ASTM F1277-02(2009)
(Test Method)Standard Test Method for Determination of Leachable Chloride in Packing and Gasketing Materials by Ion-Selective Electrode Technique (Withdrawn 2018)
Standard Test Method for Determination of Leachable Chloride in Packing and Gasketing Materials by Ion-Selective Electrode Technique (Withdrawn 2018)
SIGNIFICANCE AND USE
Chloride ion is highly detrimental to the valves, flanges, piping, etc. of stainless steel and copper-bearing alloys employed in certain types of facilities, such as nuclear and chemical plants. Therefore, the amount of chloride ion that can be leached from packing and gasketing materials used in these facilities must be controlled closely for prevention of damage. This test method is suitable for manufacturing control and for verifying that the packing and gasketing material meets specifications.
It is assumed that the users of this test method will be analysts capable of performing common laboratory procedures skillfully and safely. It is recommended that the work will be performed in a properly equipped laboratory under appropriate quality control practices such as those described in Guide E882.
SCOPE
1.1 This test method provides for the measurement of chloride ion leached from flexible graphite, asbestos, or paper-based packing and gasketing materials. Samples containing 7 to 6700 μg Cl-/g sample can be analyzed with this procedure. The upper concentration limit can be extended by dilution of the test solution.
1.2 It is the responsibility of the analyst to ensure the validity of this test method for other packing or gasketing materials.
1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
1.4 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. A specific warning statement is given in 8.3.
WITHDRAWN RATIONALE
This test method provides for the measurement of chloride ion leached from flexible graphite, asbestos, or paper-based packing and gasketing materials. Samples containing 7 to 6700 μg Cl-/g sample can be analyzed with this procedure. The upper concentration limit can be extended by dilution of the test solution.
Formerly under the jurisdiction of Committee F03 on Gaskets, this test method was withdrawn in January 2018 in accordance with section 10.6.3 of the Regulations Governing ASTM Technical Committees, which requires that standards shall be updated by the end of the eighth year since the last approval date.
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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: F1277 − 02 (Reapproved 2009)
Standard Test Method for
Determination of Leachable Chloride in Packing and
Gasketing Materials by Ion-Selective Electrode Technique
This standard is issued under the fixed designation F1277; 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 selective electrode in conjunction with a double junction,
sleeve-type reference electrode. Potentials are read using a
1.1 This test method provides for the measurement of
pH/mV meter having 0.1 mV readability.
chloride ion leached from flexible graphite, asbestos, or paper-
based packing and gasketing materials. Samples containing 7
3.2 Acalibration curve is prepared by plotting the potentials
-
to 6700 µg Cl /g sample can be analyzed with this procedure.
of known chloride solutions versus the corresponding concen-
The upper concentration limit can be extended by dilution of
trations expressed in micrograms per millilitre. The chloride
the test solution.
concentration of the test solution is determined from the
1.2 It is the responsibility of the analyst to ensure the calibrationcurve,andthisvalueisusedtocalculatetheamount
validity of this test method for other packing or gasketing
of chloride in parts per million that was leached from the
materials. packing or gasketing material. The calibration and test solu-
tions must be measured at the same temperature [within 61°C
1.3 The values stated in SI units are to be regarded as the
(62°F)].
standard. The values given in parentheses are for information
only.
3.3 The calibration and test solutions are diluted with ionic
1.4 This standard does not purport to address all of the
strength adjustor which also minimizes possible interferences
safety concerns, if any, associated with its use. It is the
such as ammonia, bromide, iodide, cyanide, or sulfide (seeTest
responsibility of the user of this standard to establish appro-
Methods D512).
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. Aspecific warning
4. Significance and Use
statement is given in 8.3.
4.1 Chloride ion is highly detrimental to the valves, flanges,
2. Referenced Documents
piping, etc. of stainless steel and copper-bearing alloys em-
ployed in certain types of facilities, such as nuclear and
2.1 ASTM Standards:
chemical plants.Therefore, the amount of chloride ion that can
D512 Test Methods for Chloride Ion In Water
be leached from packing and gasketing materials used in these
E50 Practices for Apparatus, Reagents, and Safety Consid-
erations for Chemical Analysis of Metals, Ores, and facilities must be controlled closely for prevention of damage.
This test method is suitable for manufacturing control and for
Related Materials
E691 Practice for Conducting an Interlaboratory Study to verifying that the packing and gasketing material meets speci-
fications.
Determine the Precision of a Test Method
E882 Guide for Accountability and Quality Control in the
4.2 It is assumed that the users of this test method will be
Chemical Analysis Laboratory
analysts capable of performing common laboratory procedures
3. Summary of Test Method skillfully and safely. It is recommended that the work will be
performed in a properly equipped laboratory under appropriate
3.1 Chloride ion leached from packing and gasketing mate-
quality control practices such as those described in Guide
rials is measured potentiometrically using a chloride ion-
E882.
This test method is under the jurisdiction ofASTM Committee F03 on Gaskets
andisthedirectresponsibilityofSubcommitteeF03.50onAnalyticalTestMethods. 5. Interferences
Current edition approved Oct. 1, 2009. Published March 2010. Originally
5.1 There is no interference from up to 500 µg/mL of
approved in 1990. Last previous edition approved in 2002 as F1277 – 02. DOI:
10.1520/F1277-02R09.
sulfide, 1000 µg/mL of bromide or iodide, a one hundred-fold
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
excess of cyanide over chloride, or 1000 µg/mL of ammonia.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Ferric, cupric, and permanganate ions do not interfere. Mer-
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. cury must not be present.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
F1277 − 02 (2009)
6. Apparatus 100-mL volumetric flask. Bring the solution in the flask up to
the mark with distilled water and mix thoroughly.
6.1 DigitalpH/mVMeter,with0.1mVreadabilitypreferred,
-
7.1.1.5 5 µg/mL Cl Solution—With a 5-mL volumetric
but 1 mV readability is acceptable.
–
pipet, pipet 5 mL of 100 µg/mL Cl stock solution into a
-
6.2 Chloride Ion-Selective Electrode (Cl) , having a silver
100-mL volumetric flask. Bring the solution in the flask up to
chloride(AgCl)membrane.(Warning—Chlorideion-selective
the mark with distilled water and mix thoroughly.
-
electrodes with a silver chloride/silver sulfide membrane are
7.1.1.6 2.5 µg/mL Cl Solution—With a 25-mL volumetric
-
not suitable as the sulfide can be oxidized by the ionic strength
pipet, pipet 25 mL of 10 µg/mL Cl stock solution into a
adjustor used in this procedure.)
100-mL volumetric flask. Bring the solution in the flask up to
6.3 Sleeve-Type Double Junction Reference Electrode. the mark with distilled water and mix thoroughly.
-
7.1.1.7 1 µg/mL Cl Solution—With a 10-mL volumetric
NOTE 1—Other types of double junction reference electrodes may be
–
pipet, pipet 10 mL of 10 µg/mL Cl stock solution into a
suitable, but supporting data included in this test method were obtained
100-mL volumetric flask. Bring the solution in the flask up to
with only the recommended type.
the mark with distilled water and mix thoroughly.
6.4 Oven.
7.1.1.8 Transfer each solution to a labeled polyethylene
6.5 Desiccator, containing anhydrous calcium sulfate
bottle and cap tightly.
(CaSO ).
7.2 Preparation of Test and Blank Solutions:
6.6 Hot Plate.
(Warning—When preparing packing or gasketing material
samples, precautions should be taken to avoid chloride con-
6.7 Magnetic Stirrer, with polytetrafluorethylene (PTFE)-
tamination from handling. Clean cotton gloves should be
coated stirring bars.
worn.)
6.8 Beakers, 150 and 250-mL graduated capacities.
7.2.1 Cut, with scissors or knife, or tear the packing or
1 1
6.9 Volumetric Flasks, 100, 500, and 1000-mL capacities.
gasketing material into pieces 6 to 12 mm ( ⁄4 to ⁄2 in.) square.
7.2.2 Dry the sample in an oven set at approximately 100°C
6.10 Volumetric Pipets, with 2, 5, 10, 25, and 50-mL
(212°F) for a minimum of 1 h.
capacities.
NOTE 2—If it can be demonstrated that equivalent precision can be
6.11 Graduated Cylinder, 10-mL capacity.
obtained without drying the samples, this step may be eliminated.
6.12 Watch Glasses, with ribs on the bottoms.
7.2.3 Remove the sample from the oven, place in a
6.13 Glass Stirring Rods.
desiccator, and cool to room temperature. Weigh 15 g of
sample material to the nearest 0.01 g, place in a 250-mL
6.14 Glass Funnels.
beaker, and label.
6.15 Filter Paper, with fast filtering rate.
7.2.4 Add 90 mL of distilled water to the beaker. Using a
6.16 Polyethylene Bottles, 150, 500, and 1000-mL capaci-
10-mL graduated cylinder, add 10 mL of 0.1 M NaOH.
ties.
7.2.5 Preparation of Blank Solution—Prepare a blank solu-
tion by adding 90 mL of distilled water and 10 mL of 0.1 M
6.17 Cotton Gloves.
NaOHtoa250-mLbeaker.Treattheblanksolutioninthesame
6.18 Scissors or Knife.
manner as the test solution, but do not stir.
7.2.6 Cover the beaker with a ribbed watch glass and digest
7. Preparation of Reference Materials and Samples
the specimen at 90° 6 5°C (195° 6 10°F) for a minimum of
7.1 Preparation of Calibration Solutions:
4 h. Stir the specimen occasionally (at least once per hour).
7.1.1 Seven solutions shall be prepared in order to calibrate (Warning—Use glass rods to stir specimens during digestion.
thechlorideion-selectiveelectrode.Eachsolutionshallcontain
Using a magnetic stirrer may cause the sample material to
a different concentration of chloride. Prepare the solutions as agglomerate.)
follows:
7.2.7 Remove the test solution from the hot plate and cool.
-
7.1.1.1 500 µg/mL Cl Solution—With a 5-mL volumetric Place a filter paper in a glass funnel and moisten with distilled
-
pipet, pipet 5 mL of 10 000 µg/mL Cl stock solution into a
water. Filter the test solution into a 100-mL volumetric flask.
100-mL volumetric flask. Bring the solution in the flask up to Wash the material in the beaker with about 15 mL of distilled
the mark with distilled water and mix thoroughly.
water and filter washings into flask. Repeat the washing step if
-
7.1.1.2 100 µg/mL Cl Solution—With a 10-mL volumetric possible, but do not let the volume in the flask exceed the
-
pipet, pipet 10 mL of 1000 µg/mL Cl stock solution into a
100-mL mark. Bring the solution in the flask up to 100-mL
100-mL volumetric flask. Bring the solution in the flask up to volume with distilled water and mix thoroughly. (Warning—
the mark with distilled water and mix thoroughly.
Make sure that the sample is washed sufficiently, but the final
-
7.1.1.3 50 µg/mL Cl Solution—With a 5-mL volumetric volume of the test solution must be restricted to 100 mL.)
-
pipet, pipet 5 mL of 1000 µg/mL Cl stock solution into a
8. Reagents and Materials
100-mL volumetric flask. Bring the solution in the flask up to
the mark with distilled water and mix thoroughly. 8.1 Purity and Concentration of Reagents—The purity and
-
7.1.1.4 10 µg/mL Cl Solution—With a 10-mL volumetric concentration of the chemical reagents used shall be in
-
pipet, pipet 10 mL of 100 µg/mL Cl stock solution into a accordance with the requirements prescribed in Practices E50.
F1277 − 02 (2009)
8.2 Solutions for Filling Double Junction Reference Elec- 9. Preparation of Apparatus
trode:
9.1 Prepare and operate the pH/mV meter in accordance
8.2.1 Inner-Chamber Filling Solution, available from the
with the manufacturer’s instructions.
electrode manufacturer.
NOTE3—ItisnotwithinthescopeofanASTMtestmethodtoprescribe
8.2.2 Outer-Chamber Filling Solution—Use the solution
minute details relative to the preparation of the apparatus. For a descrip-
prepared in 8.3. tion and specific details concerning the operation of a particular piece of
equipment, refer to the manufacturer’s manual.
8.3 ChlorideIonicStrengthAdjustor(CISA)—Dissolve 15.1
9.2
...
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