1、Designation: D 3465 00Standard 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, the year of last revis
2、ion. 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 ofmonomeric plastici
3、zers 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
4、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 address all of the
5、safety 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 i
6、s no ISO equivalent for this test method.2. Referenced Documents2.1 ASTM Standards:D 883 Terminology Relating to Plastics2D 1600 Terminology for Abbreviated Terms Relating toPlastics2D 2124 Test Method for Analysis of Components in Poly-(Vinyl Chloride) Compounds Using an InfraredSpectrophoto-metric
7、 Technique2E 177 Practice for Use of the Terms Precision and Bias inASTM Test Methods3E 260 Practice for Packed Column Gas Chromatography3E 355 Practice for Gas Chromatography Terms and Rela-tionships3E 594 Standard Practice for Testing Flame Ionization De-tectors in Gas or Supercritical Fluid Chrom
8、atography3E 1510 Practice for Installing Fused Silica Open TubularCapillary Columns in Gas Chromatographs3IEEE/ASTM SI-10 Practice for Use of the InternationalSystem of Units (SI), the Modernized Metric System43. Terminology3.1 Definitions:3.1.1 GeneralDefinitions are in accordance with Termi-nology
9、 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 A test portion of the plasticizer to be analyzed is injectedonto a gas chromatographic c
10、olumn 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 Use5.1 Infrared
11、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-opment. An area
12、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 Impurities that
13、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 take the neces
14、sary 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 edition approved
15、Aug. 10, 2000. Published October 2000. Originallypublished as D 3465 75. Last previous edition D 3465 75 (1990).2Annual Book of ASTM Standards, Vol 08.01.3Annual Book of ASTM Standards, Vol 14.02.4Annual Book of ASTM Standards, Vol 14.04.1*A Summary of Changes section appears at the end of this stan
16、dard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.gas chromatography/mass spectormetry may identify the pres-ence of overlapping components.7. Apparatus7.1 Gas Chromatograph, equipped with a flame ionizationor thermal conductivity
17、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 thatprovides adequate separation and definition of components.Examples are as follows:7.1.2 Packed Columns, stainless steel, 1.83 m (
18、6 ft) long,with an outside diameter of 6.4 mm (14 in.) and filled withChromosorb W or WAW,560 to 80 mesh, as the solid support.7.1.2.1 Liquid PhaseThe liquid phase sensitivity changesthe utility in detecting various impurities. Examples of detect-ability of alcohol impurities are illustrated as foll
19、ows:7.1.2.2 A coating of 5 to 15 % of SE-306silicone gumstockresults in reasonably symmetrical peaks and accurate quanti-tative measurements between 0.1 and 1 % alcoholic impurities.7.1.2.3 A coating of 15 % Igepal CO-9907results in sepa-rations of similar types of esters such as diisooctyl phthalat
20、eand di (2-ethylhexyl) phthalate at the 1 % level.7.1.2.4 A coating of 20 % Ozonite8is also effective foralcohols in the 0.1 to 1 % concentration level.7.1.3 Capillary Columns, fused silica high-temperature cap-illary column with a 100 % poly(dimethylsiloxane) stationaryphase; length: 15 to 30 m; in
21、side 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 to10.0 L capacity.7.4 Pressure Regulators, for all required gas cylinders.7.5 Flowmeter, or other means of measuring gas flow rates.8.
22、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 is flammable. Ensure that all leaks are elimi-nated.10. Preparation of the Gas Chromatograph10.1 Temperature SettingsThis test metho
23、d 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:Injection port 260 to 350CDetector 300 to 350C10.2 Program the temperature of the column suitable to bestseparate the components (see 7.
24、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 provides anadequate chromatographic efficiency (that is, do not overloadthe column). Typical quantity is 1 L.10.4 Carrier GasHelium,
25、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, (specifically, Sections 10 and 14).11.2 The method for analyzing the components shall beconsistent with Fig. 1 of Practice E 355.12. Re
26、port12.1 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 Retention times of impurities, relating them to cor-responding retention times of known substances,12.1.3 Proportion of total area relat
27、ed 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 Bias13.1 PrecisionA round robin is in progress. Table 1 isbased on a single laboratory test using two different capillarycolumns on on
28、e gas chromatograph.13.1.1 Sr is the within-laboratory standard deviation of theaverage; r = 2.8 SR (see 13.1.3 for application of r.)13.1.2 SR is the between-laboratory standard deviation ofthe average; R = 2.8 SR (see 13.1.4 for application of R).13.1.3 RepeatabilityIn comparing two test results f
29、or 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 the r value for thematerial and condition.13.1.4 ReproducibilityBy comparing two test results forthe same material, obtained by di
30、fferent 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 between different laboratories or between differ-ent equipment within the same laboratory.)13.1.5 Any judgment in accordance with
31、 13.1.2 and 13.1.3will have an approximate 95 % (0.95) probability of beingcorrect.5Trademark of Johns-Manville Products Corp.6Trademark of General Electric Co., Schenectady, NY.7Trademark of General Aniline plasticizers; poly(vinyl chloride);PVCSUMMARY OF CHANGESThis section identifies the location
32、 of selected changes to this test method. For the convenience of the user,Committee D20 has highlighted those changes that may impact the use of this test method. This section may alsoinclude descriptions of the changes or reasons for the changes, or both.D 3465-00:(1) Added flame ionization detecto
33、r.(2) Added broader selection of packed columns and tempera-ture ranges.(3) Added capillary columns.(4) Eliminated the precision and bias statement for thermalconductivity detectors (FL).ASTM International takes no position respecting the validity of any patent rights asserted in connection with any
34、 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 responsible technical
35、committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at
36、 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 Barr Harbor D
37、rive, 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 34653
