ASTM D6505-00(2012)

Standard Test Method for Assay of <emph type="bdit">normal</emph>-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

• Status: Historical
• Publication Date: 29-Feb-2012
• ICS: 71.080.20 - Halogenated hydrocarbons
• Technical Committee: D26 - Halogenated Organic Solvents and Fire Extinguishing Agents
• Drafting Committee: D26.04 - Test Methods

Relations

• Replaces: ASTM D6505-00(2006) - Standard Test Method for Assay of <i>normal</i>-Propyl Bromide Content
• Effective Date: 01-Mar-2012

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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 (Reapproved 2012)
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 4.9 Precision Balance, accurate to 0.1 mg.
1.1 This test method provides a basis for the determination
5. Required Chemicals
of the normal-propyl bromide (weight %) in the presence of
5.1 n-Propyl Bromide (1-Bromopropane), 99+ %, Aldrich
stabilizers and impurities, in virgin or reclaimednormal-propyl
Chemical Company
bromide (nPB). The application range is from 50 to 100 wt %.
5.2 n-Heptane (internal standard), Reagent Grade, 99.5+ %,
2. Summary of Test Method
J.T. Baker (or equivalent)
2.1 This analytical test method describes the determination
5.3 Methylene Chloride, 99+ %, Aldrich Chemical Com-
of the assay of n-propyl bromide by gas chromatography using
pany (or equivalent)
an internal standard.The results are reported in weight percent.
6. Suggested Analysis Conditions
3. Significance and Use
6.1 Chromatographic Conditions:
3.1 This test method provides an analysis in weight percent
Injector 150°C
of the normal-propyl bromide concentration of virgin,
formulated, or reclaimed normal-propyl bromide: compounds
Detector temperature 250°C
that co-elute with normal-propyl bromide or normal-heptane
FID detector range most sensitive setting
(internal standard) may interfere with this test method.
Temperature 30°C for 10 min
4. Apparatus
program 30 to 250°C at 15°C/min
hold at 250°C for 10 min
4.1 Gas Chromatograph—Hewlett Packard 5890 Series II
equipped with a split/splitless injector, a flame ionization Carrier gas He (or N ) at 1 mL/min
split flow: 25 mL/min
detector, and an autosampler, HP, or equivalent, if available.
column head pressure: 7.5 psi
4.2 Column—30 m by 0.25 mm, 1.0-µm film thickness
Make-up gas He (or N ) at 30 mL/min
AllTech AT-5, or equivalent, capillary column.
Injection volume 0.5 µL
4.3 Syringe—5-µL or 10-µL GC autosampler syringe.
4.4 Data Acquisition and Analysis Device—VAX MULTI-
7. Analytical Procedure
CHROM or equivalent chromatography data collection and
7.1 Internal Standard Calibration Mixture—Carefully
processing system, or integrator.
weigh about 0.25 g of n-heptane internal standard and about
4.5 Crimp Top Vials—Hewlett Packard 2-mL glass crimp 0.5gof n-propyl bromide into a 32-mL glass vial. Record the
top vials withTFE-fluorocarbon-lined silicone septa or equiva- actualweightsforeach.Pipet25mLofmethylenechlorideinto
lent. this vial and cap immediately. Mix well and then transfer
approximately 1 mL of this standard solution into an autosam-
4.6 Volumetric Pipet—25 mL.
pler vial. Cap the vial and analyze in accordance with the
4.7 Glass Vials—32–mL glass vials (25 by 95 mm), with
conditions specified in the chromatographic conditions section.
TFE-fluorocarbon-lined screw caps.
Inject this standard at least three times and calibrate an internal
4.8 Transfer Pipets—Borosilicate glass transfer pipets. standard method in the data system using the results from the
standard analyses.
7.2 Preparation of Samples forAnalysis—Weigh about 0.25
This test method is under the jurisdiction of ASTM Committee D26 on
Halogenated Organic Solvents and Fire Extinguishing Agents and is the direct
gof n-heptane and about 0.5 g of sample into a 32-mL glass
responsibility of Subcommittee D26.04 on Test Methods.
vial. Record the actual weights for each. Pipet 25 mL of
Current edition approved March 1, 2012. Published June 2012. Originally
methylene chloride into this vial and cap immediately. Mix
published in 2000. Last previous edition approved in 2006 as D6505–00 (2006).
DOI: 10.1520/D6505-00R12. well and transfer approximately 1 mL of this solution to an
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