1、Designation: D 6064 03Standard Specification forHFC-227ea, 1,1,1,2,3,3,3-Heptafluoropropane (CF3CHFCF3)1This standard is issued under the fixed designation D 6064; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last re
2、vision. 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 specification covers requirements for HFC-227eaas a fire-fighting medium.1.2 This specification does not address the fi
3、re-fightingequipment or hardware that employs HFC-227ea or the con-ditions of employing such equipment (for example, handhelds,fixed installations, etc.).1.3 This specification does not address the storage ortransportation of HFC-227ea. Storage, handling, and transpor-tation issues may be addressed
4、in future ASTM specifications.1.4 The values stated in both inch-pound and SI units are tobe regarded separately as the standard. The values given inparentheses are for information only.1.5 The following safety hazards caveat pertains only to thetest methods portion, Section 5, of this specification
5、: 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 to use. Specific hazards st
6、atements are given inNote 1.2. Referenced Documents2.1 ISO Standards:ISO 3363 Fluorochlorinated Hydrocarbons for IndustrialUse-Determination of Acidity-Titrimetric Method2ISO 3427 Gaseous Halogenated Hydrocarbons (LiquefiedGases)Taking of a Sample2ISO 5789 Fluorinated Hydrocarbons for Industrial Use
7、-Determination of Nonvolatile Residue22.2 ASRE Standard:ASRE Standard 3433. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 HFChydrofluorocarbon; a chemical compound inwhich the compound molecule is comprised exclusively ofhydrogen and fluorine and carbon atoms.3.1.2 HFC-227eathe
8、 compound 1,1,1,2,3,3,3-heptafluoropropane; CF3CHFCF3.3.1.2.1 DiscussionThe terminology system for fluorine-containing compounds (described in detail in ASRE Stan-dard 34) provides a convenient means to reference the structureof individual compounds. By definition, the first digit of thenumbering sy
9、stem represents one less than the number ofcarbon atoms in the compound molecule; the second digit, onemore than the number of hydrogen atoms in the compoundmolecule; and the third digit, the number of fluorine atoms inthe compound molecule. For molecules containing three car-bon atoms, two appended
10、 letters are added to indicate thesymmetry of the molecule. The first appended letter indicatesthe substitution on the central (C2) carbon; for example, thesubstitution CHF is assigned the designation “e.” The secondappended letter indicates the substitution at the C1 and C3carbons; for example, ide
11、ntical substitution on the C1 and C3carbons are assigned the designation “a.” For example, thedesignation HFC-227ea indicates three carbon atoms (2 + 1),one hydrogen atom (21), and seven fluorine atoms; thedesignation “e” indicates that the central carbon is substitutedas CHF, and the designation“ a
12、” indicates that the substitutionon Carbons C1 and C3 is identical, that is, the structure isCF3CHFCF3.4. Material Requirements4.1 Type IMixtures of HFC-227ea and Nitrogen:4.1.1 The nitrogen (N2) partial pressure shall be such thatthe safe working pressure of the receiving vessel is notexceeded. To
13、prevent excessive pressure, the fill density ofHFC-227ea within a container should not exceed that needed toachieve complete filling of the container at the maximumenvisaged storage temperature. For example, for the U.S. DOT4BA500 cylinder, the nitrogen partial pressure shall not exceed21.8 bar at 2
14、1C (316 psig at 70F) for a 1150-kg/m3(72-lb/ft3)fill density (yielding a total pressure of 25.8 bar at 21C (3601This specification is under the jurisdiction of ASTM Committee D26 onHalogenated Organic Solvents and is the direct responsibility of SubcommitteeD26.09 on Fire Extinguishing Agents.Curren
15、t edition approved June 10, 2003. Published August 2003. Originallyapproved in 1996. Last previous edition approved in 1996 as D 606496.2Available from American National Standards Institute, 11 W. 42nd St., 13thFloor, New York, NY 10036.3American Society of Refrigeration Engineers, Refrigeration Eng
16、ineering 65,1957, p. 49.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.psig at 70F). For this example, the safe working pressure ofthe 4BA500 cylinder is not exceeded for temperatures below54C (130F).4.1.2 HFC-227ea shall conform to
17、 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 theHFC-227ea container, partial pressure of the N2, the fill densityof HFC
18、-227ea 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 cubic metre at 21C (preferred) orpounds
19、 per cubic foot at 70F. The maximum safe storagetemperature of the HFC-227ea container shall be reported indegrees Celsius (preferred) or in degrees Fahrenheit and shallconform to applicable regulations for the HFC-227ea containerdesign and use.4.2 Type IIHFC-227eaHFC-227ea shall conform to therequi
20、rements of Type I, as listed in 3.1, and shall contain nomore than 1.5 % by volume fixed gases in vapor phase,expressed as air when tested by the appropriate test method(s)listed in Section 6.4.3 By agreement between the purchaser and the supplier,analysis may be required and limits established for
21、elements orcompounds not specified in Table 1.4.4 Unless otherwise specified, Type II is assumed.NOTE 1Prolonged exposure to concentrations of HFC-227ea in ex-cess of 10.5 % by volume in air during periods of elevated adrenalinecould produce cardiac arrhythmia in some personnel.5. Sampling5.1 Sample
22、s of HFC-227ea, taken from the liquid phase,shall be taken from filled containers in accordance with themethod specified in ISO 3427. The sampling cylinder shall becapable of safely resisting the vapor pressure of the sample atthe highest temperature that could be encountered.5.2 The HFC-227ea selec
23、ted 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 Purity:6.1.1 Determine the purity by gas-liquid chromatography inaccordance with the technique described in 6.1.2-6.1.5 or
24、another acceptable laboratory technique providing equivalentresults.6.1.2 ApparatusThe following special apparatus is re-quired to determine the percent of HFC-227ea:6.1.2.1 Gas Chromatograph, capable of programmed tem-perature operation and equipped with a thermal conductivitydetector.6.1.2.2 Colum
25、n, 3.1-m by 5-mm outside diameter (2.6-mminner diameter) glass tubing, packed with 80 to 120 meshCarbopack B4or equivalent.6.1.2.3 Gas Sampling Valve, 10-mL volume or a volumesufficient to achieve proper separation in the specified column.6.1.2.4 Glass Syringe, 20-mL Hamilton B-D,5or equivalent.6.1.
26、2.5 Three-Way Purge/Isolation Valve, Hamilton 86727miniature inert valve with Luer Lock fittings,5or equivalent.6.1.3 ReagentsThe carrier gas shall be a chromatographicgrade of helium. The column packing shall consist of astandard solution, for example 3 % (weight/weight) methylsilicone,5on 80 to 12
27、0-mesh Carbopack B5(or equivalent).6.1.4 Procedure:6.1.4.1 Install the column and adjust the temperature of thecolumn oven to 30C, injection port to 100C, and detectorblock to 150C. The temperature should be programmed to rise10 to 15C/min (from an initial temperature of 30C), to amaximum of 100C.6.
28、1.4.2 Adjust the helium flow to 25 mL/min.6.1.4.3 Adjust the detector voltage to 8 V or to the mid-range of the thermal conductivity detector (TCD) instrumentbeing used and allow the instrument to stabilize.6.1.4.4 Take the sample from the vapor phase; collectapproximately 20 mL in the glass syringe
29、.6.1.4.5 Purge the sample loop with approximately 10 mL ofsample from the syringe and transfer the sample into thechromatographic system.6.1.4.6 Allow the sample to elute, for approximately 18min, attenuating as necessary to make the peak heights aconvenient size. Under proper instrument settings, t
30、he HFC-227ea should elute after approximately 5 min.6.1.5 Calculation:6.1.5.1 Calculate percent HFC-227ea as follows:%HFC2227ea 5ACF3CHFCF3! 3 100As(1)where:A(CF3CHFCF3) = area of the HFC-227ea peak, andAs = sum of the area of all peaks, excludingthe nitrogen peak.Percent HFC-227ea below that specif
31、ied in Table 1 shallconstitute failure of this test method.6.1.5.2 Calculate percent nitrogen as follows:%N25An 3 100As(2)where:An = area of nitrogen peak, andAs = sum of the area of all other peaks, including thenitrogen peak.4Available from Alltech, 2051 Waukegan Road, Deerfield, IL 60015.5Availab
32、le from Hamilton Co., P.O. Box 10030, Reno, NV 89520-0012.TABLE 1 RequirementsProperty RequirementHFC-227ea purity 99.95 %, mol/mol, minAcidity (exclusive of any N2present)2.0 ppm by mass, as HCL, maxWater content ppm by mass, max 10 ppm by mass, maxNonvolatile residue 0.05 g/100 mL, maxHalogen ion
33、passes testSuspended matter or sediment none visibleD6064032It is useful to calculate percent nitrogen in order to judge asafe fill density.6.2 AcidityVaporize a large sample, in the presence ofdistilled water. Determine the acidity of the solution by theappropriate method described in ISO 3363, 6.2
34、.1 of thisstandard, 6.2.2 of this standard, a pH indicator, or anotheracceptable laboratory technique providing equivalent results.6.2.1 Acidity by Sodium Hydroxide Titration:6.2.1.1 Reagents:6.2.1.2 Sodium Hydroxide, 0.01 N solution, standardizedwith reagent grade potassium hydrogen phthalate, or s
35、tandard-ized by the supplier.6.2.1.3 Methyl Red Indicator, 0.1 % aqueous solution.6.2.1.4 ProcedureFill a suitable gas sampling cylinderwith liquid HFC-227ea, and weigh the cylinder. Place 50 mL ofa crushed ice-distilled water slurry in a 250-mL stopperedErlenmeyer flask, slowly add the HFC-227ea un
36、der the slurrysurface, and then reweigh the sample cylinder. Place thestopper in the flask loosely and swirl the flask gently from timeto time until the ice has melted completely. Add one drop ofmethyl red indicator, and if a reddish color remains, titrate to ayellow endpoint with 0.01 N sodium hydr
37、oxide solution. Runa crushed ice-distilled water blank (with no HFC-227ea) alongwith the sample.6.2.1.5 CalculationCalculate parts per million hydrogenchloride as follows:HCl, ppm 5 A2B! 3 N 3 0.03645 3 106weight of sample, g(3)where:A = volume of NaOH titrated in sample, mL,B = volume of NaOH titra
38、ted in the blank, mL,N = normality of NaOH,W = weight of HFC-227ea, g, andwhere:0.03645 3 106= factor to express result as ppm HCl(hydrogen chloride).Acidity in excess of the amount specified in Table 1 shallconstitute failure of this test.6.2.2 Acidity by Universal Indicator:6.2.2.1 Apparatus:6.2.2
39、.2 Fritted Glass Sparger, of coarse porosity, containedin a 100-mL glass scrubbing bottle provided with inlet andoutlet tubes.6.2.2.3 Neoprene Connecting Tubing.6.2.2.4 Wet Test Meter, 0.1 ft3revolution.6.2.2.5 Needle Valve Control.66.2.2.6 Reagent Universal Indicator,7with color chart, orequivalent
40、.6.2.2.7 ProcedurePrepare neutralized distilled water byadding 0.4 mL of universal indicator solution to 100 mL ofdeionized water, and titrate with 0.01 N sodium hydroxide untilthe water shows a pH of 7.0 when compared to the UniversalColor Chart. Add 50 mL of the neutralized water to the glassscrub
41、bing bottle fitted with the glass gas sparger. Attach aneedle valve control to the sample cylinder, and connect thecylinder, inverted, to an empty safety trap. Connect the safetytrap outlet to the scrubbing bottle inlet. Connect the scrubbingbottle outlet to the inlet of the wet test meter. Open the
42、 needlevalve slowly and pass 20 L of sample through the scrubber ata flow rate of approximately 500 mL/min. Turn off the needlevalve and disconnect the sample cylinder from the scrubbingbottle. Transfer 10 to 12 mL of water solution to a clean testtube. Add 0.3 mL of universal indicator solution and
43、 swirl.Read the pH of the solution by comparison with the universalcolor chart. Report the pH reading. No observable change inpH indicates an acidity of less than 3.0 ppm.6.3 Water ContentTest HFC-227ea for water content. Theanalysis may be conducted by the phosphorus pentoxidemethod, infrared absor
44、ption, electrolytic moisture analysis,piezoelectric analyzer, or another acceptable laboratory tech-nique. The accuracy of the results and the standard methodshould be by orthodox Karl Fischer method. Water contentgreater than specified in Table 1 shall constitute failure of thistest.6.4 Qualitative
45、 Test for Fluoride IonTest a sample for thepresence of fluoride ions in accordance with 6.4.1 through6.4.3 or by another acceptable laboratory technique providingequivalent results. Generally, a sample treated with a saturatedaqueous solution of calcium chloride shall exhibit no turbidityor precipit
46、ation of calcium fluoride.6.4.1 Apparatus:6.4.1.1 Fritted Glass Gas Sparger, of coarse or A porosity,contained in a 100-mL glass scrubbing bottle provided withinlet and outlet tubes.6.4.1.2 Neoprene Tubing.6.4.1.3 Wet Test Meter,0to1ft3/revolution.6.4.1.4 Needle Valve Control.76.4.2 Reagents:6.4.2.1
47、 Calcium Chloride, saturated solution in water.6.4.3 ProcedureAdd 10 mL of saturated calcium chloridesolution to the scrubber assembly. Attach a needle valvecontrol to the sample cylinder. Connect the sample cylinder inthe upright position to an empty safety trap with neoprenetubing. Connect the out
48、let of the safety trap to the inlet of thescrubbing bottle assembly with neoprene tubing. Connect theoutlet of the scrubbing bottle assembly to the inlet of the wettest meter. Open the needle valve slowly and pass approxi-mately 2 L of sample through the scrubber at a flow rate ofapproximately 100 m
49、L/min. Turn off the needle valve anddisconnect the scrubber assembly from the sample cylinder andthe wet test meter. Examine the contents of the scrubbervisually for the presence of turbidity. Report the fluoridepresent if any turbidity develops. The appearance of anyturbidity shall constitute failure of this test.6.5 Suspended Matter and SedimentExamine visually forany suspended matter or sediment. Observation of any sus-pended matter or sediment shall constitute failure of this test.6.6 Nonvolatile ResidueDetermine the nonvolatile resi-due in accorda
