1、Designation: D 6505 00 (Reapproved 2006)Standard Test Method forAssay of normal-Propyl Bromide Content1This standard is issued under the fixed designation D 6505; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last rev
2、ision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) 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
3、and 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 report
4、ed 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 i
5、nterfere 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, capillar
6、y 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 silicone septa or e
7、quiva-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
8、 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 150CDetector temperature 250CFID detector range most sensitive s
9、ettingTemperature 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 MixtureCarefullywe
10、igh 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
11、vial. 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 Analysi
12、sWeigh 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 accorda
13、nce with1This 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 Jan. 1, 2006. Published February 2006. Originallypublished in 2000. L
14、ast previous edition approved in 2000 as D 650500.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.the conditions specified in the chromatographic conditionssection. The following table shows components of interest,their absolute rete
15、ntion 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. Calculation8.1 A calibrated interna
16、l 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 standard relative to the n-hept
17、ane 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 = amount of n-propyl bromi
18、de 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 = area of n-propyl bromide
19、 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 criteria should be used
20、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 Precision (Within-Laboratories, B
21、etweenDays 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 % absolute.9.1.3 Reprodu
22、cibility, 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. Keywords10.1 assay; brominated; gas
23、 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 determination of the validity of any
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26、 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 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).D 6505 00 (2006)2
