are used to extend (FL) limits of detection.5.2 It is expected that this test method will be suitable forspecifications, manufacturing control, and research and devel-opmen
12、t. 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 should any question ariseabout the data, an internal standard shall be used.5.3 Impur
13、ities that may be 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 morecomponents with identical retention times. The GC operatorshould tak
14、e the necessary steps to insure that adequate sepa-ration of the plasticizer components is achieved. Analysis by1This test method is under the jurisdiction of ASTM Committee D20 on Plasticsand is the direct responsibility of Subcommittee D20.70 on Analytical Methods(Section D20.70.03).Current editio
15、n approved Nov. 1, 2007. Published November 2007. Originallyapproved in 1975. Last previous edition approved in 2000 as D3465 - 00.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume informa
16、tion, refer to the standards Document Summary page onthe ASTM website.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.gas chromatography/mass spectrometry may identify
17、 the pres-ence 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 range from 250 to 350C t
18、hatprovides adequate separation and definition of components.Examples are as follows:7.1.2 Packed Columns, stainless steel, 1.83 m (6 ft) long,with an outside diameter of 6.4 mm (14 in.) and filled withChromosorb W or WAW,360 to 80 mesh, as the solid support.7.1.2.1 Liquid PhaseThe liquid phase sens
19、itivity changesthe utility in detecting various impurities. Examples of detect-ability of alcohol impurities are illustrated as follows:7.1.2.2 A coating of 5 to 15 % of SE-304silicone gumstockresults in reasonably symmetrical peaks and accurate quanti-tative measurements between 0.1 and 1 % alcohol
20、ic impurities.7.1.2.3 A coating of 15 % Igepal CO-9905results in sepa-rations of similar types of esters such as diisooctyl phthalateand di (2-ethylhexyl) phthalate at the 1 % level.7.1.2.4 A coating of 20 % Ozonite6is also effective foralcohols in the 0.1 to 1 % concentration level.7.1.3 Capillary
21、Columns, fused silica high-temperature cap-illary column with a 100 % poly(dimethylsiloxane) stationaryphase; length: 15 to 30 m; inside diameter: 0.25 to 0.5 mm; filmthickness: 0.1 to 0.25 m.7.2 Integrator or Electronic Data Acquisition System.7.3 Gas Chromatographic Syringe or Autosampler, 0.1 to1
22、0.0 L capacity.7.4 Pressure Regulators, for all required gas cylinders.7.5 Flowmeter, or other means of measuring gas flow rates.8. Reagents and Materials8.1 Helium, chromatographic grade.8.2 Hydrogen, chromatographic grade.8.3 Nitrogen, chromatographic grade.8.4 Purified Air.9. Hazards9.1 Hydrogen
23、is flammable. Ensure that all leaks are elimi-nated.10. Preparation of the Gas Chromatograph10.1 Temperature SettingsThis test method requires injec-tion port and detector temperatures of 260 to 350C. For aplasticizer with a nominal boiling point of 410C, the follow-ing conditions are suggested:Inje
24、ction port 260 to 350CDetector 300 to 350C10.2 Program the temperature of the column suitable to bestseparate the components (see 7.1 for columns). Typical settingsare as follows:10C/min from 60 to 280C and hold.10C/min from 100 to 300C and hold for 10 min.10.3 Sample SizeSelect a sample size that p
25、rovides anadequate chromatographic efficiency (that is, do not overloadthe column). Typical quantity is 1 L.10.4 Carrier GasHelium, flow rate 30 to 60 cm3/min.11. Procedure11.1 The method of injecting the sample onto the columnand analyzing for the components is given in detail in PracticeE 260, (sp
26、ecifically, Sections 10 and 14).11.2 The method for analyzing the components shall beconsistent with Fig. 1 of Practice E 355.12. Report12.1 Report the following information:12.1.1 Proportion of the total area related to the principalcomponent(s) as the purity of the plasticizer, percent,12.1.2 Rete
27、ntion times of impurities, relating them to cor-responding retention times of known substances,12.1.3 Proportion of total area related to the impurities inpercent,12.1.4 Column description,12.1.5 Gas chromatograph conditions, and12.1.6 Internal standard when used for calibration.13. Precision and Bi
28、as13.1 PrecisionA round robin is in progress. Table 1 isbased on a single laboratory test using two different capillarycolumns on one gas chromatograph.13.1.1 Sris the within-laboratory standard deviation of theaverage; r = 2.8 SR(see 13.1.3 for application of r.)13.1.2 SRis the between-laboratory s
29、tandard deviation ofthe average; R = 2.8 SR(see 13.1.4 for application of R).13.1.3 RepeatabilityIn comparing two test results for thesame material, obtained by the same operator using the sameequipment on the same day, those test results should be judgednot equivalent if they differ by more than th
30、e r value for thematerial and condition.13.1.4 ReproducibilityBy comparing two test results forthe same material, obtained by different equipment on differentdays, those test results should be judged not equivalent if theydiffer by more than the R value for the material and condition.(This applies b
31、etween different laboratories or between differ-ent equipment within the same laboratory.)13.1.5 Any judgment in accordance with 13.1.2 and 13.1.3will have an approximate 95 % (0.95) probability of beingcorrect.3Trademark of Johns-Manville Products Corp.4Trademark of General Electric Co., Schenectad
32、y, NY.5Trademark of General Aniline plasticizers; poly(vinyl chloride);PVCSUMMARY OF CHANGESCommittee D20 has identified the location of selected changes to this standard since the last issue (D3465 - 00)that may impact the use of this standard. (November 1, 2007)(1) Changed Note 1 to read “There is
33、 no known ISO equiva-lent”(2) Corrected spelling error in 6.1.ASTM 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
34、patent 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
35、either 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 fa
36、ir hearing 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 3465 00 (2007)e13
