1、Designation: D3465 14Standard 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 revisio
2、n. 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
3、 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 rega
4、rded 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 thesafe
5、ty 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 9NOTE 1There is no
6、 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 Tec
7、hniqueE177 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 Pra
8、ctice 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
9、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 i
10、tscomponents, 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 cann
11、ot 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 con
12、centrationof 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 pla
13、sticizersinclude 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 responsibilit
14、y 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.as
15、tm.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 Bo
16、x C700, West Conshohocken, PA 19428-2959. United States1components 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
17、 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 range from 250 to 350C th
18、atprovides 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 sensi
19、tivity 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-30 silicone gumstockresults in reasonably symmetrical peaks and accurate quanti-tative measurements between 0.1 and 1 % alcoholi
20、c impurities.7.1.2.3 A coating of 15 % Igepal CO-9904results 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 % Ozonite5is also effective foralcohols in the 0.1 to 1 % concentration level.7.1.3 Capillary C
21、olumns, 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 to10
22、.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 i
23、s 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:Injec
24、tion 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 pr
25、ovides anadequate chromatographic efficiency (that is, do not overloadthe column). A typical sample size 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 PracticeE260,
26、(specifically, Sections 10 and 14).11.2 The method for analyzing the components shall beconsistent with Fig. 1 of Practice E355.12. 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 Re
27、tention 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
28、Bias13.1 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
29、 standard 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, judge those test results as notequivalent if they differ by more than the r va
30、lue for thematerial and condition.13.1.4 ReproducibilityBy comparing two test results forthe same material, obtained by different equipment on differentdays, judge those test results as not equivalent if they differ bymore than the R value for the material and condition. (This3Trademark of Imerys Mi
31、nerals California, Inc.4Trademark of Rhodia Operations.5Trademark of Alltech Associates.TABLE 1 Precision and Bias DataMaterial: Diundecyl PhthalateAveragepurity, %SrSRrR99.79 0.01 0.07 0.03 0.19D3465 142applies between different laboratories or between differentequipment within the same laboratory.
32、)13.1.5 Any judgment in accordance with 13.1.2 and 13.1.3will have an approximate 95 % (0.95) probability of beingcorrect.13.2 BiasThere are no recognized standards on which tobase an estimate of bias for this test method.14. Keywords14.1 adipate; benzoate; gas chromatography; monomeric;phthalate; p
33、lasticizers; poly(vinyl chloride); PVC; trimellitateSUMMARY OF CHANGESCommittee D20 has identified the location of selected changes to this standard since the last issue(D3465 - 00(2007)1) that may impact the use of this standard. (March 1, 2014)(1) Changed subcommittee section from D20.70.03 toD20.
34、70.02.(2) Removed “(FL)” in 5.1.(3) Removed permissive language.(4) Updated trademark information in Footnotes 3-5.(5) Changed “quantity” to “sample size” in 10.3.(6) Added new keywords to Section 14.ASTM International takes no position respecting the validity of any patent rights asserted in connec
35、tion with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such 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 responsib
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37、sideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received 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
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