ASTM D6505-00 pdf download.Standard Test Method for Assay of normal-Propyl Bromide Content.
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 accor- dance with internationally recognized principles on standard- ization established in the Decision on Principles for the Development of International Standards, Guides and Recom- mendations 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 MULTI- CHROM 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 equiva- lent.
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 Com- pany (or equivalent)
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 mLofmethylene chloride into this vial and cap immediately. Mix well and then transfer approximately 1 mL of this standard solution into an autosam- pler vial. Cap the vial and analyze in accordance with the conditions specified in the chromatographic conditions section.
Inject this standard at least three times and calibrate an internal standard method in the data system using the results from the standard analyses. 7.2 Preparation ofSamples for Analysis—Weigh about 0.25 g of 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 methylene chloride into this vial and cap immediately. Mix well and transfer approximately 1 mL of this solution to an autosampler vial. Cap the vial and analyze in accordance with the conditions specified in the chromatographic conditions section. The following table shows components of interest, their absolute retention time (ART) in minutes, their relative retention time (RRT) in relation to n-heptane, the internal standard, as well as their relative response factor (RRf).ASTM D6505 pdf download.