1、Designation: D7083 04 (Reapproved 2010)1Standard Practice forDetermination of Monomeric Plasticizers in Poly (VinylChloride) (PVC) by Gas Chromatography1This standard is issued under the fixed designation D7083; the number immediately following the designation indicates the year oforiginal adoption
2、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.1NOTEReapproved with editorial changes in July 2010.1. Scope*1.1 This practice provides f
3、or the separation and identifica-tion of monomeric plasticizers in poly (vinyl chloride) (PVC)compounds by gas chromatography (GC).1.2 The text of this practice references notes and footnoteswhich provide explanatory material. These notes and footnotes(excluding those in Tables and Figures) shall no
4、t be consideredas requirements of this standard.1.3 Test Method D2124 is an alternative infrared procedure.1.4 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.5 This standard does not purport to address all of thesafety concer
5、ns, 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.NOTE 1There is no known ISO equivalent to this standard.2. Referenced Documents2.1 A
6、STM Standards:2D883 Terminology Relating to PlasticsD1600 Terminology for Abbreviated Terms Relating toPlasticsD2124 Test Method for Analysis of Components in Poly-(Vinyl Chloride) Compounds Using an Infrared Spectro-photometric TechniqueD3465 Test Method for Purity of Monomeric Plasticizers byGas C
7、hromatographyE355 Practice for Gas Chromatography Terms and Rela-tionshipsE594 Practice for Testing Flame Ionization Detectors Usedin Gas or Supercritical Fluid ChromatographyIEEE/ASTM SI-10 Practice for Use of the InternationalSystem of Units (SI), the Modernized Metric System3. Terminology3.1 Defi
8、nitions:3.1.1 For definition of plastic terms used in this standard,see Terminologies D883 and D1600.3.2 For units, symbols, and abbreviations used in thisstandard refer to Practices E594, E355,orIEEE/ASTM SI-10.3.3 Abbreviations:3.3.1 DOABis (2-ethylhexyl) adipate3.3.2 DBPDibutyl phthalate3.3.3 DOP
9、Bis (2-ethylhexyl) phthalate3.3.4 FTIRFourier Transform Infrared Spectroscopy3.3.5 GCGas Chromatography3.3.6 GC/MSGas Chromatography/Mass Spectrometry3.3.7 GPCGel Permeation Chromatography3.3.8 HPLCHigh Performance Liquid Chromatography3.3.9 PVCPoly (Vinyl Chloride)3.3.10 TCPTricresyl phosphate3.3.1
10、1 TOPTris (2-ethylhexyl) phosphate3.3.12 TOTMTrioctyl trimellitate4. Summary of Test Method4.1 A PVC sample is extracted in accordance with TestMethod D2124 and the extract residue is re-dissolved in asolvent. The resulting solution is then analyzed by GC todetermine the identity of each plasticizer
11、 component. Theplasticizer components are identified by retention time, orchromatographic fingerprint, or both.5. Significance and Use5.1 Separation and identification of plasticizer componentsin PVC is necessary to correlate performance properties withpolymer composition. This test method provides
12、a means of1This test method is under the jurisdiction of ASTM Committee D20 on Plasticsand is the direct responsibility of Subcommittee D20.70 on Analytical Methods.Current edition approved July 1, 2010. Published October 2010. Originallyapproved in 2004. Last previous edition approved in 2004 as D7
13、083 - 04. DOI:10.1520/D7083-04R10E01.2For 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.1*A Summary of Changes s
14、ection appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.determining monomeric plasticizers including adipates, aze-lates, benzoates, citrates, phthalates, sebacates, and trimelli-tates.5.2 Other meth
15、ods successfully used to analyze plasticizersare column chromatography, HPLC, GPC, FTIR, and GC/MS.5.3 This method is not applicable to plasticizers withmolecular weights over 700 g/mol including epoxidized soy-bean oil and polymeric plasticizers.6. Interferences6.1 Retention times for GC are depend
16、ent on several vari-ables and it is quite possible to have two or more componentswith identical retention times. The GC operator should take thenecessary steps to insure that adequate separation of theplasticizer components is achieved.6.2 A source of interference can be from solvent impurities.Run
17、a solvent blank prior to analysis of an extract.7. Apparatus7.1 Gas chromatograph equipped with a flame ionizationdetector and capable of operating in the 250 to 350C range.7.2 A capillary or packed gas chromatographic columncapable of operating in the 250 to 350C range such as a30-metre 100 % poly
18、(dimethylsiloxane) phase fused silicaopen tubular capillary column; 0.32 mm ID with a 0.25 m filmthickness, or a stainless steel packed column; 1.83 m long withan outside diameter of 6.4 mm, and filled with Chromosorb Wor WAW, 60 to 80 mesh, as the solid support and coated witha liquid phase as reco
19、mmended in Practice D3465.7.3 Integrator or data handling system, capable of measur-ing the net peak area.7.4 Gas chromatographic syringe or autosampler, 0.1-10.0-mL capacity.7.5 Analytical balance, capable of weighing to + 0.001 g.7.6 Pressure regulators, for all required gas cylinders.7.7 Flowmete
20、r, or other means of measuring gas flow rates.8. Reagents and Materials8.1 Carrier gas Helium, chromatographic grade or Nitrogen,chromatographic grade.8.2 Hydrogen, chromatographic grade8.3 Air, chromatographic grade8.4 Dichloromethane, or a solvent suitable for re-dissolvingthe extract from Test Me
21、thod D2124, spectral quality orchromatographic grade. The same solvent is used for standardpreparation and dissolution of the extract from Test MethodD2124, subsection 8.2.8.5 Standards of appropriate monomeric plasticizers for usein constructing an external calibration curve.NOTE 2Should the sample
22、 contain unknown plasticizers, it is recom-mended that GC/MS, FTIR or another suitable technique be used toidentify the plasticizers.9. Safety and Precautions9.1 Hydrogen is flammableensure all leaks are eliminated.10. Sample Preparation10.1 Refer to the extraction procedure in Test MethodD2124, sub
23、section 8.2.11. Preparation of the Gas Chromatograph11.1 Example Conditions:The following conditions were used to obtain the examplechromatogram shown in Fig. 1.NOTE 3Other columns, detectors, or chromatographic conditions, or acombination of the three, can be used to accomplish the same or a simila
24、rseparation. If different plasticizers (than those in Fig. 1) are present in thesample extract, these conditions are allowed to be modified for adequateseparation (see 14.2).11.1.1 Chromatographic Column:30-m by 0.32-mm fused silica open tubular capillary columnwith a 100 % poly (dimethylsiloxane) s
25、tationary phase, filmthickness 0.25 mm.11.1.2 Carrier Gas:Helium, flow rate 1.9 mL/min (40 cm/sec).11.1.3 Injection Port:Split injection, 350C, split ratio 50 + 1.11.1.4 Detector:Flame Ionization, 350C11.1.5 Temperature Program:Initial oven temperature 200C hold for one minute, ramp to320C at 10C/mi
26、n. Hold for three minutes.11.1.6 Sample Size:1.0-mL of the re-dissolved extract. It is possible to analyzethe extract neat. When the sample is analyzed neat, the samplesize shall be small enough to maintain adequate chromato-graphic efficiency (that is, do not overload the column).12. Procedure12.1
27、Gas Chromatographic Separation12.1.1 Ensure that the gas chromatograph is set to provideresolution (R) of at least 1.5 for all plasticizers analyzed usingthis method. The resolution calculation is based on:R 5 TR,2 TR,1! / 0.5W1 W2! (1)where TR,2and TR,1are the retention times of the adjacentpeaks a
28、nd W1and W2are the peak widths at the base of the twopeaks.12.1.2 Re-dissolve the extract residue from Test MethodD2124, subsection 8.2 in 5-mL dichloromethane. Inject 1.0 mLof this extract into the gas chromatograph. It is possible toinject the extract neat. When the sample is injected neat, thesam
29、ple size should be small enough to maintain adequatechromatographic efficiency (that is, do not overload the col-umn).12.1.3 Run the separation for the length of time necessary toelute all components.12.1.4 Record the chromatogram and measure the peak areaof the components of interest using a comput
30、er or an integrator.D7083 04 (2010)1213. Identification13.1 This test method relies on peak retention times, orchromatographic fingerprint, or both (see Fig. 1) to identify theextracted plasticizer components.13.2 Match the retention times, or chromatographic finger-print, or both from the chromatog
31、ram of the extract from TestMethod D2124 to chromatograms of standard plasticizer solu-tions to identify the plasticizers in the sample extract.14. Report14.1 Column description.14.2 Temperature program.14.3 Plasticizer(s) identified.15. Keywords15.1 gas chromatography; plasticizers; Poly (Vinyl Chl
32、o-ride); PVCFIG. 1 Chromatogram ExampleD7083 04 (2010)13SUMMARY OF CHANGESCommittee D20 has identified the location of selected changes to this standard since the last issue (D7083 - 04)that may impact the use of this standard. (July 1, 2010)(1) Updated ISO equivalency statement.(2) Removed permissi
33、ve language.(3) Added Summary of Changes section.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 patent rights
34、, 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 for re
35、vision 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 hearing yo
36、u 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). Permission rights to photocopy the standard may also be secured from the ASTM website (www.astm.org/COPYRIGHT/).D7083 04 (2010)14
