ASTM D6505-2000(2012) 6875 Standard Test Method for Assay of normal-Propyl Bromide Content《检定正丙基溴含量的标准试验方法》.pdf

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1、Designation: D6505 00 (Reapproved 2012)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 %.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. The results are reported

4、in weight percent.3. Significance and Use3.1 This test method provides an analysis in weight percentof the normal-propyl bromide concentration of virgin, formu-lated, or reclaimed normal-propyl bromide: compounds thatco-elute with normal-propyl bromide or normal-heptane (in-ternal standard) may inte

5、rfere 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 equivalent, capillary c

6、olumn.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 silicone septa or equi

7、va-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+ %, AldrichChemical Co

8、mpany5.2 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 150CDetector temperature 250CFID detector range most sensitive sett

9、ingTemperature pro-gram30C for 10 min30 to 250C at 15C/minhold at 250C 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 Calibration MixtureCarefullyweigh

10、 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 into an autosam-pler via

11、l. Cap the vial and analyze in accordance with theconditions specified in the chromatographic conditions section.Inject 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 AnalysisWe

12、igh about 0.25gofn-heptane and about 0.5 g of sample into a 32-mL glassvial. 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

13、 withthe conditions specified in the chromatographic conditions1This test method is under the jurisdiction of ASTM Committee D26 onHalogenated Organic Solvents and Fire Extinguishing Agents and is the directresponsibility of Subcommittee D26.04 on Test Methods.Current edition approved March 1, 2012.

14、 Published June 2012. Originallypublished in 2000. Last previous edition approved in 2006 as D650500 (2006).DOI: 10.1520/D6505-00R12.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.section. The following table shows components of int

15、erest,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 standard) 16.08 1.00 1.00008. Calculatio

16、n8.1 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 factor (RRf) for n-propylbromide in the standa

17、rd relative to the n-heptane internalstandard. Average the peak areas of the three standard injec-tions:RRf 5Ay 3 WtlWty 3 Al(1)where:Ay = average area of n-propyl bromide peak in standardcalibration mixture,Al = average area of n-heptane (internal standard) peak instandard calibration mixture,Wty =

18、 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 3 Wtl 3 100Al 3 RRf 3 WtS(2)where:Ay =

19、 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 and Bias9.1 PrecisionThe following

20、 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 % absolute.9.1.2 Laboratory Precisio

21、n (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 differencebetween 2 such runs is 1.72

22、 % 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 runs is 2.39 % absolute.10. Keywords10

23、.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 expressly advised that determinatio

24、n of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdra

25、wn. 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 may attend. If you feel that your c

26、omments 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 States. Individual reprints (single

27、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 ASTM website (www.astm.org/COPYRIGHT/).D6505 00 (2012)2