ASTM D5320-96

Standard Test Methods for Determination of 1,1,1-Trichloroethane and Methylene Chloride Content in Stabilized Trichloroethylene and Tetrachloroethylene

SCOPE
1.1 These test methods provide a means for determining low levels of 1,1,1-trichloroethane and methylene chloride in virgin or reclaimed trichloroethylene and tetrachloroethylene.
1.2 Two test methods are covered, as follows:
1.2.1 Test Method A -Capillary column gas chromatographic determination of 1,1,1-trichloroethane and methylene chloride in trichloroethylene and tetrachloroethylene.
1.2.2 Test Method B-Packed column gas chromatographic determination of 1,1,1-trichloroethane and methylene chloride in trichloroethylene and tetrachloroethylene.
1.3 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.

General Information

• Status: Historical
• Publication Date: 31-Dec-1999
• Technical Committee: D26 - Halogenated Organic Solvents and Fire Extinguishing Agents
• Drafting Committee: D26.04 - Test Methods

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NOTICE: This standard has either been superseded and replaced by a new version or
withdrawn.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.
Designation: D 5320 – 96
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 Methods for
Determination of 1,1,1-Trichloroethane and Methylene
Chloride Content in Stabilized Trichloroethylene and
1
Tetrachloroethylene
This standard is issued under the fixed designation D 5320; 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 in trichloroethylene and tetrachloroethylene. The other compo-
nents shall be able to be resolved by recommended GC
1.1 These test methods provide a means for determining low
columns and the gas chromatograph shall be calibrated with
levels of 1,1,1-trichloroethane and methylene chloride in virgin
known concentration of these compounds.
or reclaimed trichloroethylene and tetrachloroethylene.
1.2 Two test methods are covered, as follows:
4. Interferences
1.2.1 Test Method A—Capillary column gas chromato-
4.1 Compounds that co-elute with 1,1,1-trichloroethane,
graphic determination of 1,1,1-trichloroethane and methylene
methylene chloride, or other components of interest can
chloride in trichloroethylene and tetrachloroethylene.
interfere with the accuracy of these test methods.
1.2.2 Test Method B—Packed column gas chromatographic
determination of 1,1,1-trichloroethane and methylene chloride
5. Apparatus
in trichloroethylene and tetrachloroethylene.
5.1 Gas Chromatograph, temperature programmable and
1.3 This standard does not purport to address all of the
having the following minimum capabilities:
safety concerns, if any, associated with its use. It is the
5.1.1 Chart Recorder or Electronic Integrator—An elec-
responsibility of the user of this standard to establish appro-
tronic integrator is preferable.
priate safety and health practices and determine the applica-
5.1.2 Flame Ionization Detector and Capillary Split/
bility of regulatory limitations prior to use.
Splitless Injection Port (for Test Method A).
2. Summary of Test Methods
5.1.3 Thermal Conductivity Detector and Packed Column
2.1 Samples of trichloroethylene or tetrachloroethylene are Injection Port (for Test Method B).
introduced into a gas chromatography (GC) equipped with
NOTE 1—This procedure was tested using the combinations of capillary
either a thermal conductivity detector (TCD) or a flame
column with flame ionization detector and packed GC column with
ionization detector (FID). Calibration mixtures containing
thermal conductivity detector. It should be possible, however, to perform
known concentrations of methylene chloride, 1,1,1- this analysis with either column and detector combination.
trichloroethane, or other impurities of interest are introduced
5.2 Gas Chromatography Columns:
into the chromatograph in the same manner. The amount of
5.2.1 Column for Test Method A—30-m by 0.53-mm inner
these impurities in the samples is then calculated by comparing
diameter fused silica capillary, internally coated to a 3-μm
the peak areas of these compounds from sample chromato- 2
thickness with a cross-linked polymethyl silicone.
grams with the corresponding peak areas from calibration
1
5.2.2 Column for Test Method B—10-ft by ⁄8-in. outer
standard chromatograms. Instrumental parameters are provided
diameter stainless steel packed with 3 % SP1500 on 80/100
to allow the use of either capillary or packed gas chromatog-
mesh Carbopack B, or equivalent.
raphy columns.
5.3 Syringe,10μL.
5.4 Microsyringes, assorted sizes for preparing calibration
3. Significance and Use
standards.
3.1 These test methods can be used to determine the
5.5 Volumetric Flasks, 100 mL.
impurity levels of 1,1,1-trichloroethane and methylene chloride
5.6 Flow Meter, soap bubble or electronic type.
in both trichloroethylene and tetrachloroethylene.
5.7 Analytical Balance, capable of weighing to four decimal
3.2 These test methods can be used to determine the
places.
impurity levels of other components, such as stabilizers, found
2
1
J&W Scientific DB-1 fused silica capillary column (Cat# 125-1035) available
These test methods are under the jurisdiction of ASTM Committee D-26 on
from J&W Scientific, 91 Blue Ravine Rd., Folsom, CA 95630-4917, or Supelco
Halogenated Organic Solvents and Fire Extinguishing Agents and are the direct
(SPB-1 Cat# 2-5341M) available from Supelco, Inc., Supelco Park, Bellefonte, PA
responsibility of Subcommittee D26.04 on Test Methods.
16823-0048, have been found satisfactory for this purpose. Any equivalent may be
Current edition approved June 10, 1996. Published August 1996. Originally
used.
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