1、Designation: D7083 04 (Reapproved 2010)1D7083 16Standard 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 a
2、doption 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 NOTEReapproved with editorial changes in July 2010.1. Scope*1.1 This practice p
3、rovides for the separation and identification of monomeric plasticizers in poly (vinyl chloride) (PVC)compounds by gas chromatography (GC).1.2 The text of this practice references notes and footnotes which provide explanatory material. These notes and footnotes(excluding those in Tables and Figures)
4、 shall not be considered as 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 as standard. No other units of measurement are included in this standard.1.5 This standard does not purport to address all of the
5、safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use.NOTE 1There is no known ISO equivalent to this standard.2. Referenced Docu
6、ments2.1 ASTM Standards:2D883 Terminology Relating to PlasticsD1600 Terminology for Abbreviated Terms Relating to PlasticsD2124 Test Method for Analysis of Components in Poly(Vinyl Chloride) Compounds Using an Infrared SpectrophotometricTechniqueD3465 Test Method for Purity of Monomeric Plasticizers
7、 by Gas ChromatographyD7823 Test Method for Determination of Low Level, Regulated Phthalates in Poly (Vinyl Chloride) Plastics by ThermalDesorptionGas Chromatography/Mass SpectrometryE355 Practice for Gas Chromatography Terms and RelationshipsE594 Practice for Testing Flame Ionization Detectors Used
8、 in Gas or Supercritical Fluid ChromatographyIEEE/ASTM SI-10 Practice for Use of the International System of Units (SI), the Modernized Metric System3. Terminology3.1 Definitions:3.1.1 For definition of plastic terms used in this standard, see Terminologies D883 and D1600.3.2 For units, symbols, and
9、 abbreviations used in this standard refer to Practices E594, E355, or IEEE/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 Spectroscopy1 This test method is under the jurisdiction of
10、ASTM Committee D20 on Plastics and is the direct responsibility of Subcommittee D20.70 on Analytical Methods.Current edition approved July 1, 2010May 1, 2016. Published October 2010May 2016. Originally approved in 2004. Last previous edition approved in 20042010 asD7083 - 04.D7083 - 04(2010)1. DOI:
11、10.1520/D7083-04R10E01.10.1520/D7083-16.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not
12、an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate.
13、 In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*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 States13.3.
14、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 phosphate3.3.11 TOPTris (2-ethylhexyl) phosphate3.3.12 TOTMTrioctyl trimellitate4. Summary of T
15、est Method4.1 A PVC sample is extracted in accordance with Test Method D2124 and the extract residue is re-dissolved in a solvent. Theresulting solution is then analyzed by GC to determine the identity of each plasticizer component. The plasticizer components areidentified by retention time, or chro
16、matographic fingerprint, or both.5. Significance and Use5.1 Separation and identification of plasticizer components in PVC is necessary to correlate performance properties withpolymer composition. This test method provides a means of determining monomeric plasticizers including adipates, azelates,be
17、nzoates, citrates, phthalates, sebacates, and trimellitates.5.2 Other methods successfully used to analyze plasticizers are column chromatography, HPLC, GPC, FTIR, and GC/MS.5.3 This method is not applicable to plasticizers with molecular weights over 700 g/mol including epoxidized soybean oil andpo
18、lymeric plasticizers.6. Interferences6.1 Retention times for GC are dependent on several variables and it is quite possible to have two or more components withidentical retention times. The GC operator shouldshall take the necessary steps to insure that adequate separation of the plasticizercomponen
19、ts is achieved.6.2 A source of interference can be from solvent impurities. Run a solvent blank prior to analysis of an extract.7. Apparatus7.1 Gas chromatograph equipped with a flame ionization detector and capable of operating in the 250 to 350C range.7.2 A capillary or packed gas chromatographic
20、column capable of operating in the 250 to 350C range such as a 30-metre 100% poly (dimethylsiloxane) phase fused silica open tubular capillary column; 0.32 mm ID with a 0.25 m film thickness, or astainless steel packed column; 1.83 m long with an outside diameter of 6.4 mm, and filled with Chromosor
21、b W or WAW, 60 to80 mesh, as the solid support and coated with a liquid phase as recommended in Practice D3465.7.3 Integrator or data handling system, capable of measuring the net peak area.7.4 Gas chromatographic syringe or autosampler, 0.1- 10.0-mL10.0-L capacity.7.5 Analytical balance, capable of
22、 weighing to + 0.001 g.7.6 Pressure regulators, for all required gas cylinders.7.7 Flowmeter, 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, chromatograph
23、ic grade8.4 Dichloromethane, or a solvent suitable for re-dissolving the extract from Test Method D2124, spectral quality orchromatographic grade. The same solvent is used for standard preparation and dissolution of the extract from Test Method D2124,subsection 8.2.8.5 Standards of appropriate monom
24、eric plasticizers for use in constructing an external calibration curve.NOTE 2Should the sample contain unknown plasticizers, it is recommended that GC/MS, FTIR or another suitable technique be used to identify theplasticizers.9. Safety and Precautions9.1 Hydrogen is flammableensure all leaks are el
25、iminated.D7083 16210. Sample Preparation10.1 Refer to the extraction procedure in Test Method D2124, subsection 8.2.11. Preparation of the Gas Chromatograph11.1 Example Conditions: The following conditions were used to obtain the example chromatogramchromatograms shown inFig. 1.NOTE 3Other columns,
26、detectors, or chromatographic conditions, or a combination of the three, can be used to accomplish the same or a similarseparation. If different plasticizers (than those in Fig. 1) are present in the sample extract, these conditions are allowed to be modified for adequateseparation (see 14.2).11.1.1
27、 Chromatographic Column: 30-m by 0.32-mm fused silica open tubular capillary column with a 100 % poly(dimethylsiloxane) stationary phase, film thickness 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 Detect
28、or: Flame Ionization, 350C11.1.5 Temperature Program: Initial oven temperature 200C hold for one minute, ramp to 320C at 10C/min. Hold for threeminutes.11.1.6 Sample Size: 1.0-mL of the re-dissolved extract. It is possible to analyze the extract neat. When the sample is analyzedneat, the sample size
29、 shall be small enough to maintain adequate chromatographic efficiency (that is, do not overload the column).12. Procedure12.1 Gas Chromatographic SeparationFIG. 1 Chromatogram ExampleD7083 16312.1.1 Ensure that the gas chromatograph is set to provide resolution (R) of at least 1.5 for all plasticiz
30、ers analyzed using thismethod. The resolution calculation is based on:R 5TR,22TR,1!/0.5W12W2! (1)where TR,2 and TR,1 are the retention times of the adjacent peaks and W1 and W2 are the peak widths at the base of the twopeaks.12.1.2 Re-dissolve the extract residue from Test Method D2124, subsection 8
31、.2 in 5-mL dichloromethane. Inject 1.0 mLL ofthis extract into the gas chromatograph. It is possible to inject the extract neat. When the sample is injected neat, the sample sizeshouldshall be small enough to maintain adequate chromatographic efficiency (that is, do not overload the column).12.1.3 R
32、un the separation for the length of time necessary to elute all components.12.1.4 Record the chromatogram and measure the peak area of the components of interest using a computer or an integrator.D7083 16413. Identification13.1 This test method relies on peak retention times, or chromatographic fing
33、erprint, or both (see Fig. 1) to identify the extractedplasticizer components.13.2 Match the retention times, or chromatographic fingerprint, or both from the chromatogram of the extract from Test MethodD2124 to chromatograms of standard plasticizer solutions to identify the plasticizers in the samp
34、le extract.14. Report14.1 Column description.14.2 Temperature program.14.3 Plasticizer(s) identified.15. Keywords15.1 gas chromatography; monomeric; phthalate; plasticizers; Poly (Vinyl Chloride); PVCSUMMARY OF CHANGESCommittee D20 has identified the location of selected changes to this standard sin
35、ce the last issue(D7083 - 04(2010)1) that may impact the use of this standard. (July(May 1, 2010)2016)(1) Updated ISO equivalency statement.Added Test Method D7823 to Section 2.(2) Removed permissive language.(3) Added Summary of Changes section.and “s” to chromatogram in 11.1.(4) Corrected “mL” to
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