ASTM F1374-92(2020)
(Test Method)Standard Test Method for Ionic/Organic Extractables of Internal Surfaces-IC/GC/FTIR for Gas Distribution System Components (Withdrawn 2023)
Standard Test Method for Ionic/Organic Extractables of Internal Surfaces-IC/GC/FTIR for Gas Distribution System Components (Withdrawn 2023)
SIGNIFICANCE AND USE
4.1 The purpose of this test method is to define a procedure for testing electropolished stainless steel components being considered for installation into a high-purity gas distribution system. Application of this test method is expected to yield comparable data among components tested for the purposes of qualification for this installation.
FIG. 1 Ionic/Organic Contribution Data Table Illustration
FIG. 2 Ionic/Organic Contribution Data Table Illustration
SCOPE
1.1 This test method establishes a procedure for testing components used in ultra-high-purity gas distribution systems for ionic and organic surface residues.
1.2 This test method applies to in-line components containing electronics grade materials in the gaseous form.
1.3 Limitations:
1.3.1 This test method is limited by the sensitivity of the detection instruments and by the available levels of purity in extracting solvents. While the ion and gas chromatographic methods are quantitative, the Fourier transform infrared spectroscopy (FTIR) method can be used as either a qualitative or a quantitative tool. In addition, the gas chromatography (GC) and FTIR methods are used to detect hydrocarbons and halogenated substances that remain as residues on component internal surfaces. This eliminates those materials with high vapor pressures, which are analyzed per the total hydrocarbons test, from this test method.
1.3.2 This test method is intended for use by operators who understand the use of the apparatus at a level equivalent to twelve months of experience.
1.4 The values stated in SI units are to be regarded as the standards. The inch-pound units given in parentheses are for information only.
1.5 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Specific hazard statements are given in Section 6.
1.6 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.
WITHDRAWN RATIONALE
This test method establishes a procedure for testing components used in ultra-high-purity gas distribution systems for ionic and organic surface residues.
Formerly under the jurisdiction of Committee F01 on Electronics, this test method was withdrawn in November 2023. This standard is being withdrawn without replacement because Committee F01 was disbanded.
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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: F1374 − 92 (Reapproved 2020)
Standard Test Method for
Ionic/Organic Extractables of Internal Surfaces-IC/GC/FTIR
for Gas Distribution System Components
This standard is issued under the fixed designation F1374; 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.
INTRODUCTION
Semiconductor clean rooms are serviced by high-purity gas distribution systems. This test method
presentsaprocedurethatmaybeappliedfortheevaluationofoneormorecomponentsconsideredfor
use in such systems.
1. Scope mine the applicability of regulatory limitations prior to use.
Specific hazard statements are given in Section 6.
1.1 This test method establishes a procedure for testing
1.6 This international standard was developed in accor-
components used in ultra-high-purity gas distribution systems
dance with internationally recognized principles on standard-
for ionic and organic surface residues.
ization established in the Decision on Principles for the
1.2 This test method applies to in-line components contain-
Development of International Standards, Guides and Recom-
ing electronics grade materials in the gaseous form.
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
1.3 Limitations:
1.3.1 This test method is limited by the sensitivity of the
2. Referenced Documents
detection instruments and by the available levels of purity in
extracting solvents. While the ion and gas chromatographic
2.1 ASTM Standards:
methods are quantitative, the Fourier transform infrared spec-
E1151Practice for Ion Chromatography Terms and Rela-
troscopy (FTIR) method can be used as either a qualitative or
tionships
a quantitative tool. In addition, the gas chromatography (GC)
2.2 Union Carbide Standard:
and FTIR methods are used to detect hydrocarbons and
Techniques for Measuring Trace Gas Impurities in High
halogenated substances that remain as residues on component
Purity Gases
internal surfaces. This eliminates those materials with high
vaporpressures,whichareanalyzedperthetotalhydrocarbons
3. Terminology
test, from this test method.
3.1 Definitions of Terms Specific to This Standard:
1.3.2 This test method is intended for use by operators who
understand the use of the apparatus at a level equivalent to 3.1.1 spoolpiece—anullcomponent,consistingofastraight
pieceofelectropolishedtubingandappropriatefittings,usedin
twelve months of experience.
place of the test component to establish the baseline.
1.4 The values stated in SI units are to be regarded as the
3.1.2 standard conditions—101.3 kPa, 0.0°C (14.73 psia,
standards. The inch-pound units given in parentheses are for
32.0°F).
information only.
3.1.3 test component—any device being tested, such as a
1.5 This standard does not purport to address all of the
valve, regulator, or filter.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
3.1.4 test fluid blank—a volume of test solvent adequate for
priate safety, health, and environmental practices and deter-
analysis.
1 2
This test method is under the jurisdiction of ASTM Committee F01 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Electronics and is the direct responsibility of Subcommittee F01.10 on Contamina- contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
tion Control. Standards volume information, refer to the standard’s Document Summary page on
Current edition published April 15, 2020. Published May 2020. Originally the ASTM website.
approvedin1992.Lastpreviouseditionapprovedin2012asF1374–92(2012).DOI: Available from Linde Division Union Carbide, 175 E. Park Drive,Tonawanda,
10.1520/F1374-92R20. NY 14151.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
F1374 − 92 (2020)
3.1.4.1 Discussion—This is used to determine the back-
ground impurity concentrations in the test fluid. This fluid is
drawn at the same time as the fluid that is used to fill the spool
piece and test component. It must be held in a container that
does not contaminate the fluid blank.
3.2 Abbreviations:
3.2.1 FTIR—Fourier transform infrared spectroscopy.
3.2.2 GC—gas chromatography.
3.2.3 IC—ion chromatography.
3.2.4 IPA—isopropanol (2-propanol).
3.2.5 MS—mass spectrometry.
3.2.6 ppbv—parts per billion by volume (such as nL/L).
3.2.7 ppbw—parts per billion by weight (such as ng/g).
3.2.8 ppmv—parts per million by volume (such as µL/L).
3.2.9 ppmw—parts per million by weight (such as µg/g).
3.2.10 psid—pounds per square inch differential.
3.2.11 scfm—standard cubic feet per minute.
3.2.12 slpm—standard litre per minute. The gas volumetric
flow rate measured in litres per minute at 0.0°C (32°F) and
101.3 kPa (1 atm).
4. Significance and Use
4.1 The purpose of this test method is to define a procedure
for testing electropolished stainless steel components being
considered for installation into a high-purity gas distribution
system. Application of this test method is expected to yield
comparable data among components tested for the purposes of
qualification for this installation.
5. Apparatus
5.1 Materials:
5.1.1 Test Fluid—Thepurityoffluidusedfortheextractions
will determine the detection limit of the test. Therefore,
extremely high purity fluids are required. At least 18.0 MΩ
FIG. 1 Ionic/Organic Contribution Data Table Illustration
water [corrected for 18°C (64°F)] must be used for the ionic
extractables determination. Total oxidizable carbon must be
lessthan50ppbw.Thewatermustbefilteredthrougha0.2-µm species. The retention times of the various ionic species are
(or finer) filter. Electronics grade (or better) IPA is to be used usedtoidentifythespecies.Theareaundertherespectivepeak
for the organic extractables determination.
yieldsthequantityofthespeciesintheeluant.Thistestmethod
5.1.2 Spool Piece— a straight run of electropolished 316-L uses a column for mono- and polyvalent anions and a column
stainless steel tubing with no restrictions. The length of the formono-andpolyvalentcations.Asuppressorcolumnmaybe
spool piece shall be approximately 200 mm. The spool piece used to increase sensitivity.
should be the same diameter as the test component. 5.2.2 Gas chromatograph—The GC is an analytical instru-
5.1.3 Caps—usedtosealtheendsofthetestcomponentand ment that detects organic species in the gas phase. A liquid
spool piece are to be of 316-L stainless steel. For stub end sample is injected and heated to the vapor phase. The sample
components, 316-L stainless steel compression fittings with is then passed through a column containing an adsorbent. A
nylon or polytetraflouroethylene ferrules are to be used. For carrier gas is used as the mobile phase. The retention times of
face seal fittings, stainless steel gaskets must be used. the various peaks help to identify the organic species.The area
5.1.4 Gloves—made of powder free latex or natural rubber under the respective peak yields the quantity of the species in
and resistant to the test fluids used in this test method. the mobile phase.
5.2 Instrumentation:
NOTE 1—Since the peak of the solvent will be large, it will obscure
thosespeciesthathaveacarbonnumberorretentiontimebelowthatofthe
5.2.1 Ion Chromatograph—The IC is an analytical instru-
solvent.
ment that detects ionic species in deionized (DI) water. The
eluant is passed through a column containing ion exchange 5.2.3 Fourier transform infrared spectrometer—The FTIR
resin. A conductivity detector is used to detect the ionic is an analytical instrument that qualitatively or quantitatively
F1374 − 92 (2020)
FIG. 3 Ionic/Organic Contribution Data Table Illustration
FIG. 2 Ionic/Organic Contribution Data Table Illustration
8.2 Rinse the outside of the spool piece with the test fluid
identifies contaminants based on characteristic frequencies of
(DI water (ionic) or IPA (org
...
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: F1374 − 92 (Reapproved 2020)
Standard Test Method for
Ionic/Organic Extractables of Internal Surfaces-IC/GC/FTIR
for Gas Distribution System Components
This standard is issued under the fixed designation F1374; 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.
INTRODUCTION
Semiconductor clean rooms are serviced by high-purity gas distribution systems. This test method
presents a procedure that may be applied for the evaluation of one or more components considered for
use in such systems.
1. Scope mine the applicability of regulatory limitations prior to use.
Specific hazard statements are given in Section 6.
1.1 This test method establishes a procedure for testing
1.6 This international standard was developed in accor-
components used in ultra-high-purity gas distribution systems
dance with internationally recognized principles on standard-
for ionic and organic surface residues.
ization established in the Decision on Principles for the
1.2 This test method applies to in-line components contain-
Development of International Standards, Guides and Recom-
ing electronics grade materials in the gaseous form.
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee.
1.3 Limitations:
1.3.1 This test method is limited by the sensitivity of the
2. Referenced Documents
detection instruments and by the available levels of purity in
extracting solvents. While the ion and gas chromatographic
2.1 ASTM Standards:
methods are quantitative, the Fourier transform infrared spec-
E1151 Practice for Ion Chromatography Terms and Rela-
troscopy (FTIR) method can be used as either a qualitative or
tionships
a quantitative tool. In addition, the gas chromatography (GC)
2.2 Union Carbide Standard:
and FTIR methods are used to detect hydrocarbons and
Techniques for Measuring Trace Gas Impurities in High
halogenated substances that remain as residues on component
Purity Gases
internal surfaces. This eliminates those materials with high
vapor pressures, which are analyzed per the total hydrocarbons
3. Terminology
test, from this test method.
1.3.2 This test method is intended for use by operators who 3.1 Definitions of Terms Specific to This Standard:
3.1.1 spool piece—a null component, consisting of a straight
understand the use of the apparatus at a level equivalent to
twelve months of experience. piece of electropolished tubing and appropriate fittings, used in
place of the test component to establish the baseline.
1.4 The values stated in SI units are to be regarded as the
3.1.2 standard conditions—101.3 kPa, 0.0°C (14.73 psia,
standards. The inch-pound units given in parentheses are for
32.0°F).
information only.
3.1.3 test component—any device being tested, such as a
1.5 This standard does not purport to address all of the
valve, regulator, or filter.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
3.1.4 test fluid blank—a volume of test solvent adequate for
priate safety, health, and environmental practices and deter-
analysis.
1 2
This test method is under the jurisdiction of ASTM Committee F01 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Electronics and is the direct responsibility of Subcommittee F01.10 on Contamina- contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
tion Control. Standards volume information, refer to the standard’s Document Summary page on
Current edition published April 15, 2020. Published May 2020. Originally the ASTM website.
approved in 1992. Last previous edition approved in 2012 as F1374–92(2012). DOI: Available from Linde Division Union Carbide, 175 E. Park Drive, Tonawanda,
10.1520/F1374-92R20. NY 14151.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
F1374 − 92 (2020)
3.1.4.1 Discussion—This is used to determine the back-
ground impurity concentrations in the test fluid. This fluid is
drawn at the same time as the fluid that is used to fill the spool
piece and test component. It must be held in a container that
does not contaminate the fluid blank.
3.2 Abbreviations:
3.2.1 FTIR—Fourier transform infrared spectroscopy.
3.2.2 GC—gas chromatography.
3.2.3 IC—ion chromatography.
3.2.4 IPA—isopropanol (2-propanol).
3.2.5 MS—mass spectrometry.
3.2.6 ppbv—parts per billion by volume (such as nL/L).
3.2.7 ppbw—parts per billion by weight (such as ng/g).
3.2.8 ppmv—parts per million by volume (such as µL/L).
3.2.9 ppmw—parts per million by weight (such as µg/g).
3.2.10 psid—pounds per square inch differential.
3.2.11 scfm—standard cubic feet per minute.
3.2.12 slpm—standard litre per minute. The gas volumetric
flow rate measured in litres per minute at 0.0°C (32°F) and
101.3 kPa (1 atm).
4. Significance and Use
4.1 The purpose of this test method is to define a procedure
for testing electropolished stainless steel components being
considered for installation into a high-purity gas distribution
system. Application of this test method is expected to yield
comparable data among components tested for the purposes of
qualification for this installation.
5. Apparatus
5.1 Materials:
5.1.1 Test Fluid—The purity of fluid used for the extractions
will determine the detection limit of the test. Therefore,
extremely high purity fluids are required. At least 18.0 MΩ
FIG. 1 Ionic/Organic Contribution Data Table Illustration
water [corrected for 18°C (64°F)] must be used for the ionic
extractables determination. Total oxidizable carbon must be
less than 50 ppbw. The water must be filtered through a 0.2-µm species. The retention times of the various ionic species are
(or finer) filter. Electronics grade (or better) IPA is to be used
used to identify the species. The area under the respective peak
for the organic extractables determination. yields the quantity of the species in the eluant. This test method
5.1.2 Spool Piece— a straight run of electropolished 316-L uses a column for mono- and polyvalent anions and a column
stainless steel tubing with no restrictions. The length of the for mono- and polyvalent cations. A suppressor column may be
spool piece shall be approximately 200 mm. The spool piece used to increase sensitivity.
should be the same diameter as the test component. 5.2.2 Gas chromatograph—The GC is an analytical instru-
5.1.3 Caps—used to seal the ends of the test component and ment that detects organic species in the gas phase. A liquid
spool piece are to be of 316-L stainless steel. For stub end sample is injected and heated to the vapor phase. The sample
components, 316-L stainless steel compression fittings with is then passed through a column containing an adsorbent. A
nylon or polytetraflouroethylene ferrules are to be used. For carrier gas is used as the mobile phase. The retention times of
face seal fittings, stainless steel gaskets must be used. the various peaks help to identify the organic species. The area
5.1.4 Gloves—made of powder free latex or natural rubber under the respective peak yields the quantity of the species in
and resistant to the test fluids used in this test method. the mobile phase.
5.2 Instrumentation:
NOTE 1—Since the peak of the solvent will be large, it will obscure
those species that have a carbon number or retention time below that of the
5.2.1 Ion Chromatograph—The IC is an analytical instru-
solvent.
ment that detects ionic species in deionized (DI) water. The
eluant is passed through a column containing ion exchange 5.2.3 Fourier transform infrared spectrometer—The FTIR
resin. A conductivity detector is used to detect the ionic is an analytical instrument that qualitatively or quantitatively
F1374 − 92 (2020)
FIG. 3 Ionic/Organic Contribution Data Table Illustration
FIG. 2 Ionic/Organic Contribution Data Table Illustration
8.2 Rinse the outside of the spool piece with the test fluid
identifies contaminants based on characteristic frequencies of
(DI water (ionic) or IPA (organic)) to be used for analysis.
absorption of infrared radiation. By identifying combinations
R
...
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