ASTM D6064-11(2022)

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
Designation: D6064 −11 (Reapproved 2022)
Standard Specification for
HFC-227ea, 1,1,1,2,3,3,3-Heptafluoropropane (CF CHFCF )
3 3
This standard is issued under the fixed designation D6064; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope ISO 5789Fluorinated Hydrocarbons for Industrial Use-
Determination of Nonvolatile Residue
1.1 This specification covers requirements for HFC-227ea
2.2 ASRE Standard:
as a fire-fighting medium.
ASRE Standard34
1.2 This specification does not address the fire-fighting
equipment or hardware that employs HFC-227ea or the con-
3. Terminology
ditions of employing such equipment (for example, handhelds,
3.1 Definitions of Terms Specific to This Standard:
fixed installations, etc.).
3.1.1 HFC—hydrofluorocarbon; a chemical compound in
1.3 This specification does not address the storage or
which the compound molecule is comprised exclusively of
transportation of HFC-227ea. Storage, handling, and transpor-
hydrogen and fluorine and carbon atoms.
tation issues may be addressed in futureASTM specifications.
3.1.2 HFC-227ea—the compound 1,1,1,2,3,3,3-
1.4 The values stated in both inch-pound and SI units are to
heptafluoropropane; CF CHFCF .
3 3
be regarded separately as the standard. The values given in
3.1.2.1 Discussion—The terminology system for fluorine-
parentheses are for information only.
containing compounds (described in detail in ASRE Stan-
dard34)providesaconvenientmeanstoreferencethestructure
1.5 The following safety hazards caveat pertains only to the
of individual compounds. By definition, the first digit of the
test methods portion, Section 5, of this specification: This
numbering system represents one less than the number of
standard does not purport to address all of the safety concerns,
carbon atoms in the compound molecule; the second digit, one
if any, associated with its use. It is the responsibility of the user
more than the number of hydrogen atoms in the compound
of this standard to establish appropriate safety, health, and
molecule; and the third digit, the number of fluorine atoms in
environmental practices and determine the applicability of
the compound molecule. For molecules containing three car-
regulatory limitations prior to use.Specific hazards statements
bon atoms, two appended letters are added to indicate the
are given in Note 1.
symmetry of the molecule. The first appended letter indicates
1.6 This international standard was developed in accor-
dance with internationally recognized principles on standard- the substitution on the central (C2) carbon; for example, the
substitution CHF is assigned the designation “e.” The second
ization established in the Decision on Principles for the
Development of International Standards, Guides and Recom- appended letter indicates the substitution at the C1 and C3
carbons; for example, identical substitution on the C1 and C3
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee. carbons are assigned the designation “a.” For example, the
designation HFC-227ea indicates three carbon atoms (2+1),
2. Referenced Documents one hydrogen atom (2−1), and seven fluorine atoms; the
designation “e” indicates that the central carbon is substituted
2.1 ISO Standards:
as CHF, and the designation“ a” indicates that the substitution
ISO 3363Fluorochlorinated Hydrocarbons for Industrial
on Carbons C1 and C3 is identical, that is, the structure is
Use-Determination of Acidity-Titrimetric Method
CF CHFCF .
3 3
ISO 3427Gaseous Halogenated Hydrocarbons (Liquefied
Gases)–Taking of a Sample
4. Material Requirements
4.1 Type I—Mixtures of HFC-227ea and Nitrogen:
4.1.1 The nitrogen (N ) partial pressure shall be such that
This specification is under the jurisdiction of ASTM Committee D26 on
Halogenated Organic Solvents and Fire Extinguishing Agents and is the direct
the safe working pressure of the receiving vessel is not
responsibility of Subcommittee D26.09 on Fire Extinguishing Agents.
exceeded. To prevent excessive pressure, the fill density of
Current edition approved Nov. 1, 2022. Published November 2022. Originally
approved in 1996. Last previous edition approved in 2015 as D6064–11 (2015).
DOI: 10.1520/D6064-11R22.
2 3
Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St., American Society of Refrigeration Engineers, Refrigeration Engineering 65,
4th Floor, New York, NY 10036, http://www.ansi.org. 1957, p. 49.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D6064 − 11 (2022)
HFC-227eawithinacontainershouldnotexceedthatneededto 6. Test Methods
achieve complete filling of the container at the maximum
6.1 Purity:
envisagedstoragetemperature.Forexample,fortheU.S.DOT
6.1.1 Determine the purity by gas-liquid chromatography in
4BA500cylinder,thenitrogenpartialpressureshallnotexceed
accordance with the technique described in 6.1.2 – 6.1.5 or
21.8 bar at 21°C (316 psig at 70°F) for a 1150kg⁄m
another acceptable laboratory technique providing equivalent
(72lb⁄ft ) fill density (yielding a total pressure of 25.8 bar at
results.
21°C (360 psig at 70°F). For this example, the safe working
6.1.2 Apparatus—The following special apparatus is re-
pressure of the 4BA500 cylinder is not exceeded for tempera-
quired to determine the percent of HFC-227ea:
tures below 54°C (130°F).
6.1.2.1 Gas Chromatograph, capable of programmed tem-
4.1.2 HFC-227ea shall conform to the requirements pre-
perature operation and equipped with a thermal conductivity
scribed in Table 1 when tested by the appropriate test meth-
detector.
od(s) listed in Section 6.
6.1.2.2 Column, 3.1m by 5mm outside diameter (2.6mm
4.1.3 When a material analysis is required, by agreement
innerdiameter)glasstubing,packedwith80meshto120mesh
betweenthepurchaserandthesupplier,thetotalpressureinthe
Carbopack B or equivalent.
HFC-227eacontainer,partialpressureoftheN ,thefilldensity
6.1.2.3 Gas Sampling Valve, 10mL volume or a volume
of HFC-227ea within the container, and the maximum safe
sufficient to achieve proper separation in the specified column.
storage temperature shall be part of the material analysis 5
6.1.2.4 Glass Syringe,20mLHamiltonB-D, orequivalent.
(certification).Thepressureshallbereportedinbar(preferred)
6.1.2.5 Three-Way Purge/Isolation Valve, Hamilton 86727
or pound-force per square inch gage. The fill density shall be 5
miniature inert valve with Luer Lock fittings, or equivalent.
reported in kilograms per cubic metre at 21°C (preferred) or
6.1.3 Reagents—The carrier gas shall be a chromatographic
pounds per cubic foot at 70°F. The maximum safe storage
grade of helium. The column packing shall consist of a
temperature of the HFC-227ea container shall be reported in
standard solution, for example 3% (weight⁄weight) methyl
degrees Celsius (preferred) or in degrees Fahrenheit and shall 5 5
silicone, on 80mesh to 120mesh Carbopack B (or equiva-
conformtoapplicableregulationsfortheHFC-227eacontainer
lent).
design and use.
6.1.4 Procedure:
4.2 Type II—HFC-227ea—HFC-227ea shall conform to the 6.1.4.1 Install the column and adjust the temperature of the
requirements of Type I, as listed in 3.1, and shall contain no column oven to 30°C, injection port to 100°C, and detector
more than 1.5% by volume fixed gases in vapor phase, block to 150°C. The temperature should be programmed to
expressed as air when tested by the appropriate test method(s) rise 10°C⁄min to 15°C⁄min (from an initial temperature of
listed in Section 6. 30°C), to a maximum of 100°C.
6.1.4.2 Adjust the helium flow to 25 mL/min.
4.3 By agreement between the purchaser and the supplier,
6.1.4.3 Adjust the detector voltage to 8 V or to the mid-
analysismayberequiredandlimitsestablishedforelementsor
range of the thermal conductivity detector (TCD) instrument
compounds not specified in Table 1.
being used and allow the instrument to stabilize.
4.4 Unless otherwise specified, Type II is assumed.
6.1.4.4 Take the sample from the vapor phase; collect
approximately 20 mL in the glass syringe.
NOTE1—ProlongedexposuretoconcentrationsofHFC-227eainexcess
of 10.5% by volume in air during periods of elevated adrenaline could 6.1.4.5 Purge the sample loop with approximately 10 mLof
produce cardiac arrhythmia in some personnel.
sample from the syringe and transfer the sample into the
chromatographic system.
5. Sampling
6.1.4.6 Allow the sample to elute, for approximately 18
5.1 Samples of HFC-227ea, taken from the liquid phase,
min, attenuating as necessary to make the peak heights a
shall be taken from filled containers in accordance with the
convenient size. Under proper instrument settings, the HFC-
method specified in ISO 3427. The sampling cylinder shall be
227ea should elute after approximately 5 min.
capable of safely resisting the vapor pressure of the sample at
6.1.5 Calculation:
the highest temperature that could be encountered.
6.1.5.1 Calculate percent HFC-227ea as follows:
5.2 TheHFC-227easelectedinaccordancewith5.1shallbe
A CF CHFCF 3100
~ !
3 3
tested for quality conformance in accordance with Section 6. %HFC 2227ea 5 (1)
As
The presence of one or more defects shall be cause for
where:
rejection.
A(CF CHFCF ) = area of the HFC-227ea peak, and
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TABLE 1 Requirements
As = sum of the area of all peaks, excluding
Property Requirement
the nitrogen peak.
HFC-227ea purity 99.0 %, mol/mol, min
Percent HFC-227ea below that specified in Table 1 shall
Acidity (exclusive of any N present)
2.0 ppm by mass, as HCL, max
constitute failure of this test method.
Water content ppm by mass, max 10 ppm by mass, max
Nonvolatile residue 0.05 g/100 mL, max
Halogen ion passes test
Available from Alltech, 2051 Waukegan Road, Deerfield, IL 60015.
Suspended matter or sediment none visible
Available from Hamilton Co., P.O. Box 10030, Reno, NV 89520-0012.
D6064 − 11 (2022)
6.1.5.2 Calculate percent nitrogen as follows: 6.2.2.6 Reagent Universal Indicator, with color chart, or
equivalent.
An 3100
%N 5 (2)
6.2.2.7 Procedure—Prepare neutralized distilled water by
As
adding 0.4 mL of universal indicator solution to 100 mL of
where:
deionizedwater,andtitratewith0.01 Nsodiumhydroxideuntil
An = area of nitrogen peak, and the water shows a pH of 7.0 when compared to the Universal
As = sum of the area of all other peaks, including the
Color Chart. Add 50 mL of the neutralized water to the glass
nitrogen peak.
scrubbing bottle fitted with the glass gas sparger. Attach a
needle valve control to the sample cylinder, and connect the
It is useful to calculate percent nitrogen in order to judge a
cylinder, inverted, to an empty safety trap. Connect the safety
safe fill density.
trap outlet to the scrubbing bottle inlet. Connect the scrubbing
6.2 Acidity—Vaporize a large sample, in the presence of
bottle outlet to the inlet of the wet test meter. Open the needle
distilled water. Determine the acidity of the solution by the
valve slowly and pass 20 L of sample through the scrubber at
appropriate method described in ISO 3363, 6.2.1 of this
a flow rate of approximately 500 mL/min. Turn off the needle
standard, 6.2.2 of this standard, a pH indicator, or another
valve and disconnect the sample cylinder from the scrubbing
acceptable laboratory technique providing equivalent results.
bottle. Transfer 10mL to 12 mL of water solution to a clean
6.2.1 Acidity by Sodium Hydroxide Titration:
testtube.Add0.3mLofuniversalindicatorsolutionandswirl.
6.2.1.1 Reagents:
Read the pH of the solution by comparison with the universal
6.2.1.2 Sodium Hydroxide, 0.01 N solution, standardized
color chart. Report the pH reading. No observable change in
with reagent grade potassium hydrogen phthalate, or standard-
pH indicates an acidity of less than 3.0 ppm.
ized by the supplier.
6.3 Water Content—Test HFC-227ea for water content.The
6.2.1.3 Methyl Red Indicator, 0.1% aqueous solution.
analysis may be conducted by the phosphorus pentoxide
6.2.1.4 Procedure—Fill a suitable gas sampling cylinder
method, infrared absorption, electrolytic moisture analysis,
withliquidHFC-227ea,andweighthecylinder.Place50mLof
piezoelectric analyzer, or another acceptable laboratory tech-
a crushed ice-distilled water slurry in a 250mL stoppered
nique. The accuracy of the results and the standard method
Erlenmeyer flask, slowly add the HFC-227ea under the slurry
should be by orthodox Karl Fischer method. Water content
surface, and then reweigh the sample cylinder. Place the
greater than specified in Table 1 shall constitute failure of this
stopperintheflasklooselyandswirltheflaskgentlyfromtime
test.
to time until the ice has melted completely. Add one drop of
methyl red indicator, and if a reddish color remains, titrate to a
6.4 Qualitative Test for Fluoride Ion—Test a sample for the
yellow endpoint with 0.01 N sodium hydroxide solution. Run
presence of fluoride ions in accordance with 6.4.1 through
a crushed ice-distilled water blank (with no HFC-227ea) along
6.4.3 or by another acceptable laboratory technique providing
with the sample.
equivalent results. Generally, a sample treated with a saturated
6.2.1.5 Calculation—Calculate parts per million hydrogen
aqueous solution of calcium chloride shall exhibit no turbidity
chloride as follows:
or precipitation of calcium fluoride.
6 6.4.1 Apparatus:
HCl, ppm 5 A 2 B 3N 30.03645 310 weight of sample, g (3)
~ !
6.4.1.1 Fritted Glass Gas Sparger, of coarse or A porosity,
where:
contained in a 100-mL glass scrubbing bottle provided with
A = volume of NaOH titrated in sample, mL,
inlet and outlet tubes.
B = volume of NaOH titrated in the blank, mL,
6.4.1.2 Neoprene Tubing.
N = normality of NaOH,
6.4.1.3 Wet Test Meter,0to1ft /revolution.
W = weight of HFC-227ea, g, and
6.4.1.4 Needle Valve Control.
6.4.2 Reagents:
where:
6.4.2.1 Calcium Chloride, saturated solution in water.
0.03645 × 10 = factortoexpressresultasppmHCl(hydro-
6.4.3 Procedure—Add 10 mLof saturated calcium chloride
gen chloride).
solution to the scrubber assembly. Attach a needle valve
Acidity in excess of the amount specified in Table 1 shall
control to the sample cylinder. Connect the sample cylinder in
constitute failure of this test.
the upright position to an empty safety trap with neoprene
6.2.2 Acidity by Universal Indicator:
tubing. Connect the outlet of the safety trap to the inlet of the
6.2.2.1 Apparatus.
scrubb
...