ASTM D3447-00a

Standard Test Method for Purity of Halogenated Organic Solvents

SCOPE
1.1 This test method covers the determination of common impurities found in halogenated organic solvents introduced during the manufacturing of the solvent. Although the absolute sensitivity may vary, sensitivity in the parts per million range may be achieved under the chromatographic conditions specified in this method.
1.2 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: 09-Jun-2001
• ICS: 71.080.20 - Halogenated hydrocarbons
• 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NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 3447 – 00a An American National Standard
Standard Test Method for
Purity of Halogenated Organic Solvents
This standard is issued under the fixed designation D 3447; 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.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope 4.4 Flow Meter, soap-bubble type or equivalent.
4.5 Helium, research grade carrier gas.
1.1 This test method covers the determination of common
impurities found in halogenated organic solvents introduced
5. Procedure
during the manufacturing of the solvent. Although the absolute
5.1 Install the column and adjust the helium carrier gas flow
sensitivity may vary, sensitivity in the parts per million range
to 40 mL/min.
may be achieved under the chromatographic conditions speci-
5.2 Set up the gas chromatograph according to the param-
fied in this test method.
eters listed as follows:
1.2 This standard does not purport to address all of the
Injection port temperature : 200°C
safety concerns, if any, associated with its use. It is the
Detector temperature : 220°C
responsibility of the user of this standard to establish appro-
Oven initial temperature : 50°C
priate safety and health practices and determine the applica-
Oven final temperature : 170°C
Temperature program rate : 10°C/min
bility of regulatory limitations prior to use.
5.3 Inject 1.0 μL of sample into the gas chromatograph and
2. Summary of Test Method
start the temperature program. Simultaneously start the record-
2.1 This test method is based on a temperature-programmed
ing device to begin recording peak areas.
gas chromatographic separation achieved on a packed column
5.4 If an integrator is not used, record the chromatogram
containing 30 % by weight silicone oil on 80/100 mesh
using the minimum detector attenuation setting necessary to
diatomaceous earth.
keep each peak on-scale at all times.
5.5 Terminate the chromatogram after all peaks have eluted
3. Significance and Use
from the column.
3.1 This test method can be used to check the purity of
6. Calculation
halogenated organic solvents by determining the impurities
present under the chromatographic conditions specified.
6.1 Obtain from the integrator the areas of all of the peaks
3.2 This test can be used for establishing manufacturing and
eluted in the chromatogram and calculate the solvent purity as
purchasing specifications.
follows:
purity, % 5 100 2 @~A 3 100!/~A 1 B!# (1)
4. Apparatus
4.1 Gas Chromatograph, equipped with a 1-mv recorder or
where:
electronic integrator and a thermal conductivity or flame
A = summation of the peak areas of the impurities, and
ionization detector. B = peak area of trichlorotrifluoroethane.
4.2 Column, 6-m by 3.2-mm outside diameter stainless steel
6.2 If an integrator was not used, measure the area of each
tubing
...