1、Designation: D6505 00 (Reapproved 2017)Standard Test Method forAssay of normal-Propyl Bromide Content1This standard is issued under the fixed designation D6505; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revis
2、ion. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method provides a basis for the determinationof the normal-propyl bromide (weight %) in the presence ofstabilizers and
3、 impurities, in virgin or reclaimed normal-propylbromide (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 theDevelopment of Int
4、ernational Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Summary of Test Method2.1 This analytical test method describes the determinationof the assay of n-propyl bromide by gas chromatography usingan internal standard. Th
5、e results are reported in weight percent.3. Significance and Use3.1 This test method provides an analysis in weight percentof the normal-propyl bromide concentration of virgin,formulated, or reclaimed normal-propyl bromide: compoundsthat co-elute with normal-propyl bromide or normal-heptane(internal
6、 standard) may interfere with this test method.4. Apparatus4.1 Gas ChromatographHewlett Packard 5890 Series IIequipped with a split/splitless injector, a flame ionizationdetector, and an autosampler, HP, or equivalent, if available.4.2 Column30 m by 0.25 mm, 1.0-m film thicknessAllTech AT-5, or equi
7、valent, capillary column.4.3 Syringe5-L or 10-L GC autosampler syringe.4.4 Data Acquisition and Analysis DeviceVAX MULTI-CHROM or equivalent chromatography data collection andprocessing system, or integrator.4.5 Crimp Top VialsHewlett Packard 2-mL glass crimptop vials with TFE-fluorocarbon-lined sil
8、icone septa or equiva-lent.4.6 Volumetric Pipet25 mL.4.7 Glass Vials32mL glass vials (25 by 95 mm), withTFE-fluorocarbon-lined screw caps.4.8 Transfer PipetsBorosilicate glass transfer pipets.4.9 Precision Balance, accurate to 0.1 mg.5. Required Chemicals5.1 n-Propyl Bromide (1-Bromopropane), 99+ %,
9、 AldrichChemical Company5.2 n-Heptane (internal standard), Reagent Grade, 99.5+ %,J.T. Baker (or equivalent)5.3 Methylene Chloride, 99+ %, Aldrich Chemical Com-pany (or equivalent)6. Suggested Analysis Conditions6.1 Chromatographic Conditions:Injector 150 CDetector temperature 250 CFID detector rang
10、e most sensitive settingTemperatureprogram30 C for 10 min30 to 250 C at 15 C minhold at 250 C for 10 minCarrier gas He (or N2) at 1 mL/minsplit flow: 25 mL/mincolumn head pressure: 7.5 psiMake-up gas He (or N2) at 30 mL/minInjection volume 0.5 L7. Analytical Procedure7.1 Internal Standard Calibratio
11、n MixtureCarefullyweigh about 0.25 g of n-heptane internal standard and about0.5gofn-propyl bromide into a 32-mL glass vial. Record theactual weights for each. Pipet 25 mLof methylene chloride intothis vial and cap immediately. Mix well and then transferapproximately 1 mL of this standard solution i
12、nto an autosam-pler vial. Cap the vial and analyze in accordance with theconditions specified in the chromatographic conditions section.1This test method is under the jurisdiction of ASTM Committee D26 onHalogenated Organic Solvents and Fire Extinguishing Agents and is the directresponsibility of Su
13、bcommittee D26.04 on Test Methods.Current edition approved Nov. 1, 2017. Published December 2017. Originallyapproved in 2000. Last previous edition approved in 2012 as D650500 (2012).DOI: 10.1520/D6505-00R17.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 1942
14、8-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Techni
15、cal Barriers to Trade (TBT) Committee.1Inject this standard at least three times and calibrate an internalstandard method in the data system using the results from thestandard analyses.7.2 Preparation of Samples for AnalysisWeigh about 0.25gofn-heptane and about 0.5 g of sample into a 32-mL glassvia
16、l. Record the actual weights for each. Pipet 25 mL ofmethylene chloride into this vial and cap immediately. Mixwell and transfer approximately 1 mL of this solution to anautosampler vial. Cap the vial and analyze in accordance withthe conditions specified in the chromatographic conditionssection. Th
17、e following table shows components of interest,their absolute retention time (ART) in minutes, their relativeretention time (RRT) in relation to n-heptane, the internalstandard, as well as their relative response factor (RRf).Component ART RRT RRfn-propyl bromide 13.30 0.83 0.3495n-heptane (internal
18、 standard) 16.08 1.00 1.00008. Calculation8.1 A calibrated internal standard weight percent method inthe data system will yield the required weight percent data.Alternatively, the weight percent calculations may be per-formed manually as described as follows:8.2 Calculate the relative response facto
19、r (RRf) for n-propylbromide in the standard relative to the n-heptane internalstandard. Average the peak areas of the three standard injec-tions:RRf 5Ay 3WtlWty 3Al(1)where:Ay = average area of n-propyl bromide peak in standardcalibration mixture,Al = average area of n-heptane (internal standard) pe
20、ak instandard calibration mixture,Wty = amount of n-propyl bromide in standard calibrationmixture, andWtl = amount of n-heptane (internal standard) in standardcalibration mixture.The assay of n-propyl bromide (weight % y) in the sample iscalculated as follows from the sample injection:weight % y 5Ay
21、 3Wtl 3100Al 3RRf 3WtS(2)where:Ay = area of n-propyl bromide peak in sample mixture,Al = area of n-heptane (internal standard) peak in samplemixture,Wtl = weight of internal standard in sample mixture,WtS = weight of sample in sample mixture, andRRf = relative response factor from above.9. Precision
22、 and Bias9.1 PrecisionThe following criteria should be used forjudging the acceptability of results:9.1.1 Repeatability (Single Analyst)The standard devia-tion for a single determination has been estimated to be0.037 % absolute at 22 df. The 95 % limit for the differencebetween 2 such runs is 0.10 %
23、 absolute.9.1.2 Laboratory Precision (Within-Laboratories, BetweenDays Variability, formerly called RepeatabilityThe standarddeviation of results (each the average of duplicates) obtainedby the same analyst on different days, has been estimated to be0.62 % absolute at 8 df. The 95 % limit for the di
24、fferencebetween 2 such runs is 1.72 % absolute.9.1.3 Reproducibility, MultilaboratoryThe standard de-viation of results (each the average of duplicates) obtained byanalysts at different laboratories, has been estimated to be0.93 % absolute at 7 df. The 95 % limit for the differencebetween 2 such run
25、s is 2.39 % absolute.10. Keywords10.1 assay; brominated; gas chromatography; halogenated;normal-propyl bromide; purity; solventASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are
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27、vised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee, which you
28、may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United S
29、tates. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ 00 (2017)2
