ASTM D3465-00

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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
Designation:D3465–00
Standard Test Method for
Purity of Monomeric Plasticizers by Gas Chromatography
This standard is issued under the fixed designation D 3465; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope * E 1510 Practice for Installing Fused Silica Open Tubular
Capillary Columns in Gas Chromatographs
1.1 This gas chromatographic test method covers a proce-
IEEE/ASTM SI-10 Practice for Use of the International
dure for extending the range of purity determination of
System of Units (SI), the Modernized Metric System
monomeric plasticizers beyond that now determined by other
methods. Due to the need to volatilize the plasticizer, only
3. Terminology
monomeric plasticizers having definitive boiling points and a
3.1 Definitions:
molecular weight less than 1000 Daltons, such as dioctyl
3.1.1 General—Definitions are in accordance with Termi-
phthalate, are applicable to this test method.
nology D 883 and Terminology D 1600 unless otherwise indi-
1.2 The values in SI units are to be regarded as standard.
cated.
1.3 The text of this test method references notes and
3.1.2 All gas chromatography terms and relationships used
footnotes that provide explanatory material. These notes and
in this test method are consistent with, or refer to, Practice
footnotes (excluding those in tables and figures) are not to be
E 355.
considered as requirements of this test method.
1.4 This standard does not purport to address all of the
4. Summary of Test Method
safety concerns, if any, associated with its use. It is the
4.1 Atestportionoftheplasticizertobeanalyzedisinjected
responsibility of the user of this standard to establish appro-
onto a gas chromatographic column and separated into its
priate safety and health practices and determine the applica-
components, which are sensed by the detector and quantified
bility of regulatory limitations prior to use. Specific precau-
by an electronic data acquisition system (computer) or an
tionary statements are given in Section 9
integrator. The purity is based on the total area response of the
NOTE 1—There is no ISO equivalent for this test method.
principal peak(s). All other components are impurities.
2. Referenced Documents
5. Significance and Use
2.1 ASTM Standards:
5.1 Infrared techniques frequently cannot detect low-level
D 883 Terminology Relating to Plastics
materials. Gas chromatographic methods possess higher sensi-
D 1600 Terminology for Abbreviated Terms Relating to
tivity, and are used to extend (FL) limits of detection.
Plastics
5.2 It is expected that this test method will be suitable for
D 2124 Test Method for Analysis of Components in Poly-
specifications, manufacturing control, and research and devel-
(Vinyl Chloride) Compounds Using an Infrared
opment. An area percent method of determining concentration
Spectrophoto-metric Technique
of the components shall be used if the area percent of the
E 177 Practice for Use of the Terms Precision and Bias in
plasticizer is 99.0 % or higher. However, if the area percent of
ASTM Test Methods
the plasticizer is less than 99.0 % or should any question arise
E 260 Practice for Packed Column Gas Chromatography
about the data, an internal standard shall be used.
E 355 Practice for Gas Chromatography Terms and Rela-
5.3 Impurities that may be found in monomeric plasticizers
tionships
include alcohols, dibasic acids, and monoesters.
E 594 Standard Practice for Testing Flame Ionization De-
6. Interferences
tectors in Gas or Supercritical Fluid Chromatography
6.1 Gas chromatography (GC) retention times are depen-
dentonseveralvariables,anditispossibletohavetwoormore
components with identical retention times. The GC operator
This test method is under the jurisdiction ofASTM Committee D20 on Plastics
should take the necessary steps to insure that adequate sepa-
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods
(Section D20.70.03).
ration of the plasticizer components is achieved. Analysis by
Current edition approved Aug. 10, 2000. Published October 2000. Originally
published as D 3465 – 75. Last previous edition D 3465 – 75 (1990).
Annual Book of ASTM Standards, Vol 08.01.
3 4
Annual Book of ASTM Standards, Vol 14.02. Annual Book of ASTM Standards, Vol 14.04.
*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.
D3465
gas chromatography/mass spectormetry may identify the pres- 10.2 Program the temperature of the column suitable to best
ence of overlapping components. separatethecomponents(see7.1forcolumns).Typicalsettings
are as follows:
7. Apparatus
10°C/min from 60 to 280°C and hold.
10°C/min from 100 to 300°C and hold for 10 min.
7.1 Gas Chromatograph, equipped with a flame ionization
orthermalconductivitydetectorandcapableofoperatinginthe
10.3 Sample Size—Select a sample size that provides an
range from 250 to 350°C.
adequate chromatographic efficiency (that is, do not overload
7.1.1 Capillary or Packed Gas Chromatographic Column,
the column). Typical quantity is 1 µL.
capable of operating in the range from 250 to 350°C that
10.4 Carrier Gas—Helium, flow rate 30 to 60 cm /min.
provides adequate separation and definition of components.
Examples are as follows:
11. Procedure
7.1.2 Packed Columns, stainless steel, 1.83 m (6 ft) long,
11.1 The method of injecting the sample onto the column
with an outside diameter of 6.4 mm ( ⁄4 in.) and filled with
and analyzing for
...