ASTM D3834-93

Test Method for Purity of Vinyl Chloride Monomer by Gas Chromatography (Withdrawn 1998)

SCOPE
1.1 The general availability of gas chromatography in practically every laboratory and the inherent sensitivity in the detection of trace constituents indicate that the technique would qualify as a standard test method. With this one-step technique, impurities can be determined in a range that includes major constituents and parts per million impurities.  
1.2 Inherent in this test method is the limitation that the impurities must be volatile. Resolution of some of the individual impurities may be limited by the column selected. The use of several different types of columns may be necessary if the ultimate in resolution is required. A single column will normally give the required degree of separation.  
1.3 The values stated in SI units are to be regarded as the standard.
1.4 This standard does not purport to address all of the safety problems, 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 hazards statements are given in Section 8. Note-There is no similar or equivalent ISO standard.

General Information

• Status: Withdrawn
• Publication Date: 31-Dec-1992
• Withdrawal Date: 09-Nov-1998
• ICS: 71.080.20 - Halogenated hydrocarbons
• Technical Committee: D20 - Plastics
• Drafting Committee: D20.70 - Analytical Methods

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 3834 – 93
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Method for
Purity of Vinyl Chloride Monomer by Gas Chromatography
This standard is issued under the fixed designation D 3834; 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 relative concentration of a component and the retention time.
1.1 The general availability of gas chromatography in prac-
5. Significance and Use
tically every laboratory and the inherent sensitivity in the
5.1 Vinyl chloride monomer (Warning: see 8.1) must be
detection of trace constituents indicate that the technique
very pure to produce high-quality polymers with desirable
would qualify as a standard test method. With this one-step
appearance, stability, and generally desirable physical proper-
technique, impurities can be determined in a range that
ties. Even trace concentrations of certain impurities, for ex-
includes major constituents and parts per million impurities.
ample, conjugated dienes, interfere with the mechanism of
1.2 Inherent in this test method is the limitation that the
polymerization. This test method is applied accordingly to
impurities must be volatile. Resolution of some of the indi-
process and quality control.
vidual impurities may be limited by the column selected. The
5.2 It is expected that this test method will be suitable for
use of several different types of columns may be necessary if
specifications, manufacturing control, and research and devel-
the ultimate in resolution is required. A single column will
opment. However, other specifications may be required to
normally give the required degree of separation.
define a product completely.
1.3 The values stated in SI units are to be regarded as the
standard.
6. Interferences
1.4 This standard does not purport to address all of the
6.1 Retention times are dependent upon a large number of
safety problems, if any, associated with its use. It is the
variables associated with the composition, length, and diameter
responsibility of the user of this standard to establish appro-
of the column, the size of the sample, the temperature of the
priate safety and health practices and determine the applica-
column, the carrier gas flow rate, and the temperature of the
bility of regulatory limitations prior to use. Specific hazards
injection port. It is therefore quite possible to have two
statements are given in Section 8.
components or impurities with identical retention times. Only
NOTE 1—There is no similar or equivalent ISO standard.
by changing columns or column conditions can these concur-
rent peaks be resolved.
2. Referenced Documents
6.2 Temperature programming, as recommended in this test
2.1 ASTM Standards:
method, must be precisely controlled to obtain reproducible
E 260 Practice for Packed Column Gas Chromatography
retention times and reliable identification of constituents.
E 355 Practice for Gas Chromatography Terms and Rela-
6.3 A given species has only one peak associated with it for
tionships
identification; therefore, identification from that one peak by its
retention time alone is risky unless coupled with other infor-
3. Terminology
mation. Such information might be obtained with a mass
3.1 Definitions—All terms and practices used in this test
spectrometer or chemical tests for functional groups.
method are in accordance with Practices E 260 and E 355.
7. Apparatus
4. Summary of Test Method
7.1 Many commercial instruments are suitable for this test;
4.1 Conventional gas chromatographic techniques are used.
however, there are two basic requirements. The detectors must
A small sample is injected into a gas chromatographic column
be equivalent in sensitivity to hydrogen flame ionization
packed with a liquid-coated solid support or porous polymer
detectors and the column oven must be designed for tempera-
beads. Passing over the support in a stream of helium, the
ture programming in the range from 40 to 150°C.
sample is separated into its components, which are detected by
7.2 The basic equipment includes: injection ports, columns,
a standard sensing device. The signal is recorded to indicate the
column ovens, detectors, a recorder, a suitable attenuating
device for keeping the peaks on scale, a temperature program-
This test method is under the jurisdiction of ASTM Committee D-20 on Plastics
ming unit, and a syringe or liquid-sampling valve for injection
and is the direct responsibility of Subcommittee D20.70 on Analytical Methods.
of microlitres of sample onto the columns.
Current edition approved Feb. 15, 1993. Published April 1993. Originally
7.3 Dual columns are recommended for stable baselines.
published as D 3834 – 80. Last previous edition D 3834 – 80 (1987).
Annual Book of ASTM Standards, Vol 14.01. 7.4 An electronic or mechanical integrator is recommended
D 3834
for measurement of peak areas. Porapak S or other equivalent commercial packing. Table 2
7.5 Recommended Columns—To provide greater versatility, lists average retention times and relative retention time for
two different types are recommended: one consists of a liquid some components possibly present in vinyl chloride monomer
phase on a solid support and the other is of commercially analyzed using a porous polymer column.
available porous polymer beads. Greater resolution of C-4 7.6 Other Operating Conditions:
hydrocarbons is obtained with the former column, and better 7.6.1 Temperatures:
separation of some light components is observed with the latter
Liquid phase column:
Injection port 125°C
column. Other columns with equivalent performance may be
Detector 260°C
used.
Column 40°C until elution of vinyl chlo-
7.5.1 Liquid Phase Column—A mixture consisting of 75 % ride, then program at 6.0°C/min
3 4
to 150°C
Igepal CO-880 and 25 % Antarox BL344 or LF330 is applied
to 60 to 80-mesh firebrick to produce a liquid content of 25
Porapak S column:
weight % and packed in 3.175-mm stainless steel tubing, 6 m
Injection port 150°C
Detector 280°C
long. Table 1 lists average retention times and relative retention
Column 50°C for 2 min, then pro-
times for some components possibly present in vinyl chloride
grammed at 6.0°C/min to 150°C
monomer analyzed on the liquid phase column.
7.6.2 Detector Type—Hydrogen flame ionization or other
7.5.2 Porous Polymer Bead Column—A 2-m length of
detector of equivalent sensitivity.
4.76-mm stainless steel tubing is packed with 80- to 100-mesh
7.6.3 Sample Size—5 μL liquid or 0.5 mL gas.
7.6.4 Carrier Gas—Helium, 60 mL/min.
8. Hazards
A trademark for a nonylphenoxy poly(ethyleneoxy)ethanol, which may be
8.1 Warning: Recent public information indicates that vi-
obtained from GAF Corp., Dyestuff and Chemical Div., 140 W. 51st St., New York,
NY 10020.
nyl chloride monomer may be toxic to humans, both by skin
A trademark for a series of surfactants which may be obtained from GAF Corp.,
contact and inhalation.
Dyestuff and Chemical Div., 140 W. 51st St., New York, NY 10020.
8.2 Precaution—Laboratory personnel are cauti
...