ASTM D6505-00(2006)
(Test Method)Standard Test Method for Assay of normal-Propyl Bromide Content
Standard Test Method for Assay of <i>normal</i>-Propyl Bromide Content
SIGNIFICANCE AND USE
This test method provides an analysis in weight percent of the normal-propyl bromide concentration of virgin, formulated, or reclaimed normal-propyl bromide: compounds that co-elute with normal-propyl bromide or normal-heptane (internal standard) may interfere with this test method.
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
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:D6505–00(Reapproved2006)
Standard Test Method for
Assay of normal-Propyl Bromide Content
This standard is issued under the fixed designation D6505; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope 5. Required Chemicals
1.1 This test method provides a basis for the determination 5.1 n-Propyl Bromide (1-Bromopropane), 99+ %, Aldrich
of the normal-propyl bromide (weight %) in the presence of Chemical Company
stabilizersandimpurities,invirginorreclaimednormal-propyl 5.2 n-Heptane (internal standard), Reagent Grade,
bromide (nPB). The application range is from 50 to 100 wt %. 99.5+ %, J.T. Baker (or equivalent)
5.3 Methylene Chloride, 99+ %, Aldrich Chemical Com-
2. Summary of Test Method
pany (or equivalent)
2.1 This analytical test method describes the determination
6. Suggested Analysis Conditions
of the assay of n-propyl bromide by gas chromatography using
an internal standard.The results are reported in weight percent. 6.1 Chromatographic Conditions:
Injector 150°C
3. Significance and Use
Detector temperature 250°C
3.1 This test method provides an analysis in weight percent
of the normal-propyl bromide concentration of virgin, formu-
FID detector range most sensitive setting
lated, or reclaimed normal-propyl bromide: compounds that
Temperature pro- 30°C for 10 min
co-elute with normal-propyl bromide or normal-heptane (in-
gram 30 to 250°C at 15°C/min
ternal standard) may interfere with this test method.
hold at 250°C for 10 min
Carrier gas He (or N ) at 1 mL/min
4. Apparatus 2
split flow: 25 mL/min
4.1 Gas Chromatograph—Hewlett Packard 5890 Series II
column head pressure: 7.5 psi
equipped with a split/splitless injector, a flame ionization
Make-up gas He (or N ) at 30 mL/min
detector, and an autosampler, HP, or equivalent, if available.
4.2 Column—30 m by 0.25 mm, 1.0-µm film thickness
Injection volume 0.5 µL
AllTech AT-5, or equivalent, capillary column.
7. Analytical Procedure
4.3 Syringe—5-µL or 10-µL GC autosampler syringe.
7.1 Internal Standard Calibration Mixture—Carefully
4.4 Data Acquisition and Analysis Device—VAX MULTI-
weigh about 0.25 g of n-heptane internal standard and about
CHROM or equivalent chromatography data collection and
0.5gof n-propyl bromide into a 32-mL glass vial. Record the
processing system, or integrator.
actualweightsforeach.Pipet25mLofmethylenechlorideinto
4.5 Crimp Top Vials—Hewlett Packard 2-mL glass crimp
this vial and cap immediately. Mix well and then transfer
top vials withTFE-fluorocarbon-lined silicone septa or equiva-
approximately 1 mL of this standard solution into an autosam-
lent.
pler vial. Cap the vial and analyze in accordance with the
4.6 Volumetric Pipet—25 mL.
conditions specified in the chromatographic conditions section.
4.7 Glass Vials—32–mL glass vials (25 by 95 mm), with
Inject this standard at least three times and calibrate an internal
TFE-fluorocarbon-lined screw caps.
standard method in the data system using the results from the
4.8 Transfer Pipets—Borosilicate glass transfer pipets.
standard analyses.
4.9 Precision Balance, accurate to 0.1 mg.
7.2 PreparationofSamplesforAnalysis—Weigh about 0.25
gof n-heptane and about 0.5 g of sample into a 32-mL glass
vial. Record the actual weights for each. Pipet 25 mL of
This test method is under the jurisdiction of ASTM Committee D26 on
Halogenated Organic Solvents and Fire Extinguishing Agents and is the direct
methylene chloride into this vial and cap immediately. Mix
responsibility of Subcommittee D26.04 on Test Methods.
well and transfer approximately 1 mL of this solution to an
Current edition approved Jan. 1, 2006. Published February 2006. Originally
autosampler vial. Cap the vial and analyze in accordance with
published in 2000. Last previous edition approved in 2000 as D6505–00. DOI:
10.1520/D6505-00R06.
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