ASTM D3465-00(2007)e1
(Test Method)Standard Test Method for Purity of Monomeric Plasticizers by Gas Chromatography
Standard Test Method for Purity of Monomeric Plasticizers by Gas Chromatography
SCOPE
1.1 This gas chromatographic test method covers a procedure for extending the range of purity determination of monomeric plasticizers beyond that now determined by other methods. Due to the need to volatilize the plasticizer, only monomeric plasticizers having definitive boiling points and a molecular weight less than 1000 Daltons, such as dioctyl phthalate, are applicable to this test method.
1.2 The values in SI units are to be regarded as standard.
1.3 The text of this test method references notes and footnotes that provide explanatory material. These notes and footnotes (excluding those in tables and figures) are not to be considered as requirements of this test method.
This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific precautionary statements are given in Section 9.Note 1
There is no known ISO equivalent for this test method.
General Information
Relations
Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
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Designation: D3465 − 00(Reapproved 2007)
Standard Test Method for
Purity of Monomeric Plasticizers by Gas Chromatography
This standard is issued under the fixed designation D3465; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
´ NOTE—Reapproved with editorial changes to Note 1 and 6.1 in November 2007.
1. Scope* E260 Practice for Packed Column Gas Chromatography
E355 Practice for Gas ChromatographyTerms and Relation-
1.1 This gas chromatographic test method covers a proce-
ships
dure for extending the range of purity determination of
E594 Practice for Testing Flame Ionization Detectors Used
monomeric plasticizers beyond that now determined by other
in Gas or Supercritical Fluid Chromatography
methods. Due to the need to volatilize the plasticizer, only
E1510 Practice for Installing Fused Silica Open Tubular
monomeric plasticizers having definitive boiling points and a
Capillary Columns in Gas Chromatographs
molecular weight less than 1000 Daltons, such as dioctyl
IEEE/ASTM SI-10 Practice for Use of the International
phthalate, are applicable to this test method.
System of Units (SI), the Modernized Metric System
1.2 The values in SI units are to be regarded as standard.
1.3 The text of this test method references notes and 3. Terminology
footnotes that provide explanatory material. These notes and
3.1 Definitions:
footnotes (excluding those in tables and figures) are not to be
3.1.1 General—Definitions are in accordance with Termi-
considered as requirements of this test method.
nology D883 and Terminology D1600 unless otherwise indi-
1.4 This standard does not purport to address all of the
cated.
safety concerns, if any, associated with its use. It is the
3.1.2 All gas chromatography terms and relationships used
responsibility of the user of this standard to establish appro-
in this test method are consistent with, or refer to, Practice
priate safety and health practices and determine the applica-
E355.
bility of regulatory limitations prior to use. Specific precau-
tionary statements are given in Section 9
4. Summary of Test Method
NOTE 1—There is no known ISO equivalent for this test method.
4.1 Atestportionoftheplasticizertobeanalyzedisinjected
onto a gas chromatographic column and separated into its
2. Referenced Documents
components, which are sensed by the detector and quantified
2.1 ASTM Standards:
by an electronic data acquisition system (computer) or an
D883 Terminology Relating to Plastics
integrator. The purity is based on the total area response of the
D1600 TerminologyforAbbreviatedTermsRelatingtoPlas-
principal peak(s). All other components are impurities.
tics
D2124 Test Method forAnalysis of Components in Poly(Vi-
5. Significance and Use
nyl Chloride) Compounds Using an Infrared Spectropho-
5.1 Infrared techniques frequently cannot detect low-level
tometric Technique
materials. Gas chromatographic methods possess higher
E177 Practice for Use of the Terms Precision and Bias in
sensitivity, and are used to extend (FL) limits of detection.
ASTM Test Methods
5.2 It is expected that this test method will be suitable for
specifications, manufacturing control, and research and devel-
This test method is under the jurisdiction ofASTM Committee D20 on Plastics
opment.An area percent method of determining concentration
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods
(Section D20.70.03).
of the components shall be used if the area percent of the
Current edition approved Nov. 1, 2007. Published November 2007. Originally
plasticizer is 99.0 % or higher. However, if the area percent of
approved in 1975. Last previous edition approved in 2000 as D3465 - 00. DOI:
the plasticizer is less than 99.0 % or should any question arise
10.1520/D3465-00R07E01.
about the data, an internal standard shall be used.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
5.3 Impurities that may be found in monomeric plasticizers
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. include alcohols, dibasic acids, and monoesters.
*A Summary of Changes section appears at the end of this standard
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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D3465 − 00 (2007)
6. Interferences 10. Preparation of the Gas Chromatograph
6.1 Gas chromatography (GC) retention times are depen- 10.1 Temperature Settings—This test method requires injec-
dentonseveralvariables,anditispossibletohavetwoormore tion port and detector temperatures of 260 to 350°C. For a
components with identical retention times. The GC operator plasticizer with a nominal boiling point of 410°C, the follow-
should take the necessary steps to insure that adequate sepa- ing conditions are suggested:
ration of the plasticizer components is achieved. Analysis by
Injection port 260 to 350°C
Detector 300 to 350°C
gas chromatography/mass spectrometry may identify the pres-
ence of overlapping components.
10.2 Program the temperature of the column suitable to best
separatethecomponents(see7.1forcolumns).Typicalsettings
7. Apparatus
are as follows:
7.1 Gas Chromatograph, equipped with a flame ionization
10°C/min from 60 to 280°C and hold.
10°C/min from 100 to 300°C and hold for 10 min.
orthermalconductivitydetectorandcapableofoperatinginthe
range from 250 to 350°C.
10.3 Sample Size—Select a sample size that provides an
7.1.1 Capillary or Packed Gas Chromatographic Column,
adequate chromat
...
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