ASTM D6505-00(2017)

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

SIGNIFICANCE AND USE
3.1 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 %.  
1.2 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

• Status: Historical
• Publication Date: 31-Oct-2017
• 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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D6505 − 00 (Reapproved 2017)
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 4.5 Crimp Top Vials—Hewlett Packard 2-mL glass crimp
top vials withTFE-fluorocarbon-lined silicone septa or equiva-
1.1 This test method provides a basis for the determination
lent.
of the normal-propyl bromide (weight %) in the presence of
4.6 Volumetric Pipet—25 mL.
stabilizersandimpurities,invirginorreclaimednormal-propyl
bromide (nPB). The application range is from 50 to 100 wt %.
4.7 Glass Vials—32–mL glass vials (25 by 95 mm), with
1.2 This international standard was developed in accor- TFE-fluorocarbon-lined screw caps.
dance with internationally recognized principles on standard-
4.8 Transfer Pipets—Borosilicate glass transfer pipets.
ization established in the Decision on Principles for the
4.9 Precision Balance, accurate to 0.1 mg.
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
5. Required Chemicals
Barriers to Trade (TBT) Committee.
5.1 n-Propyl Bromide (1-Bromopropane), 99+ %, Aldrich
Chemical Company
2. Summary of Test Method
5.2 n-Heptane (internal standard), Reagent Grade, 99.5+ %,
2.1 This analytical test method describes the determination
J.T. Baker (or equivalent)
of the assay of n-propyl bromide by gas chromatography using
an internal standard.The results are reported in weight percent.
5.3 Methylene Chloride, 99+ %, Aldrich Chemical Com-
pany (or equivalent)
3. Significance and Use
6. Suggested Analysis Conditions
3.1 This test method provides an analysis in weight percent
6.1 Chromatographic Conditions:
of the normal-propyl bromide concentration of virgin,
Injector 150 °C
formulated, or reclaimed normal-propyl bromide: compounds
that co-elute with normal-propyl bromide or normal-heptane
Detector temperature 250 °C
(internal standard) may interfere with this test method.
FID detector range most sensitive setting
4. Apparatus
Temperature 30 °C for 10 min
program 30 to 250 °C at 15 °C ⁄min
4.1 Gas Chromatograph—Hewlett Packard 5890 Series II
hold at 250 °C for 10 min
equipped with a split/splitless injector, a flame ionization
detector, and an autosampler, HP, or equivalent, if available. Carrier gas He (or N ) at 1 mL/min
split flow: 25 mL/min
4.2 Column—30 m by 0.25 mm, 1.0-µm film thickness
column head pressure: 7.5 psi
AllTech AT-5, or equivalent, capillary column.
Make-up gas He (or N ) at 30 mL/min
4.3 Syringe—5-µL or 10-µL GC autosampler syringe.
Injection volume 0.5 µL
4.4 Data Acquisition and Analysis Device—VAX MULTI-
7. Analytical Procedure
CHROM or equivalent chromatography data collection and
processing system, or integrator.
7.1 Internal Standard Calibration Mixture—Carefully
weigh about 0.25 g of n-heptane internal standard and about
0.5gof n-propyl bromide into a 32-mL glass vial. Record the
actualweightsforeach.Pipet25mLofmethylenechlorideinto
This test method is under the jurisdiction of ASTM Committee D26 on
Halogenated Organic Solvents and Fire Extinguishing Agents and is the direct
this vial and cap immediately. Mix well and then transfer
responsibility of Subcommittee D26.04 on Test Methods.
approximately 1 mL of this standard solution into an autosam-
Current edition approved Nov. 1, 2017. Published December 2017. Originally
pler vial. Cap the vial and analyze in accordance with the
approved in 2000. Last previous edition approved in 2012 as D6505–00 (2012).
DOI: 10.1520/D6505-00R17. conditions specified in the chromatographic conditions section.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D6505 − 00 (2017)
Inject this standard at least three times and calibrate an internal
Wtl = amount of n-heptane (internal standard) in standard
standard method in the data system using the results from the
calibration mixture.
standard analyses.
The
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This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D6505 − 00 (Reapproved 2012) D6505 − 00 (Reapproved 2017)
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
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 %.
1.2 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Summary of Test Method
2.1 This analytical test method describes the determination of the assay of n-propyl bromide by gas chromatography using an
internal standard. The results are reported in weight percent.
3. Significance and Use
3.1 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.
4. Apparatus
4.1 Gas Chromatograph—Hewlett Packard 5890 Series II equipped with a split/splitless injector, a flame ionization detector,
and an autosampler, HP, or equivalent, if available.
4.2 Column—30 m by 0.25 mm, 1.0-μm film thickness AllTech AT-5, or equivalent, capillary column.
4.3 Syringe—5-μL or 10-μL GC autosampler syringe.
4.4 Data Acquisition and Analysis Device—VAX MULTICHROM or equivalent chromatography data collection and processing
system, or integrator.
4.5 Crimp Top Vials—Hewlett Packard 2-mL glass crimp top vials with TFE-fluorocarbon-lined silicone septa or equivalent.
4.6 Volumetric Pipet—25 mL.
4.7 Glass Vials—32–mL glass vials (25 by 95 mm), with TFE-fluorocarbon-lined screw caps.
4.8 Transfer Pipets—Borosilicate glass transfer pipets.
4.9 Precision Balance, accurate to 0.1 mg.
5. Required Chemicals
5.1 n-Propyl Bromide (1-Bromopropane), 99+ %, Aldrich Chemical Company
5.2 n-Heptane (internal standard), Reagent Grade, 99.5+ %, J.T. Baker (or equivalent)
5.3 Methylene Chloride, 99+ %, Aldrich Chemical Company (or equivalent)
This test method is under the jurisdiction of ASTM Committee D26 on Halogenated Organic Solvents and Fire Extinguishing Agents and is the direct responsibility of
Subcommittee D26.04 on Test Methods.
Current edition approved March 1, 2012Nov. 1, 2017. Published June 2012December 2017. Originally publishedapproved in 2000. Last previous edition approved in
20062012 as D6505–00 (2006).(2012). DOI: 10.1520/D6505-00R12.10.1520/D6505-00R17.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D6505 − 00 (2017)
6. Suggested Analysis Conditions
6.1 Chromatographic Conditions:
Injector 150°C
Injector 150 °C
Detector temperature 250°C
Detector temperature 250 °C
FID detector range most sensitive setting
Temperature 30°C for 10 min
program 30 to 250°C at 15°C/min
hold at 250°C for 10 min
Temperature 30 °C for 10 min
program 30 to 250 °C at 15 °C ⁄min
hold at 250 °C for 10 min
Carrier gas He (or N ) at 1 mL/min
split flow: 25 mL/min
column head pressure: 7.5 psi
Make-up gas He (or N ) at 30 mL/min
Injection volume 0.5 μL
7. Analytical Procedure
7.1 Internal Standard Calibration Mixture—Carefully weigh about 0.25 g of n-heptane internal standard and about 0.5 g of
n-propyl bromide into a 32-mL glass vial. Record the actual weights for each. Pipet 25 mL of methylene chloride into this vial
and cap immediately. Mix well and then transfer approximately 1 mL of this standard solution into an autosampler vial. Cap the
vial and analyze in accordance with the conditions specified in the chromatographic conditions section. Inject this standard at leas
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