1、Designation: D5632/D5632M 17Standard Specification forHalon 1301, Bromotrifluoromethane (CF3Br)1This standard is issued under the fixed designation D5632/D5632M; the number immediately following the designation indicates theyear of original adoption or, in the case of revision, the year of last revi
2、sion. A number in parentheses indicates the year of lastreapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the U.S. Department of Defense.1. Scope1.1 This specification covers the requirement
3、s for Halon1301 as a fire-fighting medium.1.2 This specification does not address the fire-fightingequipment or hardware that employs Halon 1301 or theconditions of employing such equipment (for example,handhelds, fixed installations, etc.).1.3 This specification does not address the storage ortrans
4、portation of Halon 1301. Storage, handling, and transpor-tation issues are addressed in Practice D5631.1.4 The values stated in either SI units or inch-pound unitsare to be regarded separately as standard. The values stated ineach system may not be exact equivalents; therefore, eachsystem shall be u
5、sed independently of the other. Combiningvalues from the two systems may result in non-conformancewith the standard.1.5 The following safety hazards caveat pertains only to thetest methods portion, Section 6, of this specification: Thisstandard does not purport to address all of the safety concerns,
6、if any, associated with its use. It is the responsibility of the userof this standard to establish appropriate safety and healthpractices and determine the applicability of regulatory limita-tions prior to use. Specific hazards statements are given in 4.5.1.6 This international standard was develope
7、d in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documen
8、ts2.1 ASTM Standards:2D2108 Test Method for Color of Halogenated OrganicSolvents and Their Admixtures (Platinum-Cobalt Scale)D5631 Practice for Handling, Transportation, and Storage ofHalon 1301, Bromotrifluoromethane (CF3Br)2.2 ISO Standard:3ISO 3427 Gaseous Halogenated Hydrocarbons (LiquefiedGases
9、)Taking of a Sample2.3 AHRI Standard:42008 Appendix C for Analytical Procedures for AHRIStandard 700-20142.4 U.S. Government Standard:5CFR Title 49, Part 172 U.S. DOT Hazardous MaterialsTable, Special Provisions, Hazardous MaterialsCommunications, Emergency Response Information, andTraining Requirem
10、ents3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 Halon 1301The halogenated hydrocarbon com-pound Bromotrifluoromethane used as a fire extinguishingmedium.3.1.1.1 DiscussionThe halon terminology system pro-vides a convenient means to reference halogenated hydrocar-bon fire e
11、xtinguishants. Halogenated hydrocarbons are acyclicsaturated hydrocarbons in which one or more of the hydrogenatoms have been replaced by atoms from the halogen series(that is, fluorine, chlorine, bromine, and iodine). By definition,the first digit of the halon numbering system represents thenumber
12、of carbon atoms in the compound molecule; the seconddigit, the number of fluorine atoms; the third digit, the numberof chlorine atoms; the fourth digit, the number of bromine1This specification is under the jurisdiction of ASTM Committee D26 onHalogenated Organic Solvents and Fire Extinguishing Agen
13、ts, and is the directresponsibility of Subcommittee D26.09 on Fire Extinguishing Agents.Current edition approved May 1, 2017. Published May 2017. Originallyapproved in 1994. Last previous edition approved in 2012 as D5632/D5632M-121.DOI: 10.1520/D5632_D5632M-17.2For referenced ASTM standards, visit
14、the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, N
15、Y 10036, http:/www.ansi.org.4Available from Air-Conditioning, Heating, and Refrigeration Institute (AHRI),2111 Wilson Blvd, Suite 500, Arlington, VA 22201, http:/www.ahrinet.org.5Available from U.S. Government Publishing Office (GPO), 732 N. CapitolStreet, NW, Washington, DC 20401-0001, http:/www.gp
16、o.gov.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of
17、 International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.1atoms; and the fifth digit, the number of iodine atoms. Trailingzeros are not expressed. Unaccounted for valence requirementsare assumed to be hydrogen atoms.numbe
18、r of hydrogen atoms5 (1)number of carbon atoms 32!12! 2 sum of halogen atoms!#For example, (2)bromotrifluoromethane 2 CF3Br 2 Halon 13013.1.2 non-condensable gasesnon-condensable gases con-sist primarily of air (nitrogen, oxygen) accumulated in thevapor phase of a liquefied compressed gas where the
19、solubilityof air in the liquid phase is extremely low and air is notsignificant as a liquid phase contaminant. Non-condensablegases are in some instances termed non-absorbable gases.4. Material Requirements4.1 Type IMixtures of Halon 1301 and nitrogen:4.1.1 The nitrogen (N2) partial pressure shall b
20、e such thatthe safe working pressure of the receiving vessel is notexceeded. To prevent excessive pressure, the fill density of theHalon 1301 within a container should not exceed that neededto achieve complete filling of the container at the maximumenvisaged storage temperature. For example, for a U
21、.S. DOT4BA 500 cylinder, the nitrogen partial pressure shall notexceed 161 psi at 70 F 12.1 bar at 21 C for a 70 lb/ft31121kg/m3 fill density, which yields a total pressure of 360 psig at70 F 25.8 bar at 21 C. For this example, the safe workingpressure of the 4BA500 cylinder is not exceeded for temp
22、era-tures below 130 F 54 C. (See Practice D5631.) (See Fig. 1.)4.1.2 Halon 1301 shall conform to the requirements pre-scribed in Table 1 when tested by the appropriate test meth-od(s) listed in Section 6.4.1.3 When a material analysis is required, by agreementbetween the purchaser and the supplier,
23、the total pressure in theHalon 1301 container, partial pressure of the N2, the fill densityof the Halon 1301 within the container, and the maximum safestorage temperature shall be part of the material analysis(certification). The pressure shall be reported in pound-forceper square inch gauge (prefer
24、red) or bar. The fill density shallbe reported in pounds per cubic foot at 70 F (preferred) orkilograms per cubic metre at 21 C. The maximum safe storagetemperature of the Halon 1301 container shall be reported indegrees Fahrenheit (preferred) or in degrees Celsius and shallconform to applicable reg
25、ulations for the Halon 1301 containerdesign and use.4.2 Type IIHalon 1301 shall conform to the requirementsof Type I, as listed in 4.1, and shall contain no more than 1.5 %by volume non-condensable gases in the vapor phase, ex-pressed as air when tested by the appropriate test method(s)listed in Sec
26、tion 6.4.3 By agreement between the purchaser and the supplier,analysis may be required and limits established for elements orcompounds not specified in Table 1.4.4 Unless otherwise specified, Type I is assumed.FIG. 1 Isometric Diagram for BromotrifluoromethaneD5632/D5632M 1724.5 WarningExposure to
27、concentrations of Halon 1301in excess of 7.5 % by volume in air during periods of elevatedadrenaline could produce cardiac arrhythmia in some person-nel.5. Sampling5.1 Samples of Halon 1301 shall be taken from the liquid orvapor phase as appropriate. Samples of Halon 1301, taken fromthe liquid phase
28、, shall be taken from filled containers inaccordance with the method specified in ISO 3427 or themethod specified in 2008 Appendix C for Analytical Proce-dures for AHRI Standard 700-2014, Part 7.5.1.1 The sampling bottle shall be capable of safely resist-ing the vapor pressure of the sample at the h
29、ighest temperaturethat could be encountered during handling, storage, or trans-port. (See Practice D5631.)5.2 The Halon 1301 selected in accordance with 5.1 shall betested for quality conformance in accordance with Section 6.The presence of one or more defects shall be cause forrejection.6. Test Met
30、hods6.1 PurityDetermine the purity by gas chromatography inaccordance with the technique described in 6.1.1 6.1.1.6 orby gas chromatography/mass spectrometry (GC/MS) in accor-dance with 6.1.2 6.1.2.5.6.1.1 Purity by GC:6.1.1.1 Prior to sample introduction, a standardization of theGC shall be perform
31、ed using a known bromotrifluoromethanepurity standard.6.1.1.2 ApparatusThe following special apparatus is re-quired to determine the percent of Halon 1301 by GC:(a) Gas Chromatograph System (GC System), equippedwith a flame ionization detector (FID), capillary column splitinjector, subambient (liqui
32、d nitrogen) cooling valve, and anelectronic integrator or suitable computer data gathering andreduction system.(b) 210 m Chromatographic ColumnConnect the twocolumns below together with the first column end attached tothe injection port:(1) 105 m Rtx6-1701 (14 % cyanopropylphenyl 86 %methylpolysilox
33、ane), 0.25 mm, 1m.(2) 105 m Rtx6-200 (5 % diphenyl 95 % dimethylpolysiloxane), 0.25 mm, 1m.(3) The two columns are attached together, with the first(Column 1) attached to the injection port of the GC system.Columns are available from several chromatographic supplyvendors.6.1.1.3 Sample IntroductionT
34、ake sample from the liquidphase employing the procedure described in 5.1 of thisspecification. Introduce and transfer the sample into the GCusing a standard gas-tight syringe.6.1.1.4 ReagentsThe carrier gas shall be a chromato-graphic grade of helium.6.1.1.5 Temperature Programming:(a) Install the c
35、olumn in the gas chromatograph and adjustthe oven temperature to -20 C. Inject the sample and hold thecolumn oven at -20 C for 21 min, then program the tempera-ture to rise 15 C min to a maximum of 165 C, then post holdfor 20 min before recycling.6.1.1.6 Calculation:(a) Calculate weight percent of H
36、alon 1301 as follows, andconvert it to mole percent in 6.1.1.6(b) if necessary.Wi5Ai3RRFi3100(Ai3RRFi#(3)where:Wi= weight percent of component i,Ai= peak area of component i,RRFi= relative response factor for component i,andAi RRFi = sum of all component peak areas times theirrespective relative res
37、ponse factors.(b) For ASTM specifications, the results shall be convertedto and reported in mole percentages. Convert individualimpurities from wt % to mol % as follows:mol %i5 100 3 Wi/Mi!/(Wi/Mi# (4)where:mol %i= mol percent of component i,Wi= weight percent of component i,Mi= molecular weight of
38、component i, andWi/Mi = sum of all component weights divided by theirrespective molecular weights.NOTE 1The GC method described in 6.1.1 6.1.1.6 may not detectcertain impurities, for example, impurities that may elute within or nearthe relatively large Halon 1301 peak. If other tests indicate the pr
39、esence ofunidentified impurities, then the gas chromatography/mass spectrometry(GC/MS) method described in 6.1.2 is recommended.6.1.2 Purity by GC/MS:6.1.2.1 Prior to sample introduction, a standardization of theGC/MS shall be performed using a known bromotrifluo-romethane purity standard.6.1.2.2 Ap
40、paratusThe following special apparatus is re-quired to determine the percent of Halon 1301:(a) Gas Chromatography/Mass Spectrometry System(GC/MS System) and an electronic integrator or suitablecomputer data-gathering and reduction system.(b) Chromatographic Column, 344 ft 105 m Rtx6-1capillary colum
41、n, 0.01 in. 0.25 mm internal diameter, station-ary film thickness of approximately 1 m. (Column is availablefrom several chromatographic supply vendors.)6Rtx is a registered trademark of Restek Corporation.TABLE 1 RequirementsProperty RequirementHalon 1301 purity, %, mol/mol, min 99.6 (exclusive of
42、any N2present)Acidity, ppm by mass, as Hbr, max 3.0Water content, ppm by mass, max 10Nonvolatile residue, % by weight, max 0.01Halogen ion Passes testSuspended matter or sediment None visibleColor Report valueD5632/D5632M 173(c) Sample IntroductionTake sample from the liquidphase employing the proce
43、dure described in 5.1. Using astandard gas-tight syringe introduce the sample into the GC/MS.6.1.2.3 ReagentsThe carrier gas shall be a chromato-graphic grade of helium.6.1.2.4 Temperature Programming:(a) Install the column in the gas chromatograph/massspectrometer and adjust the oven temperature to
44、 -30 C. Injectthe sample and hold the column oven at -30 C for 13 min, thenprogram the temperature to rise 10 C min to a maximum of200 C, then posthold for 10 min before recycling.6.1.2.5 Calculation:(a) Calculate weight percent of Halon 1301 as follows, andconvert it to mol percent in 6.1.2.5(b) if
45、 necessary:Wi5Ai3RRFi3100(Ai3RRFi#(5)where:Wi= weight percent of component i,Ai= peak area of component i,RRFi= relative response factor for component i,andAi RRFi = sum of all component peak areas times theirrespective relative response factors.(b) ForASTM specifications, the results shall be conve
46、rtedto and reported in mole percentages. Convert individualimpurities from wt % to mol % as follows:mol %i5 100 3 Wi/Mi!/(Wi/Mi# (6)where:mol %i= mole percent of component i,Wi= weight percent of component i,Mi= molecular weight of component i, andWi/Mi = sum of all component weights divided by thei
47、rrespective molecular weights.6.2 AcidityDetermine acidity using the method specifiedin 2008 Appendix C to AHRI Standard 700-2014, Part 1.6.3 Water ContentDetermine water content using themethod specified in 2008 Appendix C to AHRI Standard700-2014, Part 2.6.4 Qualitative Test for Halogen IonTest a
48、sample for thepresence of halogen ions in accordance with 6.4.1 6.4.2 or byanother acceptable laboratory technique providing equivalentresults. Generally, a sample treated with an alcoholic solutionof silver nitrate shall exhibit no turbidity or precipitation ofsilver halide.6.4.1 Reagents:6.4.1.1 3
49、M Silver Nitrate SolutionDissolve 5.1 g of anhy-drous silver nitrate in DI water to give a total volume of 10.0mL. Store in a brown glass bottle away from light.6.4.1.2 Nitric Acid, 1:1 v/v in water.6.4.2 ProcedureTo the water scrubber solution savedduring the acidity test (6.2), add 1 drop of 1:1 HNO3, swirl tomix. Then add 3 to 4 drops of 3M silver nitrate solution andswirl to mix. The appearance of any haze or turbidity shallconstitute failure of this test.6.5 Nonvolatile ResidueDetermi
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