ASTM D6064-11(2015)

Standard Specification for HFC-227ea, 1,1,1,2,3,3,3-Heptafluoropropane (CF<inf>3</inf >CHFCF<inf>3</inf>)

ABSTRACT
This specification covers the requirements for 1,1,1,2,3,3,3-Heptafluoropropane (HFC-227ea) for use as a fire-fighting medium. However, this specification does not include the fire-fighting equipment or hardware that employs HFC-227ea, the conditions for employing such equipment, nor the storage or transportation of HFC-227ea. Material covered by this specification is of two types: Type I (mixtures of HFC-227ea and nitrogen) and Type II (HFC-227ea). Tests for purity, acidity, water content, fluoride ion content, suspended matter and sediment, nonvolatile residue, and fixed gases in the vapor phase shall be performed and shall conform to the requirements specified.
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.

General Information

• Status: Historical
• Publication Date: 31-May-2015
• ICS: 13.220.10 - Fire-fighting
• Technical Committee: D26 - Halogenated Organic Solvents and Fire Extinguishing Agents
• Drafting Committee: D26.09 - Fire Extinguishing Agents

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation:D6064 −11 (Reapproved 2015)
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 3. Terminology
1.1 This specification covers requirements for HFC-227ea 3.1 Definitions of Terms Specific to This Standard:
as a fire-fighting medium. 3.1.1 HFC—hydrofluorocarbon; a chemical compound in
which the compound molecule is comprised exclusively of
1.2 This specification does not address the fire-fighting
hydrogen and fluorine and carbon atoms.
equipment or hardware that employs HFC-227ea or the con-
3.1.2 HFC-227ea—the compound 1,1,1,2,3,3,3-
ditions of employing such equipment (for example, handhelds,
heptafluoropropane; CF CHFCF .
fixed installations, etc.). 3 3
3.1.2.1 Discussion—The terminology system for fluorine-
1.3 This specification does not address the storage or
containing compounds (described in detail in ASRE Stan-
transportation of HFC-227ea. Storage, handling, and transpor-
dard34)providesaconvenientmeanstoreferencethestructure
tation issues may be addressed in futureASTM specifications.
of individual compounds. By definition, the first digit of the
1.4 The values stated in both inch-pound and SI units are to
numbering system represents one less than the number of
be regarded separately as the standard. The values given in
carbon atoms in the compound molecule; the second digit, one
parentheses are for information only.
more than the number of hydrogen atoms in the compound
molecule; and the third digit, the number of fluorine atoms in
1.5 The following safety hazards caveat pertains only to the
the compound molecule. For molecules containing three car-
test methods portion, Section 5, of this specification: This
bon atoms, two appended letters are added to indicate the
standard does not purport to address all of the safety concerns,
symmetry of the molecule. The first appended letter indicates
if any, associated with its use. It is the responsibility of the user
the substitution on the central (C2) carbon; for example, the
of this standard to establish appropriate safety and health
substitution CHF is assigned the designation “e.” The second
practices and determine the applicability of regulatory limita-
appended letter indicates the substitution at the C1 and C3
tions prior to use.SpecifichazardsstatementsaregiveninNote
carbons; for example, identical substitution on the C1 and C3
1.
carbons are assigned the designation “a.” For example, the
2. Referenced Documents designation HFC-227ea indicates three carbon atoms (2+1),
one hydrogen atom (2−1), and seven fluorine atoms; the
2.1 ISO Standards:
designation “e” indicates that the central carbon is substituted
ISO 3363Fluorochlorinated Hydrocarbons for Industrial
as CHF, and the designation“ a” indicates that the substitution
Use-Determination of Acidity-Titrimetric Method
on Carbons C1 and C3 is identical, that is, the structure is
ISO 3427Gaseous Halogenated Hydrocarbons (Liquefied
CF CHFCF .
2 3 3
Gases)–Taking of a Sample
ISO 5789Fluorinated Hydrocarbons for Industrial Use- 4. Material Requirements
Determination of Nonvolatile Residue
4.1 Type I—Mixtures of HFC-227ea and Nitrogen:
2.2 ASRE Standard: 4.1.1 The nitrogen (N ) partial pressure shall be such that
ASRE Standard34
the safe working pressure of the receiving vessel is not
exceeded. To prevent excessive pressure, the fill density of
HFC-227eawithinacontainershouldnotexceedthatneededto
This specification is under the jurisdiction of ASTM Committee D26 on
achieve complete filling of the container at the maximum
Halogenated Organic Solvents and Fire Extinguishing Agents and is the direct
envisagedstoragetemperature.Forexample,fortheU.S.DOT
responsibility of Subcommittee D26.09 on Fire Extinguishing Agents.
4BA500cylinder,thenitrogenpartialpressureshallnotexceed
Current edition approved June 1, 2015. Published June 2015. Originally
3 3
21.8barat21°C(316psigat70°F)fora1150-kg/m (72-lb/ft )
approved in 1996. Last previous edition approved in 2011 as D6064–11. DOI:
10.1520/D6064-11R15.
fill density (yielding a total pressure of 25.8 bar at 21°C (360
Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
psig at 70°F). For this example, the safe working pressure of
4th Floor, New York, NY 10036, http://www.ansi.org.
the 4BA500 cylinder is not exceeded for temperatures below
American Society of Refrigeration Engineers, Refrigeration Engineering 65,
1957, p. 49. 54°C (130°F).
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D6064−11 (2015)
4.1.2 HFC-227ea shall conform to the requirements pre- 6.1.2 Apparatus—The following special apparatus is re-
scribed in Table 1 when tested by the appropriate test meth- quired to determine the percent of HFC-227ea:
od(s) listed in Section 6. 6.1.2.1 Gas Chromatograph, capable of programmed tem-
4.1.3 When a material analysis is required, by agreement perature operation and equipped with a thermal conductivity
betweenthepurchaserandthesupplier,thetotalpressureinthe detector.
HFC-227eacontainer,partialpressureoftheN ,thefilldensity 6.1.2.2 Column, 3.1-m by 5-mm outside diameter (2.6-mm
of HFC-227ea within the container, and the maximum safe inner diameter) glass tubing, packed with 80 to 120 mesh
storage temperature shall be part of the material analysis Carbopack B or equivalent.
(certification).Thepressureshallbereportedinbar(preferred) 6.1.2.3 Gas Sampling Valve, 10-mL volume or a volume
or pound-force per square inch gage. The fill density shall be sufficient to achieve proper separation in the specified column.
reported in kilograms per cubic metre at 21°C (preferred) or 6.1.2.4 GlassSyringe,20-mLHamiltonB-D, orequivalent.
pounds per cubic foot at 70°F. The maximum safe storage 6.1.2.5 Three-Way Purge/Isolation Valve, Hamilton 86727
temperature of the HFC-227ea container shall be reported in miniature inert valve with Luer Lock fittings, or equivalent.
degrees Celsius (preferred) or in degrees Fahrenheit and shall 6.1.3 Reagents—The carrier gas shall be a chromatographic
conformtoapplicableregulationsfortheHFC-227eacontainer grade of helium. The column packing shall consist of a
design and use. standard solution, for example 3% (weight/weight) methyl
5 5
silicone, on 80 to 120-mesh Carbopack B (or equivalent).
4.2 Type II—HFC-227ea—HFC-227ea shall conform to the
6.1.4 Procedure:
requirements of Type I, as listed in 3.1, and shall contain no
6.1.4.1 Install the column and adjust the temperature of the
more than 1.5% by volume fixed gases in vapor phase,
column oven to 30°C, injection port to 100°C, and detector
expressed as air when tested by the appropriate test method(s)
blockto150°C.Thetemperatureshouldbeprogrammedtorise
listed in Section 6.
10 to 15°C/min (from an initial temperature of 30°C), to a
4.3 By agreement between the purchaser and the supplier,
maximum of 100°C.
analysismayberequiredandlimitsestablishedforelementsor
6.1.4.2 Adjust the helium flow to 25 mL/min.
compounds not specified in Table 1.
6.1.4.3 Adjust the detector voltage to 8 V or to the mid-
range of the thermal conductivity detector (TCD) instrument
4.4 Unless otherwise specified, Type II is assumed.
being used and allow the instrument to stabilize.
NOTE1—ProlongedexposuretoconcentrationsofHFC-227eainexcess
6.1.4.4 Take the sample from the vapor phase; collect
of 10.5% by volume in air during periods of elevated adrenaline could
approximately 20 mL in the glass syringe.
produce cardiac arrhythmia in some personnel.
6.1.4.5 Purge the sample loop with approximately 10 mLof
5. Sampling
sample from the syringe and transfer the sample into the
chromatographic system.
5.1 Samples of HFC-227ea, taken from the liquid phase,
6.1.4.6 Allow the sample to elute, for approximately 18
shall be taken from filled containers in accordance with the
min, attenuating as necessary to make the peak heights a
method specified in ISO 3427. The sampling cylinder shall be
convenient size. Under proper instrument settings, the HFC-
capable of safely resisting the vapor pressure of the sample at
227ea should elute after approximately 5 min.
the highest temperature that could be encountered.
6.1.5 Calculation:
5.2 TheHFC-227easelectedinaccordancewith5.1shallbe
6.1.5.1 Calculate percent HFC-227ea as follows:
tested for quality conformance in accordance with Section 6.
A CF CHFCF 3100
~ !
3 3
The presence of one or more defects shall be cause for
%HFC 2227ea 5 (1)
As
rejection.
where:
6. Test Methods
A(CF CHFCF ) = area of the HFC-227ea peak, and
3 3
6.1 Purity: As = sum of the area of all peaks, excluding
the nitrogen peak.
6.1.1 Determine the purity by gas-liquid chromatography in
accordance with the technique described in 6.1.2 – 6.1.5 or
Percent HFC-227ea below that specified in Table 1 shall
another acceptable laboratory technique providing equivalent
constitute failure of this test method.
results.
6.1.5.2 Calculate percent nitrogen as follows:
An 3100
%N 5 (2)
As
TABLE 1 Requirements
where:
Property Requirement
An = area of nitrogen peak, and
HFC-227ea purity 99.0 %, mol/mol, min
As = sum of the area of all other peaks, including the
Acidity (exclusive of any N present)
2.0 ppm by mass, as HCL, max
nitrogen peak.
Water content ppm by mass, max 10 ppm by mass, max
Nonvolatile residue 0.05 g/100 mL, max
Halogen ion passes test
Suspended matter or sediment none visible Available from Alltech, 2051 Waukegan Road, Deerfield, IL 60015.
Available from Hamilton Co., P.O. Box 10030, Reno, NV 89520-0012.
D6064−11 (2015)
It is useful to calculate percent nitrogen in order to judge a scrubbing bottle fitted with the glass gas sparger. Attach a
safe fill density. needle valve control to the sample cylinder, and connect the
cylinder, inverted, to an empty safety trap. Connect the safety
6.2 Acidity—Vaporize a large sample, in the presence of
trap outlet to the scrubbing bottle inlet. Connect the scrubbing
distilled water. Determine the acidity of the solution by the
bottle outlet to the inlet of the wet test meter. Open the needle
appropriate method described in ISO 3363, 6.2.1 of this
valve slowly and pass 20 L of sample through the scrubber at
standard, 6.2.2 of this standard, a pH indicator, or another
a flow rate of approximately 500 mL/min. Turn off the needle
acceptable laboratory technique providing equivalent results.
valve and disconnect the sample cylinder from the scrubbing
6.2.1 Acidity by Sodium Hydroxide Titration:
bottle. Transfer 10 to 12 mL of water solution to a clean test
6.2.1.1 Reagents:
tube. Add 0.3 mL of universal indicator solution and swirl.
6.2.1.2 Sodium Hydroxide, 0.01 N solution, standardized
Read the pH of the solution by comparison with the universal
with reagent grade potassium hydrogen phthalate, or standard-
color chart. Report the pH reading. No observable change in
ized by the supplier.
pH indicates an acidity of less than 3.0 ppm.
6.2.1.3 Methyl Red Indicator, 0.1% aqueous solution.
6.2.1.4 Procedure—Fill a suitable gas sampling cylinder
6.3 Water Content—Test HFC-227ea for water content.The
withliquidHFC-227ea,andweighthecylinder.Place50mLof
analysis may be conducted by the phosphorus pentoxide
a crushed ice-distilled water slurry in a 250-mL stoppered
method, infrared absorption, electrolytic moisture analysis,
Erlenmeyer flask, slowly add the HFC-227ea under the slurry
piezoelectric analyzer, or another acceptable laboratory tech-
surface, and then reweigh the sample cylinder. Place the
nique. The accuracy of the results and the standard method
stopperintheflasklooselyandswirltheflaskgentlyfromtime
should be by orthodox Karl Fischer method. Water content
to time until the ice has melted completely. Add one drop of
greater than specified in Table 1 shall constitute failure of this
methyl red indicator, and if a reddish color remains, titrate to a
test.
yellow endpoint with 0.01 N sodium hydroxide solution. Run
6.4 Qualitative Test for Fluoride Ion—Test a sample for the
a crushed ice-distilled water blank (with no HFC-227ea) along
presence of fluoride ions in accordance with 6.4.1 through
with the sample.
6.4.3 or by another acceptable laboratory technique providing
6.2.1.5 Calculation—Calculate parts per million hydrogen
equivalent results. Generally, a sample treated with a saturated
chloride as follows:
aqueous solution of calcium chloride shall exhibit no turbidity
HCl, ppm 5 A 2 B 3N 30.03645 310 weight of sample, g (3)
~ !
or precipitation of calcium fluoride.
6.4.1 Apparatus:
where:
6.4.1.1 Fritted Glass Gas Sparger, of coarse or A porosity,
A = volume of NaOH titrated in sample, mL,
contained in a 100-mL glass scrubbing bottle provided with
B = volume of NaOH titrated in the blank, mL,
N = normality of NaOH, inlet and outlet tubes.
W = weight of HFC-227ea, g, and
6.4.1.2 Neoprene Tubing.
6.4.1.3 Wet Test Meter,0to1ft /revolution.
where:
6.4.1.4 Needle Valve Control.
0.03645 × 10 = factortoexpressresultasppmHCl(hydro-
6.4.2 Reagents:
gen chloride).
6.4.2.1 Calcium Chloride, saturated solution in water.
Acidity in excess of the amount specified in Table 1 shall
6.4.3 Procedure—Add 10 mLof saturated calcium chloride
constitute failure of this test.
solution to the scrubber assembly. Attach a needle valve
6.2.2 Acidity by Universal Indicator:
control to the sample cylinder. Connect the sample cylinder in
6.2.2.1 Apparatus:
the upright position to an empty safety trap with neoprene
6.2.2.2 Fritted Glass Sparger, of coarse porosity, contained
tubing. Connect the outlet of the safety trap to the inlet of the
in a 100-mL glass scrubbing bottle provided with inlet and
scrubbing bottle assembly with neoprene tubing. Connect the
outlet tubes.
outlet of the scrubbing bottle assembly to the inlet of the wet
6.2.2.3 Neoprene Connecting Tubing.
test meter. Open the needle valve slowly and pass approxi-
6.2.2.4 Wet Test Meter, 0.1 ft revolution.
mately 2 L of sample through the scrubber at a flow rate of
6.2.2.5 Needle Valve Control.
approximately 100 mL/min. Turn off the needle valve and
6.2.2.6 Reagent Universal Indicator, with color chart, or
disconnectthescrubberassemblyfromthesamplecylinderand
equivalent.
the wet test meter. Examine the contents of the scrubber
6.2.2.7 Procedure—Prepare neutralized distilled water by
visually for the presence of turbidity. Report the fluoride
adding 0.4 mL of universal indicator solution to 100 mL
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: D6064 − 11 D6064 − 11 (Reapproved 2015)
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. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. 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.
2. Referenced Documents
2.1 ISO Standards:
ISO 3363 Fluorochlorinated Hydrocarbons for Industrial Use-Determination of Acidity-Titrimetric Method
ISO 3427 Gaseous Halogenated Hydrocarbons (Liquefied Gases)–Taking of a Sample
ISO 5789 Fluorinated Hydrocarbons for Industrial Use-Determination of Nonvolatile Residue
2.2 ASRE Standard:
ASRE Standard 34
3. Terminology
3.1 Definitions of Terms Specific to This Standard:
3.1.1 HFC—hydrofluorocarbon; a chemical compound in which the compound molecule is comprised exclusively of hydrogen
and fluorine and carbon atoms.
3.1.2 HFC-227ea—the compound 1,1,1,2,3,3,3-heptafluoropropane; CF CHFCF .
3 3
This specification is under the jurisdiction of ASTM Committee D26 on Halogenated Organic Solvents and Fire Extinguishing Agents and is the direct responsibility
of Subcommittee D26.09 on Fire Extinguishing Agents.
Current edition approved Aug. 1, 2011June 1, 2015. Published September 2011June 2015. Originally approved in 1996. Last previous edition approved in 20032011 as
D6064–03.–11. DOI: 10.1520/D6064-11.10.1520/D6064-11R15.
Available from American National Standards Institute, 11 W. 42nd St., 13thInstitute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036.10036, http://www.ansi.org.
American Society of Refrigeration Engineers, Refrigeration Engineering 65, 1957, p. 49.
3.1.2.1 Discussion—
The terminology system for fluorine-containing compounds (described in detail in ASRE Standard 34) provides a convenient
means to reference the structure of individual compounds. By definition, the first digit of the numbering system represents one less
than the number of carbon atoms in the compound molecule; the second digit, one more than the number of hydrogen atoms in
the compound molecule; and the third digit, the number of fluorine atoms in the compound molecule. For molecules containing
three carbon atoms, two appended letters are added to indicate the symmetry of the molecule. The first appended letter indicates
the substitution on the central (C2) carbon; for example, the substitution CHF is assigned the designation “e.” The second appended
letter indicates the substitution at the C1 and C3 carbons; for example, identical substitution on the C1 and C3 carbons are assigned
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D6064 − 11 (2015)
the designation “a.” For example, the designation HFC-227ea indicates three carbon atoms (2 + 1), one hydrogen atom (2−1), and
seven fluorine atoms; the designation “e” indicates that the central carbon is substituted as CHF, and the designation“ a” indicates
that the substitution on Carbons C1 and C3 is identical, that is, the structure is CF CHFCF .
3 3
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 the safe working pressure of the receiving vessel is not exceeded. To
prevent excessive pressure, the fill density of HFC-227ea within a container should not exceed that needed to achieve complete
filling of the container at the maximum envisaged storage temperature. For example, for the U.S. DOT 4BA500 cylinder, the
3 3
nitrogen partial pressure shall not exceed 21.8 bar at 21°C (316 psig at 70°F) for a 1150-kg/m (72-lb/ft ) fill density (yielding a
total pressure of 25.8 bar at 21°C (360 psig at 70°F). For this example, the safe working pressure of the 4BA500 cylinder is not
exceeded for temperatures below 54°C (130°F).
4.1.2 HFC-227ea shall conform to the requirements prescribed in Table 1 when tested by the appropriate test method(s) listed
in Section 6.
4.1.3 When a material analysis is required, by agreement between the purchaser and the supplier, the total pressure in the
HFC-227ea container, partial pressure of the N , the fill density of HFC-227ea within the container, and the maximum safe storage
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 be reported in kilograms per cubic metre at 21°C (preferred) or pounds per cubic foot
at 70°F. The maximum safe storage temperature of the HFC-227ea container shall be reported in degrees Celsius (preferred) or
in degrees Fahrenheit and shall conform to applicable regulations for the HFC-227ea container design and use.
4.2 Type II—HFC-227ea—HFC-227ea shall conform to the requirements of Type I, as listed in 3.1, and shall contain no more
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 elements or
compounds not specified in Table 1.
4.4 Unless otherwise specified, Type II is assumed.
NOTE 1—Prolonged exposure to concentrations of HFC-227ea in excess of 10.5 % by volume in air during periods of elevated adrenaline could produce
cardiac arrhythmia in some personnel.
5. Sampling
5.1 Samples of HFC-227ea, taken from the liquid phase, shall be taken from filled containers in accordance with the method
specified in ISO 3427. The sampling cylinder shall be capable of safely resisting the vapor pressure of the sample at the highest
temperature that could be encountered.
5.2 The HFC-227ea selected in accordance with 5.1 shall be tested for quality conformance in accordance with Section 6. The
presence of one or more defects shall be cause for rejection.
6. Test Methods
6.1 Purity:
TABLE 1 Requirements
Property Requirement
HFC-227ea purity 99.0 %, mol/mol, min
Acidity (exclusive of any N present)
2.0 ppm by mass, as HCL, max
Water content ppm by mass, max 10 ppm by mass, max
Nonvolatile residue 0.05 g/100 mL, max
Halogen ion passes test
Suspended matter or sediment none visible
TABLE 1 Requirements
Property Requirement
HFC-227ea purity 99.0 %, mol/mol, min
Acidity (exclusive of any N present)
2.0 ppm by mass, as HCL, max
Water content ppm by mass, max 10 ppm by mass, max
Nonvolatile residue 0.05 g/100 mL, max
Halogen ion passes test
Suspended matter or sediment none visible
D6064 − 11 (2015)
6.1.1 Determine the purity by gas-liquid chromatography in accordance with the technique described in 6.1.2 – 6.1.5 or another
acceptable laboratory technique providing equivalent results.
6.1.2 Apparatus—The following special apparatus is required to determine the percent of HFC-227ea:
6.1.2.1 Gas Chromatograph, capable of programmed temperature operation and equipped with a thermal conductivity detector.
6.1.2.2 Column, 3.1-m by 5-mm outside diameter (2.6-mm inner diameter) glass tubing, packed with 80 to 120 mesh Carbopack
B or equivalent.
6.1.2.3 Gas Sampling Valve, 10-mL volume or a volume sufficient to achieve proper separation in the specified column.
6.1.2.4 Glass Syringe, 20-mL Hamilton B-D, or equivalent.
6.1.2.5 Three-Way Purge/Isolation Valve, Hamilton 86727 miniature inert valve with Luer Lock fittings, or equivalent.
6.1.3 Reagents—The carrier gas shall be a chromatographic grade of helium. The column packing shall consist of a standard
5 5
solution, for example 3 % (weight(weight/weight)⁄weight) methyl silicone, on 80 to 120-mesh Carbopack B (or equivalent).
6.1.4 Procedure:
6.1.4.1 Install the column and adjust the temperature of the column oven to 30°C, injection port to 100°C, and detector block
to 150°C. The temperature should be programmed to rise 10 to 15°C/min (from an initial temperature of 30°C), to a maximum
of 100°C.
6.1.4.2 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) instrument being used
and allow the instrument to stabilize.
6.1.4.4 Take the sample from the vapor phase; collect approximately 20 mL in the glass syringe.
6.1.4.5 Purge the sample loop with approximately 10 mL of sample from the syringe and transfer the sample into the
chromatographic system.
6.1.4.6 Allow the sample to elute, for approximately 18 min, attenuating as necessary to make the peak heights a convenient
size. Under proper instrument settings, the HFC-227ea should elute after approximately 5 min.
6.1.5 Calculation:
6.1.5.1 Calculate percent HFC-227ea as follows:
A CF CHFCF 3100
~ !
3 3
%HFC 2 227ea 5 (1)
As
where:
A(CF CHFCF ) = area of the HFC-227ea peak, and
3 3
As = sum of the area of all peaks, excluding the nitrogen peak.
Percent HFC-227ea below that specified in Table 1 shall constitute failure of this test method.
6.1.5.2 Calculate percent nitrogen as follows:
An 3100
%N 5 (2)
As
where:
An = area of nitrogen peak, and
As = sum of the area of all other peaks, including the nitrogen peak.
It is useful to calculate percent nitrogen in order to judge a safe fill density.
6.2 Acidity—Vaporize a large sample, in the presence of distilled water. Determine the acidity of the solution by the appropriate
method described in ISO 3363, 6.2.1 of this standard, 6.2.2 of this standard, a pH indicator, or another acceptable 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, standardized with reagent grade potassium hydrogen phthalate, or standardized by
the supplier.
6.2.1.3 Methyl Red Indicator, 0.1 % aqueous solution.
6.2.1.4 Procedure—Fill a suitable gas sampling cylinder with liquid HFC-227ea, and weigh the cylinder. Place 50 mL of a
crushed ice-distilled water slurry in a 250-mL stoppered Erlenmeyer flask, slowly add the HFC-227ea under the slurry surface, and
then reweigh the sample cylinder. Place the stopper in the flask loosely and swirl the flask gently from time to time until the ice
has melted completely. Add one drop of methyl red indicator, and if a reddish color remains, titrate to a yellow endpoint with 0.01
N sodium hydroxide solution. Run a crushed ice-distilled water blank (with no HFC-227ea) along with the sample.
6.2.1.5 Calculation—Calculate parts per million hydrogen chloride as follows:
Available from Alltech, 2051 Waukegan Road, Deerfield, IL 60015.
Available from Hamilton Co., P.O. Box 10030, Reno, NV 89520-0012.
D6064 − 11 (2015)
HCl, ppm 5 A 2 B 3N 30.03645 310 weight of sample, g (3)
~ !
where:
A = volume of NaOH titrated in sample, mL,
B = volume of NaOH titrated in the blank, mL,
N = normality of NaOH,
W = weight of HFC-227ea, g, and
where:
0.03645 × 10 = factor to express result as ppm HCl (hydrogen chloride).
Acidity in excess of the amount specified in Table 1 shall constitute failure of this test.
6.2.2 Acidity by Universal Indicator:
6.2.2.1 Apparatus:
6.2.2.2 Fritted Glass Sparger, of coarse porosity, contained in a 100-mL glass scrubbing bottle provided with inlet and outlet
tubes.
6.2.2.3 Neoprene Connecting Tubing.
6.2.2.4 Wet Test Meter, 0.1 ft revolution.
6.2.2.5 Needle Valve Control.
6.2.2.6 Reagent Universal Indicator, with color chart, or equivalent.
6.2.2.7 Procedure—Prepare neutralized distilled water by adding 0.4 mL of universal indicator solution to 100 mL of deionized
water, and titrate with 0.01 N sodium hydroxide until the water shows a pH of 7.0 when compared to the Universal Color Chart.
Add 50 mL of the neutralized water to the glass scrubbing bottle fitted with the glass gas sparger. Attach a needle valve control
to the sample cylinder, and connect the cylinder, inverted, to an empty safety trap. Connect the safety trap outlet to the scrubbing
bottle inlet. Connect the scrubbing bottle outlet to the inlet of the wet test meter. Open the needle valve slowly and pass 20 L of
sample through the scrubber at a flow rate of approximately 500 mL/min. Turn off the needle valve and disconnect the sample
cylinder from the scrubbing bottle. Transfer 10 to 12 mL of water solution to a clean test tube. Add 0.3 mL of universal indicator
solution and swirl. Read the pH of the solution by comparison with the universal color chart. Report the pH reading. No observable
change in pH indicates an acidity of less than 3.0 ppm.
6.3 Water Content—Test HFC-227ea for water content. The analysis may be conducted by the phosphorus pentoxide method,
infrared absorption, electrolytic moisture analysis, piezoelectric analyzer, or another acceptable laboratory technique. The accuracy
of the results and the standard method should be by orthodox Karl Fischer method. Water content greater than specified in Table
1 shall constitute failure of this test.
6.4 Qualitative Test for Fluoride Ion—Test a sample for the presence of fluoride ions in accordance with 6.4.1 through 6.4.3
or by another acceptable laboratory technique providing equivalent results. Generally, a sample treated with a saturated aqueous
solution of calcium chloride shall exhibit no turbidity or precipitation of calcium flu
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