1、Designation: D5632/D5632M 121Standard 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 rev
2、ision. 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 Department of Defense.1NOTEDesignation was corrected editorially in October 201
3、3.1. Scope1.1 This specification covers the requirements 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
4、This specification does not address the storage ortransportation of Halon 1301. Storage, handling, and transpor-tation issues are addressed in Practice D5631.1.4 The values stated in both inch-pound and SI units are tobe regarded separately as the standard. The values given inparentheses are mathema
5、tical conversions that are provided forinformation only.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,if any, associated with its use. It is the responsibility of
6、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 4.5.2. Referenced Documents2.1 ASTM Standards:2D5631 Practice for Handling, Transportation, and Storage ofHalo
7、n 1301, Bromotrifluoromethane (CF3Br)2.2 ISO Standards:3ISO 3427 Gaseous Halogenated Hydrocarbons (LiquefiedGases)Taking of a Sample2.3 AHRI Standards:42008 Appendix C for Analytical Procedures for AHRIStandard 700-20062.4 U.S. Government Standards:5CFR Title 49, Part 172.101 Tables of Hazardous Mat
8、erialsand Special ProvisionsCFR Title 49, Part 172 Subpart D Marking Requirements ofPackaging for Transportation3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 Halon 1301 The halogenated hydrocarbon com-pound Bromotrifluoromethane used as a fire extinguishingmedium.3.1.1.1 Dis
9、cussionThe halon terminology system pro-vides a convenient means to reference halogenated hydrocar-bon fire extinguishants. 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, chlo
10、rine, bromine, and iodine). By definition,the first digit of the halon numbering system represents thenumber 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 bromineatoms; and the fi
11、fth digit, the number of iodine atoms. Trailingzeros are not expressed. Unaccounted for valence requirementsare assumed to be hydrogen atoms.number 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-condensa
12、ble gases non-condensable gasesconsist primarily of air (nitrogen, oxygen) accumulated in the1This specification is under the jurisdiction of ASTM Committee D26 onHalogenated Organic Solvents and Fire Extinguishing Agents, and is the directresponsibility of Subcommittee D26.09 on Fire Extinguishing
13、Agents.Current edition approved March 1, 2012. Published April 2012. Originallyapproved in 1994. Last previous edition approved in 2008 as D5632 - 08. DOI:10.1520/D5632-12E01.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For
14、 Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from American National Standards Institute, 11 W. 42nd St., 13thFloor, New York, NY 10036.4Available from Air-Conditioning, Heating, and Refrigeration Institute, 2111Wilson Bl
15、vd, Suite 500, Arlington, VA 22201.5Available from Superintendent of Documents, U.S. Government PrintingOffice, Washington, DC 20036.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1vapor phase of a liquefied compressed gas where the s
16、olubilityof 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 be
17、 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.
18、S. DOT4BA 500 cylinder, the nitrogen partial pressure shall notexceed 161 psi at 70F (12.1 bar at 21C) for a 70 lb/ft3(1121kg/m3) fill density, which yields a total pressure of 360 psig at70F (25.8 bar at 21C). For this example, the safe workingpressure of the 4BA500 cylinder is not exceeded for tem
19、pera-tures below 130F (54C).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, the total pressure in theHalon 1301
20、 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 (preferred) or bar. The fill density shall
21、be reported in pounds per cubic foot at 70F (preferred) orkilograms per cubic metre at 21C. The maximum safe storagetemperature of the Halon 1301 container shall be reported indegrees Fahrenheit (preferred) or in degrees Celsius and shallconform to applicable regulations for the Halon 1301 container
22、design 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 vapor phase, expressed asnitrogen when tested by the appropriate test method(s) listed inSection 6.4.3 By agreement between the pu
23、rchaser 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.4.5 WarningExposure to concentrations of Halon 1301in excess of 7.5 % by volume in air during periods of elevatedadrenaline cou
24、ld 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, shall be taken from filled containers inaccordance with the method specified in ISO 3427 or themethod
25、specified in 2008 Appendix C for Analytical Proce-dures for AHRI Standard 700-2006, Part 7.5.1.1 The sampling bottle shall be capable of safely resist-ing the vapor pressure of the sample at the highest temperaturethat could be encountered during handling, storage, or trans-port.5.2 The Halon 1301 s
26、elected 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 Methods6.1 PurityDetermine the purity by gas chromatography inaccordance with the technique described in 6.1.1-6.1.1.6 or bygas c
27、hromatography/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 performed using a known bromotrifluoromethanepurity standard.6.1.1.2 ApparatusThe following special apparatus is re-quired to determi
28、ne the percent of Halon 1301 by GC:(a)Gas Chromatograph System (GC System), equipped witha flame ionization detector (FID), capillary column splitinjector, subambient (liquid nitrogen) cooling valve, and anelectronic integrator or suitable computer data gathering andreduction system.(b)210 m Chromat
29、ographic ColumnConnect the two col-umns below together with the first column end attached to theinjection port:(1) 105 m RTx-1701 (14 % cyanopropylphenyl 86 %methylpolysiloxane), 0.25 mm, 1m.(2) 105 m RTx-200 (5 % diphenyl 95 % dimethylpolysiloxane), 0.25 mm, 1m.(3) The two columns are attached toge
30、ther, 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 IntroductionTake sample from the liquidphase employing the procedure described in 5.1 of thisspecification. Introduce and transfer the sample
31、 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 column in the gas chromatograph and adjustthe oven temperature to -20 C. Inject the sample and hold thecolumn oven at -20C for 21
32、 min, then program the tempera-ture to rise 15C/min to a maximum of 165C, then postholdfor 20 min before recycling.6.1.1.6 Calculation:(a) Calculate weight percent of Halon 1301 as follows, andconvert it to mole percent in 6.1.1.6(b) if necessary.TABLE 1 RequirementsProperty RequirementHalon 1301 pu
33、rity, %, mol/mol, min 99.6 (exclusive of 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 visibleD5632/D5632M 1212Wi5Ai3RRFi3100(Ai3RRFi#(3)where:Wi= weight percent
34、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) For ASTM specifications, the results shall be convertedto and reported in mole percentages. Convert individualim
35、purities from wt % to mol % as follows:mol %i5 100 3 Wi/Mi!/(Wi/Mi# (4)mol %i= mol 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 theirrespective molecular weights.NOTE 1The GC method described in 6.1.1
36、-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 presence ofunidentified impurities, then the gas chromatography/mass spectrometry(GC/MS) method described in 6.1.2 is recommended.6.1.2 Pu
37、rity 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 ApparatusThe following special apparatus is re-quired to determine the percent of Halon 1301:(a)Gas Chromatography/Mass Spectrometry Syste
38、m(GC/MS System) and an electronic integrator or suitablecomputer data-gathering and reduction system.(b)Chromatographic Column, 344 ft (105 m) Rtx-1 capil-lary column, 0.01 in. (0.25 mm) internal diameter, stationaryfilm thickness of approximately 1 m. (Column is availablefrom several chromatographi
39、c supply vendors.)(c)Sample IntroductionTake sample from the liquid phaseemploying the procedure described in 5.1. Using a standardgas-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) Ins
40、tall the column in the gas chromatograph/mass spec-trometer and adjust the oven temperature to -30C. Inject thesample and hold the column oven at -30C for 13 min, thenprogram the temperature to rise 10C/min to a maximum of200C, then posthold for 10 min before recycling.6.1.2.5 Calculation:(a) Calcul
41、ate weight percent of Halon 1301 as follows, andconvert it to mol percent in 6.1.2.5(b) if 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 timestheir r
42、espective relative response 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# (6)where:mol %i= mole percent of component i,Wi= weight percent of component i,M
43、i= molecular weight of component i, andWi/Mi = sum of all component weights divided bytheir respective molecular weights.6.2 AcidityDetermine acidity using the method specifiedin 2008 Appendix C to AHRI Standard 700-2006, Part 1.6.3 Water ContentDetermine water content using themethod specified in 2
44、008 Appendix C to AHRI Standard700-2006, Part 2.6.4 Qualitative Test for Halogen IonTest a 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 n
45、itrate shall exhibit no turbidity or precipitation ofsilver halide.6.4.1 Reagents:6.4.1.1 3M 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 Proc
46、edureTo 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 ResidueDetermine the nonvolat
47、ile residuein accordance with the gravimetric method specified in 2008Appendix C to AHRI Standard 700-2006, Part 3.6.6 Non-Condensable GasesDetermine non-condensablegases using the method specified in 2008 Appendix C to AHRIStandard 700-2006, Part 4.6.7 Suspended Matter and SedimentWhile performing
48、thenonvolatile residue analysis, examine visually for any sus-pended matter or sediment. Observation of any suspendedmatter or sediment shall constitute failure of this test.7. Container, Packaging, and Package Marking7.1 Containers used for shipping and storage of Halon 1301conforming to this speci
49、fication shall be marked in accordanceto Code of Federal Regulations CFR Title 49, Part 172 SubpartD “Marking Requirements of Packaging for Transportation”.The proper shipping name for ASTM D5632 Type II (pure)Halon 1301 is “Bromotrifluoromethane (Refrigerant Gas R13B1),” UN 1009, Hazard Class 2.2 (nonflammable gas). Theproper shipping name for nitrogen superpressurized HalonD5632/D5632M 12131301 is “Liquefied Gas, nonflammable charged with nitrogen,”UN1058, Hazard Class 2.2. In addition to DOT requiremen
