1、Designation: D 5632 01Standard 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 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 it
5、s 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 4.3.2. Referenced Documents2.1 ASTM Standards:D 5631 Practice for Handling
6、, Transportation, and Storageof Halon 1301, Bromotrifluoromethane (CF3Br)22.2 ISO Standards:3ISO 3363 Fluorochlorinated Hydrocarbons for IndustrialUseDetermination of AcidityTitrimetric MethodISO 3427 Gaseous Halogenated Hydrocarbons (LiquifiedGases)Taking of a SampleISO 5789 Fluorinated Hydrocarbon
7、s for Industrial UseDetermination of Nonvolatile Residue2.3 U.S. Industry Standard:4ASQ Z1.4 Sampling Procedures and Tables for Inspectionby Attributes (ANSI Approved, DoD Adopted)3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 halon 1301The halogenated hydrocarbon com-pound B
8、romotrifluoromethane used as a fire extinguishingmedium.3.1.1.1 DiscussionThe 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 bee
9、n 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 of carbon atoms in the compound molecule; the seconddigit, the number of fluorine atoms; the third digit, the numberof chlor
10、ine atoms; the fourth digit, the number of bromineatoms; and the fifth digit, the number of iodine atoms. Trailingzeros are not expressed. Unaccounted for valence requirementsare assumed to be hydrogen atoms.number of hydrogen atoms 5number of carbon atoms3 2!12!2sum of halogen atoms!# (1)For exampl
11、e,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 thatthe safe working pressure of the receiving vessel is notexceeded. To prevent excessive pressure, the fill density of thehal
12、on 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 cylinder partial pressure shall not exceed 12.1 bar at21C (161 psi at 70F) for a 1121-kg/m3(70 lb/ft3) fill density(yielding a
13、 total pressure of 25.8 bar at 21C (360 psig at1This 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 Agents.Current edition approved Oct. 10, 2001
14、. Published December 2001. Originallypublished as D 5632 94a. Last previous edition D 5632 95.2Annual Book of ASTM Standards, Vol 15.05.3Available from American National Standards Institute, 11 W. 42nd St., 13thFloor, New York, NY 10036.4Available from Standardization Documents Order Desk, Bldg. 4 S
15、ection D, 100Robbins Ave., Philadelphia, PA 191115904, Attn: NPODS.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.70F). For this example, the safe working pressure of the4BA500 cylinder is not exceeded for temperatures below 54C(130
16、F).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 container, partial press
17、ure 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 bar (preferred)or pound-force per square inch gage. The fill density shall bereported in kilograms per cu
18、bic metre at 21C (preferred) orpounds per cubic foot at 70F. The maximum safe storagetemperature of the Halon 1301 container shall be reported indegrees Celsius (preferred) or in degrees Fahrenheit and shallconform to applicable regulations for the Halon 1301 containerdesign and use.4.2 Type IIHalon
19、 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 the supplier,analysis may be requ
20、ired 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 otherwise specified, Type I is
21、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 S-4. The sampling bottle shall
22、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 Section 6.The presence of one or mor
23、e 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 known bromotrifluoromethanepurit
24、y 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 integrator or suitablecomputer data ga
25、thering 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, from several chromatographic supp
26、ly 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 from gas dispersion tube andint
27、roduce 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 Install the column in the gas chro
28、matograph 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 temperature to rise 10C per minute to a ma
29、xi-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= Relative Response Factor for componen
30、t 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 % 3 148.9M(4)where:Wt %i= weight p
31、ercent 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 diameter. The presence of methano
32、l 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 sediment None visibleD5632012inac
33、curate 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 theacidity of the solution by the appro
34、priate 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, standardizedagainst reagent grade po
35、tassium 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 the flask gently during theadditi
36、on 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 two drops of methyl red indicato
37、r, 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 halides, ppm 5A 2 B! 3 N 3 80.9 3 10
38、3grams 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 specified in Table 1shall constit
39、ute 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-ml glass scrubbing bottle provi
40、ded 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 neutralized distilled water byadding 0.4
41、 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 neutralized water to the glassscrubbi
42、ng 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 the wet test meter. Open the needl
43、e 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, and save for the Halogen Ion t
44、est, 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 shall be per-formed by Coulometric K
45、arl 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 acceptable laboratory technique
46、 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 give a total volume of 10.0mL. S
47、tore 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 swirl to mix. The appearance of any
48、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 s
49、tep 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 Nonabsorbable Gases (NAG) in the vaporphaseTest Halon 1301 for air in the vapor phase usingisothermal gas chromatography or another accepted laboratorytechnique providing equivalent results.6.8.1 Prior to sample introduction, calibration of the GCusing a 15 % air or nitrogen calibration standard in heliummust be performed as described for
