1、Designation: D 7083 04Standard Practice forDetermination of Monomeric Plasticizers in Poly (VinylChloride) (PVC) by Gas Chromatography1This standard is issued under the fixed designation D 7083; the number immediately following the designation indicates the year oforiginal adoption or, in the case o
2、f 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.1. Scope1.1 This practice provides for the separation and identifica-tion of monomeric plasticizers in po
3、ly (vinyl chloride) (PVC)compounds by gas chromatography (GC).1.2 The values in SI units are to be regarded as standard.1.3 The text of this practice references notes and footnoteswhich provide explanatory material. These notes and footnotes(excluding those in Tables and Figures) shall not be consid
4、eredas requirements of this standard.1.4 Test Method D 2124 is an alternative infrared proce-dure.1.5 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
5、 practices and determine the applica-bility of regulatory limitations prior to use.NOTE 1There is no ISO equivalent for this standard.2. Referenced Documents2.1 ASTM Standards:2D 883 Terminology Relating to PlasticsD 1600 Terminology for Abbreviated Terms Relating toPlasticsD 2124 Test Method for An
6、alysis of Components in Poly(Vinyl Chloride) Compounds Using an Infrared Spectro-photometric TechniqueD 3465 Practice for Purity of Monomeric Plasticizers byGas ChromatographyE 355 Practice for Gas Chromatography Terms and Rela-tionshipsE 594 Practice for Testing Flame Ionization Detectors inGas or
7、Supercritical Fluid ChromatographyIEEE/ASTM SI-10 Practice for Use of the InternationalSystem of Units (SI), the Modernized Metric System3. Terminology3.1 Definitions:3.1.1 For definition of plastic terms used in this standard,see Terminologies D 883 and D 1600.3.2 For units, symbols, and abbreviati
8、ons used in thisstandard refer to Practices E 594, E 355,orIEEE/ASTM SI-10.3.3 Abbreviations:3.3.1 DOABis (2-ethylhexyl) adipate3.3.2 DBPDibutyl phthalate3.3.3 DOPBis (2-ethylhexyl) phthalate3.3.4 FTIRFourier Transform Infrared Spectroscopy3.3.5 GCGas Chromatography3.3.6 GC/MSGas Chromatography/Mass
9、 Spectrometry3.3.7 GPCGel Permeation Chromatography3.3.8 HPLCHigh Performance Liquid Chromatography3.3.9 PVCPoly (Vinyl Chloride)3.3.10 TCPTricresyl phosphate3.3.11 TOPTris (2-ethylhexyl) phosphate3.3.12 TOTMTrioctyl trimellitate4. Summary of Test Method4.1 A PVC sample is extracted in accordance wi
10、th TestMethod D 2124 and the extract residue is re-dissolved in asolvent. The resulting solution is then analyzed by GC todetermine the identity of each plasticizer component. Theplasticizer components are identified by retention time, orchromatographic fingerprint, or both.5. Significance and Use5.
11、1 Separation and identification of plasticizer componentsin PVC is necessary to correlate performance properties withpolymer composition. This test method provides a means ofdetermining monomeric plasticizers including adipates, aze-lates, benzoates, citrates, phthalates, sebacates, and trimelli-tat
12、es.5.2 Other methods successfully used to analyze plasticizersare column chromatography, HPLC, GPC, FTIR, and GC/MS.1This 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 Octo
13、ber 1, 2004. Published October 2004.2For 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.1Copyright ASTM Internati
14、onal, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.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 dependent on se
15、veral 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 a solvent
16、 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 a 30meter 100 % poly (dimethyl
17、siloxane) phase fused silica opentubular capillary column; 0.32 mm ID with a 0.25 mm 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 recommended
18、in Practice D 3465.7.3 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 Flowmeter, or o
19、ther 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 Method D
20、2124, spectral quality orchromatographic grade. The same solvent is used for standardpreparation and dissolution of the extract from Test MethodD 2124, subsection 8.2.8.5 Standards of appropriate monomeric plasticizers for usein constructing an external calibration curve.NOTE 2Should the sample cont
21、ain 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 MethodD 2124, subsect
22、ion 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 similarsep
23、aration. If different plasticizers (than those in Fig. 1) are present in thesample extract, these conditions may need to be modified for adequateseparation (see 14.2).11.1.1 Chromatographic Column:30 m 3 0.32 mm fused silica open tubular capillary columnwith a 100 % poly (dimethylsiloxane) stationar
24、y 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/min. Hold
25、for three minutes.11.1.6 Sample Size:1.0-mL of the re-dissolved extract. The extract may also beanalyzed neat. When the sample is analyzed neat, the samplesize should be small enough to maintain adequate chromato-graphic efficiency (that is, do not overload the column).12. Procedure12.1 Gas Chromato
26、graphic 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 and W1and W2a
27、re the peak widths at the base of the twopeaks.12.1.2 Re-dissolve the extract residue from Test MethodD 2124, subsection 8.2 in 5-mL dichloromethane. Inject 1.0mL of this extract into the gas chromatograph. It may not benecessary or desirable to re-dissolve the extract from TestMethod D 2124. The ex
28、tract may also be injected neat. Whenthe sample is injected neat, the sample size should be smallenough to maintain adequate chromatographic efficiency (thatis, do not overload the column).12.1.3 Run the separation for the length of time necessary toelute all components.12.1.4 Record the chromatogra
29、m and measure the peak areaof the components of interest using a computer or an integrator.D708304213. 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 time
30、s, or chromatographic finger-print, or both from the chromatogram of the extract from TestMethod D 2124 to chromatograms of standard plasticizersolutions to identify the plasticizers in the sample extract.14. Report14.1 Column description.14.2 Temperature program.14.3 Plasticizer(s) identified.15. K
31、eywords15.1 gas chromatography; plasticizers; Poly (Vinyl Chlo-ride); PVCASTM 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 o
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34、ceived a fair 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).FIG. 1 Chromatogram ExampleD7083043
