ASTM D6505-00

Standard Test Method for Assay of <i>normal</i>-Propyl Bromide Content

SCOPE
1.1 This test method provides a basis for the determination of the normal-propyl bromide (weight %) in the presence of stabilizers and impurities, in virgin or reclaimed normal-propyl bromide (nPB). The application range is from 50 to 100 wt %.

General Information

• Status: Historical
• Publication Date: 09-Jan-2000
• ICS: 71.080.20 - Halogenated hydrocarbons
• Technical Committee: D26 - Halogenated Organic Solvents and Fire Extinguishing Agents
• Drafting Committee: D26.04 - Test Methods

Relations

• Replaced By: ASTM D6505-00(2006) - Standard Test Method for Assay of <i>normal</i>-Propyl Bromide Content
• Effective Date: 01-Jan-2006

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:D6505–00
Standard Test Method for
Assay of normal-Propyl Bromide Content
This standard is issued under the fixed designation D 6505; 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 5.2 n-Heptane (internal standard), Reagent Grade,
99.5+ %, J.T. Baker (or equivalent)
1.1 This test method provides a basis for the determination
5.3 Methylene Chloride, 99+ %, Aldrich Chemical Com-
of the normal-propyl bromide (weight %) in the presence of
pany (or equivalent)
stabilizersandimpurities,invirginorreclaimednormal-propyl
bromide (nPB). The application range is from 50 to 100 wt %.
6. Suggested Analysis Conditions
2. Summary of Test Method 6.1 Chromatographic Conditions:
Injector 150°C
2.1 This analytical test method describes the determination
of the assay of n-propyl bromide by gas chromatography using
Detector temperature 250°C
an internal standard.The results are reported in weight percent.
FID detector range most sensitive setting
3. Significance and Use
Temperature pro- 30°C for 10 min
3.1 This test method provides an analysis in weight percent
gram 30 to 250°C at 15°C/min
hold at 250°C for 10 min
of the normal-propyl bromide concentration of virgin, formu-
lated, or reclaimed normal-propyl bromide: compounds that
Carrier gas He (or N ) at 1 mL/min
co-elute with normal-propyl bromide or normal-heptane (in-
split flow: 25 mL/min
column head pressure: 7.5 psi
ternal standard) may interfere with this test method.
Make-up gas He (or N ) at 30 mL/min
4. Apparatus
Injection volume 0.5 µL
4.1 Gas Chromatograph—Hewlett Packard 5890 Series II
equipped with a split/splitless injector, a flame ionization
7. Analytical Procedure
detector, and an autosampler, HP, or equivalent, if available.
7.1 Internal Standard Calibration Mixture—Carefully
4.2 Column—30 m by 0.25 mm, 1.0-µm film thickness
weigh about 0.25 g of n-heptane internal standard and about
AllTech AT-5, or equivalent, capillary column.
0.5gof n-propyl bromide into a 32-mL glass vial. Record the
4.3 Syringe—5-µL or 10-µL GC autosampler syringe.
actualweightsforeach.Pipet25mLofmethylenechlorideinto
4.4 Data Acquisition and Analysis Device—VAX MULTI-
this vial and cap immediately. Mix well and then transfer
CHROM or equivalent chromatography data collection and
approximately 1 mL of this standard solution into an autosam-
processing system, or integrator.
pler vial. Cap the vial and analyze in accordance with the
4.5 Crimp Top Vials—Hewlett Packard 2-mL glass crimp
conditions specified in the chromatographic conditions section.
top vials withTFE-fluorocarbon-lined silicone septa or equiva-
Inject this standard at least three times and calibrate an internal
lent.
standard method in the data system using the results from the
4.6 Volumetric Pipet—25 mL.
standard analyses.
4.7 Glass Vials—32–mL glass vials (25 by 95 mm), with
7.2 PreparationofSamplesforAnalysis—Weigh about 0.25
TFE-fluorocarbon-lined screw caps.
gof n-heptane and about 0.5 g of sample into a 32-mL glass
4.8 Transfer Pipets—Borosilicate glass transfer pipets.
vial. Record the actual weights for each. Pipet 25 mL of
4.9 Precision Balance, accurate to 0.1 mg.
methylene chloride into this vial and cap immediately. Mix
well and transfer approximately 1 mL of this solution to an
5. Required Chemicals
autosampler vial. Cap the vial and analyze in accordance with
5.1 n-Propyl Bromide (1-Bromopropane), 99+ %, Aldrich
the conditions specified in the chromatographic conditions
Chemical Company
section. The following table shows components of interest,
their absolute retention time (ART) in minutes, their relative
This test method is under the jurisdiction of ASTM Committee D-26 on
retention time (RRT) in relation to n-heptane, the internal
Halogenate
...