1、Designation: D 5632 08Standard Specification forHalon 1301, Bromotrifluoromethane (CF3Br)1This standard is issued under the fixed designation D 5632; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A numb
2、er in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the Department of Defense.1. Scope1.1 This specification covers the requirements for Halon1301
3、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, hand-helds, fixed installations, etc.).1.3 This specification does not address the storage ortransportation of H
4、alon 1301. Storage, handling, and transpor-tation issues are addressed in Practice D 5631.1.4 The values stated in inch-pound units are to be regardedas standard. The values in parentheses are for information only.1.5 The following safety hazards caveat pertains only to thetest methods portion, Sect
5、ion 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 the userof this standard to establish appropriate safety and healthpractices and determine the applicability of regulatory limita-tions prior
6、 to use. Specific hazards statements are given in 4.3.2. Referenced Documents2.1 ASTM Standards:2D 5631 Practice for Handling, Transportation, and Storageof Halon 1301, Bromotrifluoromethane (CF3BR)2.2 ISO Standards:3ISO 3363 Fluorochlorinated Hydrocarbons for IndustrialUseDetermination of AcidityTi
7、trimetric MethodISO 3427 Gaseous Halogenated Hydrocarbons (LiquefiedGases)Taking of a SampleISO 5789 Fluorinated Hydrocarbons for Industrial UseDetermination of Nonvolatile Residue2.3 U.S. Industry Standard:4ASQ Z1.4 Sampling Procedures and Tables for Inspectionby Attributes (ANSI Approved, DoD Adop
8、ted)3. 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
9、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
10、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 fifth digit, the number of iodine atoms. Trailingzeros are not expressed. Unaccounted for valence requirementsa
11、re assumed to be hydrogen atoms.number of hydrogen atoms 5number of carbon atoms3 2!12!2sum of halogen atoms!# (1)For example,bromotrifluoromethane 2 CF3Br 2 Halon 1301 (2)4. Material Requirements4.1 Type IMixtures of Halon 1301 and Nitrogen:4.1.1 The nitrogen (N2) partial pressure shall be such tha
12、tthe safe working pressure of the receiving vessel is notexceeded. To prevent excessive pressure, the fill density of thehalon within a container should not exceed that needed toachieve complete filling of the container at the maximumenvisaged storage temperature. For example, the U.S. DOT4BA 500 cy
13、linder partial pressure shall not exceed 161 psi at70F (12.1 bar at 21C) for a 70 lb/ft3(1121 kg/m3) fill density1This specification is under the jurisdiction of ASTM Committee D26 onHalogenated Organic Solvents and Fire Extinguishing Agents , and is the directresponsibility of Subcommittee D26.09 o
14、n Fire Extinguishing Agents.Current edition approved Jan. 1, 2008. Published January 2008. Originallyapproved in 1994. Last previous edition approved in 2001 as D 5632 01.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Ann
15、ual 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 Standardization Documents Order Desk, Bldg. 4 Section D, 100Robbins Ave.,
16、 Philadelphia, PA 191115904, Attn: NPODS.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.(yielding a total pressure of 360 psig at 70F (25.8 bar at21C). For this example, the safe working pressure of the4BA500 cylinder is not exceede
17、d for temperatures below130F (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 theHal
18、on 1301 container, partial pressure of the N2, the fill densityof the halon 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 gage (preferred) or bar. The fill density shal
19、l bereported 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 containe
20、rdesign 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 fixed gases in vapor phase, expressed as air whentested by the appropriate test method(s) listed in Section 6.4.3 By agreement between the purchaser and t
21、he supplier,analysis may be required and limits established for elements orcompounds not specified in Table 1. WarningExposure toconcentrations of Halon 1301 in excess of 7.5 % (halonvolume/air volume) during periods of elevated adrenalinecould produce cardiac arrhythmia in some personnel.4.4 Unless
22、 otherwise specified, Type I is assumed.5. Sampling5.1 Samples of halons shall be taken from the liquid orvapor phase as appropriate. Samples of halons, taken from theliquid phase, shall be taken from filled containers in accor-dance with the method specified in ISO 3427 or ASQ Z1.4,Inspection Level
23、 S-4. The sampling bottle shall be capable ofsafely resisting the vapor pressure of the sample at the highesttemperature that could be encountered during handling, stor-age, or transport.5.2 The Halon 1301 selected in accordance with 5.1 shall betested for quality conformance in accordance with Sect
24、ion 6.The presence of one or more defects shall be cause forrejection.6. Test Methods6.1 Purity:6.1.1 Determine the purity by gas-liquid chromatography inaccordance with the technique described in 6.1.2-6.1.5.6.1.1.1 Prior to sample introduction, a standardization of theGC must be performed using a
25、known bromotrifluoromethanepurity standard. The standardization must be performed asdescribed herein.6.1.2 ApparatusThe following special apparatus is re-quired to determine the percent of Halon 1301:6.1.2.1 Gas Chromatograph, equipped with a flame ioniza-tion detector (FID) and an electronic integr
26、ator or suitablecomputer data gathering and reduction system.6.1.2.2 Chromatographic Column, 7.34 m (24 ft) by18 in.(3.175 mm) outside diameter thin-wall stainless steel tubingpacked with Carbopack B, 60 to 80 mesh, containing 1 %SP1000 (also known as Carbowax 20M). (Column is available,prepacked, f
27、rom several chromatographic supply vendors.)6.1.2.3 Sample IntroductionTake sample from liquidphase and flash into evacuated 125-cc gas dispersion tubeequipped with side outlet tube and septum. Bring gas disper-sion tube to 1 atmosphere pressure. Using standard gas tightsyringe take14 to12 cc sample
28、 from gas dispersion tube andintroduce into GC.6.1.3 ReagentsThe carrier gas shall be a chromatographicgrade of helium. Column packing shall consist of 1 % SP1000(Carbowax 20M) weight/weight on Carbopack B, 60 to 80mesh.6.1.4 Procedure for Programmed Temperature Gas Chro-motography (PTGC):6.1.4.1 In
29、stall the column in the gas chromatograph andadjust the oven temperature to 40C. Adjust the helium carriergas flow rate to 30 cc per minute. Adjust injection porttemperature to 200C and the detector to 250C. Inject thesample and hold the column oven at 40C for six minutes, thenprogram the temperatur
30、e to rise 10C per minute to a maxi-mum of 180C, then posthold for 10 min before recycling.6.1.5 Calculation:6.1.5.1 Calculate weight percent and convert to mole per-cent Halon 1301 as follows:Wi5Ai3 RRFi3 100(Ai 3 RRFi#(3)where:Wi= weight percent of component iAi= peak area of component iRRFi= Relat
31、ive Response Factor for component i(Ai3 RRFi = sum of all component peak areas timestheir respective relative response factors.6.1.5.2 For ASTM specification, the results must be con-verted to and reported in mole percentages. Convert individualimpurities from Wt % to Mole % as follows:Mole %i5Wt %
32、3 148.9M(4)where:Wt %i= weight percent of component i149.8 = Molecular weight of Halon 1301M = Molecular weight of component i6.2 Methanol ImpurityThe methanol impurity may bedetermined using capillary column programmed temperaturegas chromatography. The column is 105 meter DB-1701 30.25 mm inside d
33、iameter. The presence of methanol may causeTABLE 1 RequirementsProperty RequirementHalon 1301 purity, %, mol/mol, min 99.6 (exclusive of any N2present)Acidity, ppm by mass, max 3.0Water content, ppm by mass, max 10Nonvolatile residue, % by weight, max 0.01Halogen ion Passes testSuspended matter or s
34、ediment None visibleD5632082inaccurate indication of other contaminants such as R115 andR22, possibly causing artificial enhancement of the R115/R22contaminant peaks when present.6.3 AcidityFrom the Halon 1301 liquid phase, vaporize alarge sample in the presence of distilled water. Determine theacid
35、ity of the solution by the appropriate method specified inISO 3363, titration in accordance with 6.3.1.2-6.3.2.3, using apH indicator or another acceptable laboratory technique pro-viding equivalent results.6.3.1 Sodium Hydroxide Titration:6.3.1.1 Reagents:(1) Sodium Hydroxide, 0.01 N solution, stan
36、dardizedagainst reagent grade potassium acid phthalate.(2) Methyl Red Indicator, 0.1 % solution.6.3.1.2 ProcedureMeasure (graduate) 50 mL of ice-colddistilled water (stored in a 34F refrigerator) in a 250-mlstoppered Erlenmeyer flask. Sparge 50g of bromotrifluo-romethane into the cold water. Swirl t
37、he flask gently during theaddition or, alternatively, add a magnetic stirring bar and stirthe solution during the addition. Following the sample addi-tion, pipet 5.0 mL of the water solution into a small glass vial,cap, and save for the Halogen ion test, 6.5. To the remainingwater in the flask, add
38、two drops of methyl red indicator, swirl,and if a reddish color remains, titrate to a yellow end point with0.01 normal sodium hydroxide (NaOH). Run a blank (no Halon1301) by titrating 45 mL of the cold DI water.6.3.1.3 CalculationCalculate parts per million acid ha-lide, as HBr, as follows:acid hali
39、des, ppm 5A 2 B! 3 N 3 80.9 3 103grams of sample 3 0.9(5)where:A = mL of NaOH for sample,B = mL of NaOH for blank,N = normality of the NaOH titrantNaOH = sodium hydroxide80.9 3 103= equivalent weight of HBr (hydrogen bro-mide)103= Factor to convert result to ppmAcid halides in excess of the amount s
40、pecified in Table 1shall constitute test failure by this method. Should no acidity bedetected (that is, no color change of the indicator is observed),report result as“ passes test.”6.3.2 Acidity by Universal Indicator:6.3.2.1 Apparatus:(1) Fritted Glass Sparger, of coarse porosity, contained ina 100
41、-ml glass scrubbing bottle provided with inlet and outlettubes.(2) Neoprene Connecting Tubing.(3) Wet Test Meter, 0.1 ft3revolutions.(4) Needle Valve Control, No. 55-660, Matheson Co5., orequivalent.6.3.2.2 Reagent Universal Indicator,6with color chart, orequivalent.6.3.2.3 ProcedurePrepare neutrali
42、zed distilled water byadding 0.4 ml of universal indicator solution to 100 ml ofdistilled water and titrate to a pH of 7.0 with 0.01 N sodiumhydroxide (if acidic) or with 0.01N HCl (if alkali) solution untilthe water reads a pH of 7.0 when compared to the universalcolor chart. Add 50 ml of the neutr
43、alized water to the glassscrubbing bottle fitted with the glass sparger. Attach a needlevalve control to the sample cylinder, and connect the cylinder,inverted, to an empty safety trap. Connect the safety trap outletto the scrubbing bottle inlet. Connect the scrubbing bottleoutlet to the inlet of th
44、e wet test meter. Open the needle valveslowly and pass 20 litres (66 gm) of sample through thescrubber at a flow rate of approximately 500 ml/min. Turn offthe needle valve and disconnect the sample cylinder from thescrubbing bottle. Also transfer 10 ml of the water solution to asmall glass vial, cap
45、, and save for the Halogen Ion test, 6.5.Add 0.3 ml of universal indicator solution and swirl. Read thepH of the solution by comparison with the universal colorchart. Report the pH reading. No observable change in pHindicates an acidity of less than 3 ppm.6.4 Water ContentMoisture determination shal
46、l be per-formed by Coulometric Karl Fischer titration or suitablealternative methodology. Water content greater than specifiedin Table 1 shall constitute failure of this test.6.5 Qualitative Test for Halogen IonTest a sample for thepresence of halogen ions in accordance with 6.5.1-6.5.4 or byanother
47、 acceptable laboratory technique providing equivalentresults. Generally, a sample treated with an alcoholic solutionof silver nitrate shall exhibit no turbidity or precipitation ofsilver halide.6.5.1 Reagents:6.5.2 3M silver Nitrate solutionDissolve 5.1 g of anhy-drous silver nitrate in DI water to
48、give a total volume of 10.0mL. Store in a brown glass bottle away from light.6.5.3 Nitric Acid, 1:1 v/v in water:6.5.4 ProcedureTo the water scrubber solution savedduring the acidity test (from 6.3.2.3), add 1 drop of 1:1 HNO3,swirl to mix. Then add 3 to 4 drops of 3M silver nitrate solutionand swir
49、l to mix. The appearance of any haze or turbidity shallconstitute failure of this test.6.6 Nonvolatile ResidueDetermine the nonvolatile resi-due in accordance with the method specified in ISO 5789 oranother accepted laboratory technique providing equivalentresults.6.7 Suspended Matter and SedimentDuring the Halon1301 evaporation step of the nonvolatile residue test (see 6.6),examine visually for any suspended matter or sediment.Observation of any suspended matter or sediment shall consti-tute failure of this test.6.8 Fixed or Nonabsorb
