ASTM D6064-96
(Specification)Standard Specification for HFC-227ea, 1,1,1,2,3,3,3-Heptafluoropropane (CF3CHFCF3)
Standard Specification for HFC-227ea, 1,1,1,2,3,3,3-Heptafluoropropane (CF<sub>3</sub>CHFCF<sub>3</sub>)
SCOPE
1.1 This specification covers requirements for HFC-227ea as a fire-fighting medium.
1.2 This specification does not address the fire-fighting equipment or hardware that employs HFC-227ea or the conditions of employing such equipment (for example, handhelds, fixed installations, etc.).
1.3 This specification does not address the storage or transportation of HFC-227ea. Storage, handling, and transportation issues may be addressed in future ASTM specifications.
1.4 The values stated in both inch-pound and SI units are to be regarded separately as the standard. The values given in parentheses are for information only.
1.5 The following safety hazards caveat pertains only to the test methods portion, Section 5, of this specification: This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. Specific hazards statements are given in Note 1.
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Designation: D 6064 – 96
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 D 6064; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope hydrogen and fluorine and carbon atoms.
3.1.2 HFC-227ea—the compound 1,1,1,2,3,3,3-
1.1 This specification covers requirements for HFC-227ea
heptafluoropropane; CF CHFCF .
3 3
as a fire-fighting medium.
3.1.2.1 Discussion—The terminology system for fluorine-
1.2 This specification does not address the fire-fighting
containing compounds (described in detail in ASRE Stan-
equipment or hardware that employs HFC-227ea or the con-
dard 34) provides a convenient means to reference the structure
ditions of employing such equipment (for example, handhelds,
of individual compounds. By definition, the first digit of the
fixed installations, etc.).
numbering system represents one less than the number of
1.3 This specification does not address the storage or
carbon atoms in the compound molecule; the second digit, one
transportation of HFC-227ea. Storage, handling, and transpor-
more than the number of hydrogen atoms in the compound
tation issues may be addressed in future ASTM specifications.
molecule; and the third digit, the number of fluorine atoms in
1.4 The values stated in both inch-pound and SI units are to
the compound molecule. For molecules containing three car-
be regarded separately as the standard. The values given in
bon atoms, two appended letters are added to indicate the
parentheses are for information only.
symmetry of the molecule. The first appended letter indicates
1.5 The following safety hazards caveat pertains only to the
the substitution on the central (C2) carbon; for example, the
test methods portion, Section 5, of this specification: This
substitution CHF is assigned the designation “e.” The second
standard does not purport to address all of the safety concerns,
appended letter indicates the substitution at the C1 and C3
if any, associated with its use. It is the responsibility of the user
carbons; for example, identical substitution on the C1 and C3
of this standard to establish appropriate safety and health
carbons are assigned the designation “a.” For example, the
practices and determine the applicability of regulatory limita-
designation HFC-227ea indicates three carbon atoms (2 + 1),
tions prior to use. Specific hazards statements are given in
one hydrogen atom (2−1), and seven fluorine atoms; the
Note 1.
designation “e” indicates that the central carbon is substituted
2. Referenced Documents as CHF, and the designation“ a” indicates that the substitution
on Carbons C1 and C3 is identical, that is, the structure is
2.1 ISO Standards:
CF CHFCF .
3 3
ISO 3363 Fluorochlorinated Hydrocarbons for Industrial
Use-Determination of Acidity-Titrimetric Method
4. Material Requirements
ISO 3427 Gaseous Halogenated Hydrocarbons (Liquefied
4.1 Type I—Mixtures of HFC-227ea and Nitrogen:
Gases)–Taking of a Sample
4.1.1 The nitrogen (N ) partial pressure shall be such that
ISO 5789 Fluorinated Hydrocarbons for Industrial Use- 2
the safe working pressure of the receiving vessel is not
Determination of Nonvolatile Residue
exceeded. To prevent excessive pressure, the fill density of
2.2 ASRE Standard:
HFC-227ea within a container should not exceed that needed to
ASRE Standard 34
achieve complete filling of the container at the maximum
3. Terminology
envisaged storage temperature. For example, for the U.S. DOT
4BA500 cylinder, the nitrogen partial pressure shall not exceed
3.1 Definitions of Terms Specific to This Standard:
3 3
21.8 bar at 21°C (316 psig at 70°F) for a 1150-kg/m (72-lb/ft )
3.1.1 HFC—hydrofluorocarbon; a chemical compound in
fill density (yielding a total pressure of 25.8 bar at 21°C (360
which the compound molecule is comprised exclusively of
psig at 70°F). For this example, the safe working pressure of
the 4BA500 cylinder is not exceeded for temperatures below
This specification is under the jurisdiction of ASTM Committee D26 on
54°C (130°F).
Halogenated Organic Solvents and is the direct responsibility of Subcommittee
D26.09 on Fire Extinguishing Agents. 4.1.2 HFC-227ea shall conform to the requirements pre-
Current edition approved Dec. 10, 1996. Published February 1997.
scribed in Table 1 when tested by the appropriate test meth-
Available from American National Standards Institute, 11 W. 42nd St., 13th
od(s) listed in Section 6.
Floor, New York, NY 10036.
4.1.3 When a material analysis is required, by agreement
American Society of Refrigeration Engineers, Refrigeration Engineering 65,
1957, p. 49.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D 6064
TABLE 1 Requirements
Carbopack B or equivalent.
Property Requirement 6.1.2.3 Gas Sampling Valve, 10-mL volume or a volume
sufficient to achieve proper separation in the specified column.
HFC-227ea purity 99.95 %, mol/mol, min
Acidity (exclusive of any N present)
6.1.2.4 Glass Syringe, 20-mL Hamilton B-D, or equivalent.
2.0 ppm by mass, max
6.1.2.5 Three-Way Purge/Isolation Valve, Hamilton 86727
Water content ppm by mass, max 10 ppm by mass, max
miniature inert valve with Luer Lock fittings, or equivalent.
Nonvolatile residue 0.05 g/100 mL, max
Halogen ion passes test
6.1.3 Reagents—The carrier gas shall be a chromatographic
Suspended matter or sediment none visible
grade of helium. The column packing shall consist of a
standard solution, for example 3 % (weight/weight) methyl
5 5
silicone, on 80 to 120-mesh Carbopack B (or equivalent).
between the purchaser and the supplier, the total pressure in the
6.1.4 Procedure:
HFC-227ea container, partial pressure of the N , the fill density
6.1.4.1 Install the column and adjust the temperature of the
of HFC-227ea within the container, and the maximum safe
column oven to 30°C, injection port to 100°C, and detector
storage temperature shall be part of the material analysis
block to 150°C. The temperature should be programmed to rise
(certification). The pressure shall be reported in bar (preferred)
10 to 15°C/min (from an initial temperature of 30°C), to a
or pound-force per square inch gage. The fill density shall be
maximum of 100°C.
reported in kilograms per cubic metre at 21°C (preferred) or
6.1.4.2 Adjust the helium flow to 25 mL/min.
pounds per cubic foot at 70°F. The maximum safe storage
6.1.4.3 Adjust the detector voltage to 8 V or to the mid-
temperature of the HFC-227ea container shall be reported in
range of the thermal conductivity detector (TCD) instrument
degrees Celsius (preferred) or in degrees Fahrenheit and shall
being used and allow the instrument to stabilize.
conform to applicable regulations for the HFC-227ea container
6.1.4.4 Take the sample from the vapor phase; collect
design and use.
approximately 20 mL in the glass syringe.
4.2 Type II—HFC-227ea—HFC-227ea shall conform to the
6.1.4.5 Purge the sample loop with approximately 10 mL of
requirements of Type I, as listed in 3.1, and shall contain no
sample from the syringe and transfer the sample into the
more than 1.5 % by volume fixed gases in vapor phase,
chromatographic system.
expressed as air when tested by the appropriate test method(s)
6.1.4.6 Allow the sample to elute, for approximately 18
listed in Section 6.
min, attenuating as necessary to make the peak heights a
4.3 By agreement between the purchaser and the supplier,
convenient size. Under proper instrument settings, the HFC-
analysis may be required and limits established for elements or
227ea should elute after approximately 5 min.
compounds not specified in Table 1.
6.1.5 Calculation:
4.4 Unless otherwise specified, Type II is assumed.
6.1.5.1 Calculate percent HFC-227ea as follows:
NOTE 1—Prolonged exposure to concentrations of HFC-227ea in ex-
A~CF CHFCF ! 3 100
3 3
cess of 10.5 % by volume in air during periods of elevated adrenaline
%HFC2227ea 5 (1)
As
could produce cardiac arrhythmia in some personnel.
where:
5. Sampling
A(CF CHFCF ) = area of the HFC-227ea peak, and
3 3
5.1 Samples of HFC-227ea, taken from the liquid phase,
As = sum of the area of all peaks, excluding
shall be taken from filled containers in accordance with the
the nitrogen peak.
method specified in ISO 3427. The sampling cylinder shall be
Percent HFC-227ea below that specified in Table 1 shall
capable of safely resisting the vapor pressure of the sample at
constitute failure of this test method.
the highest temperature that could be encountered.
6.1.5.2 Calculate percent nitrogen as follows:
5.2 The HFC-227ea selected in accordance with 5.1 shall be
An 3 100
tested for quality conformance in accordance with Section 6.
%N 5 (2)
As
The presence of one or more defects shall be cause for
rejection.
where:
An = area of nitrogen peak, and
6. Test Methods
As = sum of the area of all other peaks, including the
6.1 Purity:
nitrogen peak.
6.1.1 Determine the purity by gas-liquid chromatography in
It is useful to calculate percent nitrogen in order to judge a
accordance with the technique described in 6.1.2-6.1.5 or
safe fill density.
another acceptable laboratory technique providing equivalent
6.2 Acidity—Vaporize a large sample, in the presence of
results.
distilled water. Determine the acidity of the solution by the
6.1.2 Apparatus—The following special apparatus is re-
appropriate method described in ISO 3363, titration in accor-
quired to determine the percent of HFC-227ea:
dance with 6.2.1.4 through 6.2.2.7, a pH indicator, or another
6.1.2.1 Gas Chromatograph, capable of programmed tem-
acceptable laboratory technique providing equivalent results.
perature operation and equipped with a thermal conductivity
6.2.1 Acidity by Sodium Hydroxide Titration:
detector.
6.1.2.2 Column, 3.1-m by 5-mm outside diameter (2.6-mm
Available from Alltech, 2051 Waukegan Road, Deerfield, IL 60015.
inner diameter) glass tubing, packed with 80 to 120 mesh
Available from Hamilton Co., P.O. Box 10030, Reno, NV 89520-0012.
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
D 6064
6.2.1.1 Reagents:
B = volume of NaOH titrated in the blank, mL,
6.2.1.2 Sodium Hydroxide, 0.01 N solution, standardized
N = normality of NaOH,
with reagent grade potassium hydrogen phthalate, or standard- W = weight of HFC-227ea, g, and
ized by the supplier.
20 000 5 20 3 1000 (6)
6.2.1.3 Methyl Red Indicator, 0.1 % aqueous solution.
6.2.1.4 Procedure—Fill a suitable gas sampling cylinder
where:
with liquid HFC-227ea, and collect 25 mL of liquid from the
20 = grams HF/equivalent HF, and
gas sampling cylinder in a 100-mL graduated cylinder. Place
1000 = conversion factor to express result in ppm.
50 mL of a crushed ice-distilled water slurry in a 250-mL
Acidity in excess of the amount specified in Table 1 shall
stoppered Erlenmeyer flask, and add the 25 mL of HFC-227ea
constitute failure of this test.
to the slurry. Place the stopper in the flask loosely, and swirl the
6.2.3 Acidity by Universal Indicator:
flask gently from time to time until the ice has melted
6.2.3.1 Apparatus:
completely. Add one drop of methyl red indicator, and if a
6.2.3.2 Fritted Glass Sparger, of coarse porosity, contained
reddish color remains, titrate to a yellow end point with 0.01 N
in a 100-mL glass scrubbing bottle provided with inlet and
sodium hydroxide solution. Run a crushed ice-distilled water
outlet tubes.
blank (with no HFC-227ea) along with the sample.
6.2.3.3 Neoprene Connecting Tubing.
6.2.1.5 Calculation—Calculate parts per million hydrogen
6.2.3.4 Wet Test Meter, 0.1 ft revolution.
fluoride (HF), as follows:
6.2.3.5 Needle Valve Control.
HF, ppm 5 ~A 2 B! 3 N 3 523.7 (3) 7
6.2.3.6 Reagent Universal Indicator, with color chart, or
equivalent.
where:
6.2.3.7 Procedure—Prepare neutralized distilled water by
A = volume of NaOH titrated in sample, mL,
adding 0.4 mL of universal indicator solution to 100 mL of
B = volume of NaOH titrated in the blank, mL
deionized water, and titrate with 0.01 N sodium hydroxide until
N = normality of NaOH, and
the water shows a pH of 7.0 when compared to the Universal
523.7 5 20 3 1000/~1.5277 3 25! (4)
Color Chart. Add 50 mL of the neutralized water to the glass
scrubbing bottle fitted with the glass gas sparger. Attach a
where:
needle valve control to the sample cylinder, and connect the
20 = grams HF/equivalent HF,
cylinder, inverted, to an empty safety trap. Connect the safety
1.5277 = density of HFC-227ea at its boiling point, g/mL,
trap outlet to the scrubbing bottle inlet. Connect the scrubbing
25 = sample size of HFC-227ea, mL, and
bottle outlet to the inlet of the wet test meter. Open the needle
1000 = conversion factor to express result in ppm.
valve slowly and pass 20 L of sample through the scrubber at
Acidity in excess of the amount specified in Table 1 shall
a flow rate of approximately 500 mL/min. Turn off the needle
constitute failure of this test.
valve and disconnect the sample cylinder from the scrubbing
6.2.2 Acidity by Sodium Hydroxide Titration—Alternate
bottle. Transfer 10 to 12 mL of water solution to a clean test
Procedure:
tube. Add 0.3 mL of universal indicator solution and swirl.
6.2.2.1 Reagents:
Read the pH of the solution by comparison with the universal
6.2.2.2 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
6.2.2.3 Methyl Red Indicator, 0.1 % aqueous solution.
analysis may be conducted by the phosphorus pentoxide
6.2.2.4 Procedure—Fill a suitable gas sampling cylinder
method, infrared absorption, electrolytic moisture analysis,
with liquid HFC-227ea, and weigh the cylinder. Place 50 mL of
piezoelectric analyzer, or another acceptable laboratory tech-
a crushed ice-distilled water slurry in a 250-mL 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
...
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