ASTM F1396-93(2020)
(Test Method)Standard Test Method for Determination of Oxygen Contribution by Gas Distribution System Components (Withdrawn 2023)
Standard Test Method for Determination of Oxygen Contribution by Gas Distribution System Components (Withdrawn 2023)
SIGNIFICANCE AND USE
3.1 This test method defines a procedure for testing 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 purposes of qualification for this installation.
SCOPE
1.1 This test method covers a procedure for testing components for oxygen contribution to ultra-high purity gas distribution systems at ambient temperature. In addition, this test method allows testing of the component at elevated ambient temperatures as high as 70°C.
1.2 This test method applies to in-line components containing electronics grade materials such as those used in a semiconductor gas distribution system.
1.3 Limitations:
1.3.1 This test method is limited by the sensitivity of current instrumentation, as well as the response time of the instrumentation. This test method is not intended to be used for test components larger than 12.7-mm (1/2-in.) outside diameter nominal size. This test method could be applied to larger components; however, the stated volumetric flow rate may not provide adequate mixing to ensure a representative sample. Higher flow rates may improve the mixing but excessively dilute the sample.
1.3.2 This test method is written with the assumption that the operator understands the use of the apparatus at a level equivalent to six months of experience.
1.4 The values stated in SI units are to be regarded as the standard. 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 5.
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WITHDRAWN RATIONALE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 covers a procedure for testing components for oxygen contribution to ultra-high purity gas distribution systems at ambient temperature. In addition, this test method allows testing of the component at elevated ambient temperatures as high as 70°C.
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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Standards Content (Sample)
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: F1396 − 93 (Reapproved 2020)
Standard Test Method for
Determination of Oxygen Contribution by Gas Distribution
System Components
This standard is issued under the fixed designation F1396; 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 5.
1.1 This test method covers a procedure for testing compo-
1.6 This international standard was developed in accor-
nents for oxygen contribution to ultra-high purity gas distribu-
dance with internationally recognized principles on standard-
tion systems at ambient temperature. In addition, this test
ization established in the Decision on Principles for the
method allows testing of the component at elevated ambient
Development of International Standards, Guides and Recom-
temperatures as high as 70°C.
mendations issued by the World Trade Organization Technical
1.2 This test method applies to in-line components contain-
Barriers to Trade (TBT) Committee.
ing electronics grade materials such as those used in a
semiconductor gas distribution system.
2. Terminology
1.3 Limitations:
2.1 Definitions:
1.3.1 Thistestmethodislimitedbythesensitivityofcurrent
2.1.1 baseline—the instrument response under steady state
instrumentation, as well as the response time of the instrumen-
conditions.
tation. This test method is not intended to be used for test
components larger than 12.7-mm ( ⁄2-in.) outside diameter
2.1.2 glove bag—an enclosure that contains a controlled
nominal size. This test method could be applied to larger atmosphere. A glove box could also be used for this test
components; however, the stated volumetric flow rate may not
method.
provide adequate mixing to ensure a representative sample.
2.1.3 heat trace— heating of a component, spool piece, or
Higher flow rates may improve the mixing but excessively
teststandbyauniformandcompletewrappingoftheitemwith
dilute the sample.
resistant heat tape.
1.3.2 This test method is written with the assumption that
2.1.4 minimum detection limit (MDL) of the instrument—the
the operator understands the use of the apparatus at a level
lowest instrument response detectable and readable by the
equivalent to six months of experience.
instrument, and at least two times the amplitude of the noise.
1.4 The values stated in SI units are to be regarded as the
2.1.5 response time—the time required for the system to
standard. The inch-pound units given in parentheses are for
information only. reach steady state after a change in concentration.
1.5 This standard does not purport to address all of the
2.1.6 spool piece—a null component, consisting of a
safety concerns, if any, associated with its use. It is the
straightpieceofelectropolishedtubingandappropriatefittings,
responsibility of the user of this standard to establish appro-
used in place of the test component to establish the baseline.
priate safety, health, and environmental practices and deter-
2.1.7 standard conditions—101.3 kPa, 0.0°C (14.73 psia,
32°F).
This test method is under the jurisdiction of ASTM Committee F01 on
2.1.8 test component—any device being tested, such as a
Electronicsand is the direct responsibility of Subcommittee F01.10 on Contamina-
valve, regulator, or filter.
tion Control.
Current edition approved April 15, 2020. Published May 2020. Originally
2.1.9 test stand—the physical test system used to measure
approved in 1992. Last previous edition approved in 2012 as F1396 – 93(2012).
DOI: 10.1520/F1396-93R20. impurity levels.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
F1396 − 93 (2020)
2.1.10 zero gas—a purified gas that has an impurity concen- around each component for the duration of the test. In the case
tration below the MDLof the analytical instrument.This gas is of long pieces of electropolished tubing, use two glove bags,
to be used for both instrument calibration and component one at each end.
testing.
4.1.3 Tubing, used downstream of the test component shall
be 316L electropolished stainless steel seamless tubing. The
2.2 Symbols:
diameter of the sample line to the analyzer shall not be larger
2.2.1 P —The inlet pressure measured upstream of the
than 6.4 mm ( ⁄4 in.).The length of the sample line from the tee
purifier and filter in the test apparatus.
(installed upstream of the pressure gage P ) to the analyzer
2.2.2 P —The outlet pressure measured downstream of the
shall not be more than 600 mm, so as to minimize the effect
analyzer in the test apparatus.
(adsorption/desorption) of the sample line on the result. The
2.2.3 ppbv—Parts per billion by volume assuming ideal gas
sample line shall have no more than two mechanical joints.
behavior, equivalent to nmole/mole (such as nL/L). The same
4.1.4 Valves, diaphragm or bellows type, capable of unim-
as molar parts per billion (ppb).
paired operation at 94°C (200°F). The use of all-welded,
2.2.4 ppbw—Parts per billion by weight (such as ng/g). all-metal valves is preferred.
2.2.5 ppmv—Parts per million by volume assuming ideal
4.2 Instrumentation:
gas behavior, equivalent to µmole/mole (such as µL/L). The
4.2.1 Oxygen Analyzer—The oxygen analyzer is to be
same as molar parts per million (ppm).
placed downstream of the test component. Accurate baseline
2.2.6 ppmw—Parts per million by weight (such as µg/g). readings must be obtained prior to and subsequent to each of
the tests. Excessive deviations in baseline levels (610 ppbv)
2.2.7 Q —the bypass sample flow not going through the
before or after the tests require that all results be rejected. The
analytical system.
analyzer must be capable of accurately recording changes in
2.2.8 Q —the total sample flow through the analytical
oxygen concentrations on a real time basis.
system.
4.2.2 Oxygen Analyzer Calibration—Zero gas shall be at an
2.2.9 Q —the flow through the spool piece or component.
s
oxygen level below the MDL of the instrument, supplied by
2.2.10 T —the temperature of the air discharged by the purifiedgas,withthepurifierincloseproximitytotheanalyzer.
a
analyzer’s cooling exhaust.
The instrument’s internal standard, if available, is to be used
for the span calibration.Alternatively, span gas from a cylinder
2.2.11 T —the temperature of the spool piece or component.
s
may be used.
2.2.11.1 Discussion—Precautions must be taken to insure
that the temperature measured by the thermocouple is as close
4.3 Pressure and Flow Control—Upstream pressure is to be
as possible to that of the spool piece and test component.
controlled with a regular upstream of the test component. Flow
Appropriate insulation and conductive shield should be used to
is to be controlled at a point downstream of the sampling port
achieve as uniform a temperature as possible. The thermo-
and monitored at that point.Amass flow controller is preferred
couple must be in contact with the outside wall of the
for maintaining the flow as described in 7.4. Sampling is to be
component or spool piece.
performed via a tee in the line, with a section of straight tubing
2.2.12 V-1, V-2—inlet and outlet valves of bypass loop, before the mass flow controller. All lines must conform to
respectively. 4.1.3. Inlet pressure is monitored by P .Test flow is the sum of
Q and Q . Q is directly controlled, and Q is the measured
1 2 1 2
2.2.13 V-3, V-4—inlet and outlet valves of test loop, respec-
flow through the analyzer. Refer to Fig. 1.
tively.
4.4 Bypass Loop—The design of the bypass loop is not
3. Significance and Use
restrictedtoanyonedesign.Itcouldbe,forexample,a3.2-mm
3.1 This test method defines a procedure for testing compo- ( ⁄8-in) 316L stainless steel coil or a flexible tube section. This
allows the flexibility necessary to install test components of
nents being considered for installation into a high-purity gas
distribution system.Application of this test method is expected different lengths.
to yield comparable data among components tested for pur-
poses of qualification for this installation.
4. Apparatus
4.1 Materials:
4.1.1 Nitrogen or Argon, clean and dry, as specified in 7.5.
4.1.2 Spool Piece, that can be installed in place of the test
component is required. This piece is to be a straight section of
316Lelectropolished stainless steel tubing with no restrictions.
The length of the spool piece shall be 200 mm.The spool piece
has the same end connections as the test component.
4.1.2.1 Components With Stub Ends—Use compression fit-
tings with nylon or teflon ferrules to connect the spool piece
and test component to the test loop. Keep the purged glove bag FIG. 1 Test Schematic
F1396 − 93 (2020)
5. Hazards of the test apparatus during the installation and removal of the
spool piece and the test piece.
5.1 It is required that the user have a working knowledge of
the respective instrumentation and that the user practice proper 8.3 A trace oxygen analyzer capable of detecting oxygen
handling of test components for trace oxygen analysis. Good concentration levels down to 2 ppb is connected to the test
laboratory practices must also be understood. stand to sample the gas flowing through the test piece. The
purified and filtered base gas from the test stand containing <
5.2 It is required that the user be familiar with proper
10 ppb oxygen is used as the zero oxygen gas source for the
component installation, and that the test components be in-
analyzer.Sincetheanalyzerissensitivetothesampleflowrate,
stalled on the test stand in accordance with manufacturer’s
the metering valves within the analyzer should be adjusted to
instructions.
yield the flow rates required by the specification for an inlet
5.3 Do not exceed ratings (such as pressure, temperature,
pressure of 30 psig. The gas flow rate Q is set to 1 L/min.
s
and flow) of component.
8.4 Inlet gas pressure is controlled by a pressure regulator
5.4 Gloves are to be worn for all steps.
and measured immediately upstream of the purifier by an
electronic grade pressure gage. Flow measurement is carried
5.5 Limit exposure of the instrument and test component to
atmospheric contamination before and during the test. outbyamassflowcontroller(MFC)locateddownstreamofthe
analyzer. The outlet pressure of the gas is measured immedi-
6. Calibration
ately downstream of the analyzer by another electronic grade
pressure gage. The MFC along with its digital readout should
6.1 Calibrate instruments using standard laboratory prac-
be calibrated before use to control and display the gas flow rate
tices and manufacturer’s recommendations.
Q .
7. Conditioning
8.5 The temperature of the spool piece, test specimen,
7.1 Ensure that adequate mixing of the test gas is attained. analyzer cell compartment, and the oxygen concentration
measured by the analyzer can either be recorded continuously
7.2 Pressure—Test component at 200 kPa gage (30 psig)
by a 25 channel data logger or collected and stored in a
measured at P .
computer using a data acquisition program.
7.3 Temperature— T is to be in the ambient temperature
s
range of 18 to 26°C (64 to 78°F) and in the higher mean
9. Procedure (see Fig. 2)
temperature range of 69 to 71°C (156 to 160°F). T must not
a
9.1 Bake-Out—With the spool piece installed and valves
deviate more than 6 2°C (4°F) from the time of calibration to
V-1, V-2, V-3, and V-4 open, bake out the system (downstream
the termination of the test. T must either be within the range
a
of purifier to upstream of analyzer, exclusive of the exhaust
of 18 to 26°C (64 to 78°F) or be consistent with the analytical
leg) at 94°C (200°F) until outlet oxygen concentration is stable
systems manufacturer’s specifications, whichever is more
below <20 ppbv. Flow of the gas is specified in 7.4. Cool to
stringent.
lower T . Close valves V-1 and V-2.
s
7.4 The flow rate Q for components is 1 standard L/min
s
9.2 Baseline—Flowgasthroughtheteststandwiththespool
with 6 2 % tolerance.
piece installed on the test stand. Use the flow rate as defined in
7.5 The test gas shall be purified nitrogen or argon with a
7.4. Flow for 30 min after the oxygen concentration has
maximum oxygen concentration not exceeding an oxygen
attained a level of <20 ppbv. Utilizing heat tape, heat the spool
concentration of 10 ppb. Gas quality must be maintained at
piece and upstream tubing to within 80 mm of the upstream
flow specified in 7.4. The test gas must be passed through a
valve. Monitor the oxygen of the outlet and the T , as specified
s
filter having a pore size rating of 0.02 µm or finer. the filter
in 7.3. The time required to reach the higher T must be less
s
must be compatible with the 94°C (200°F) bake-out.
than or equal to 10 min. Continue testing for 30 min after a
stable baseline is reestablished (<20 ppbv) as specified in 9.1.
8. Preparation of Apparatus
Cool until the lower T is reached.
s
8.1 A schematic drawing of a recommended test apparatus
located inside a clean laboratory is shown in Fig. 1. Deviations
from this design are acceptable as long as baseline levels
consistent with 4.2.1 can be maintained. Nitrogen or argon gas
is purified to remove water and hydrocarbons. The base gas is
then filtered by an electronics grade, high purity, point of use
filter (pore size rating ≤ 0.02 µm) before it is delivered to the
test component.
8.2 A bypass loop may be used to divert gas flow through
the test stand and the analyzer whenever the spool piece or a
testcomponentisinstalledorremovedfromtheteststand.This
prevents the ambient air from contaminating the test apparatus
and the oxygen analyzer; thus, the analyzer baseline remains
the same. A glove bag is used to enclose test component lines FIG. 2 Test Procedure Sequence
F1396 − 93 (2020)
9.3 Place the spool piece, test component (in original
bagging), and fittings into a glove bag or nitrogen tent without
disconnecting. Purge the glove bag with approximately five
glove bag volumes of inert gas. Disconnect the spool piece
while maintaining the flow through the system. Maintain the
spool piece in the proximity of the positiv
...
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: F1396 − 93 (Reapproved 2020)
Standard Test Method for
Determination of Oxygen Contribution by Gas Distribution
System Components
This standard is issued under the fixed designation F1396; 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 5.
1.1 This test method covers a procedure for testing compo-
1.6 This international standard was developed in accor-
nents for oxygen contribution to ultra-high purity gas distribu-
dance with internationally recognized principles on standard-
tion systems at ambient temperature. In addition, this test
ization established in the Decision on Principles for the
method allows testing of the component at elevated ambient
Development of International Standards, Guides and Recom-
temperatures as high as 70°C.
mendations issued by the World Trade Organization Technical
1.2 This test method applies to in-line components contain-
Barriers to Trade (TBT) Committee.
ing electronics grade materials such as those used in a
semiconductor gas distribution system.
2. Terminology
1.3 Limitations:
2.1 Definitions:
1.3.1 This test method is limited by the sensitivity of current
2.1.1 baseline—the instrument response under steady state
instrumentation, as well as the response time of the instrumen-
conditions.
tation. This test method is not intended to be used for test
components larger than 12.7-mm ( ⁄2-in.) outside diameter 2.1.2 glove bag—an enclosure that contains a controlled
nominal size. This test method could be applied to larger
atmosphere. A glove box could also be used for this test
components; however, the stated volumetric flow rate may not method.
provide adequate mixing to ensure a representative sample.
2.1.3 heat trace— heating of a component, spool piece, or
Higher flow rates may improve the mixing but excessively
test stand by a uniform and complete wrapping of the item with
dilute the sample.
resistant heat tape.
1.3.2 This test method is written with the assumption that
2.1.4 minimum detection limit (MDL) of the instrument—the
the operator understands the use of the apparatus at a level
lowest instrument response detectable and readable by the
equivalent to six months of experience.
instrument, and at least two times the amplitude of the noise.
1.4 The values stated in SI units are to be regarded as the
standard. The inch-pound units given in parentheses are for 2.1.5 response time—the time required for the system to
reach steady state after a change in concentration.
information only.
1.5 This standard does not purport to address all of the
2.1.6 spool piece—a null component, consisting of a
safety concerns, if any, associated with its use. It is the
straight piece of electropolished tubing and appropriate fittings,
responsibility of the user of this standard to establish appro-
used in place of the test component to establish the baseline.
priate safety, health, and environmental practices and deter-
2.1.7 standard conditions—101.3 kPa, 0.0°C (14.73 psia,
32°F).
This test method is under the jurisdiction of ASTM Committee F01 on
2.1.8 test component—any device being tested, such as a
Electronicsand is the direct responsibility of Subcommittee F01.10 on Contamina-
valve, regulator, or filter.
tion Control.
Current edition approved April 15, 2020. Published May 2020. Originally
2.1.9 test stand—the physical test system used to measure
approved in 1992. Last previous edition approved in 2012 as F1396 – 93(2012).
DOI: 10.1520/F1396-93R20. impurity levels.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
F1396 − 93 (2020)
2.1.10 zero gas—a purified gas that has an impurity concen- around each component for the duration of the test. In the case
tration below the MDL of the analytical instrument. This gas is of long pieces of electropolished tubing, use two glove bags,
to be used for both instrument calibration and component one at each end.
testing.
4.1.3 Tubing, used downstream of the test component shall
be 316L electropolished stainless steel seamless tubing. The
2.2 Symbols:
diameter of the sample line to the analyzer shall not be larger
2.2.1 P —The inlet pressure measured upstream of the
than 6.4 mm ( ⁄4 in.). The length of the sample line from the tee
purifier and filter in the test apparatus.
(installed upstream of the pressure gage P ) to the analyzer
2.2.2 P —The outlet pressure measured downstream of the
shall not be more than 600 mm, so as to minimize the effect
analyzer in the test apparatus.
(adsorption/desorption) of the sample line on the result. The
2.2.3 ppbv—Parts per billion by volume assuming ideal gas
sample line shall have no more than two mechanical joints.
behavior, equivalent to nmole/mole (such as nL/L). The same
4.1.4 Valves, diaphragm or bellows type, capable of unim-
as molar parts per billion (ppb).
paired operation at 94°C (200°F). The use of all-welded,
2.2.4 ppbw—Parts per billion by weight (such as ng/g).
all-metal valves is preferred.
2.2.5 ppmv—Parts per million by volume assuming ideal
4.2 Instrumentation:
gas behavior, equivalent to µmole/mole (such as µL/L). The
4.2.1 Oxygen Analyzer—The oxygen analyzer is to be
same as molar parts per million (ppm).
placed downstream of the test component. Accurate baseline
2.2.6 ppmw—Parts per million by weight (such as µg/g).
readings must be obtained prior to and subsequent to each of
the tests. Excessive deviations in baseline levels (610 ppbv)
2.2.7 Q —the bypass sample flow not going through the
before or after the tests require that all results be rejected. The
analytical system.
analyzer must be capable of accurately recording changes in
2.2.8 Q —the total sample flow through the analytical
oxygen concentrations on a real time basis.
system.
4.2.2 Oxygen Analyzer Calibration—Zero gas shall be at an
2.2.9 Q —the flow through the spool piece or component.
s
oxygen level below the MDL of the instrument, supplied by
2.2.10 T —the temperature of the air discharged by the
purified gas, with the purifier in close proximity to the analyzer.
a
analyzer’s cooling exhaust. The instrument’s internal standard, if available, is to be used
for the span calibration. Alternatively, span gas from a cylinder
2.2.11 T —the temperature of the spool piece or component.
s
may be used.
2.2.11.1 Discussion—Precautions must be taken to insure
that the temperature measured by the thermocouple is as close
4.3 Pressure and Flow Control—Upstream pressure is to be
as possible to that of the spool piece and test component.
controlled with a regular upstream of the test component. Flow
Appropriate insulation and conductive shield should be used to
is to be controlled at a point downstream of the sampling port
achieve as uniform a temperature as possible. The thermo-
and monitored at that point. A mass flow controller is preferred
couple must be in contact with the outside wall of the
for maintaining the flow as described in 7.4. Sampling is to be
component or spool piece.
performed via a tee in the line, with a section of straight tubing
2.2.12 V-1, V-2—inlet and outlet valves of bypass loop, before the mass flow controller. All lines must conform to
respectively. 4.1.3. Inlet pressure is monitored by P . Test flow is the sum of
Q and Q . Q is directly controlled, and Q is the measured
1 2 1 2
2.2.13 V-3, V-4—inlet and outlet valves of test loop, respec-
flow through the analyzer. Refer to Fig. 1.
tively.
4.4 Bypass Loop—The design of the bypass loop is not
3. Significance and Use
restricted to any one design. It could be, for example, a 3.2-mm
( ⁄8-in) 316L stainless steel coil or a flexible tube section. This
3.1 This test method defines a procedure for testing compo-
nents being considered for installation into a high-purity gas allows the flexibility necessary to install test components of
different lengths.
distribution system. Application of this test method is expected
to yield comparable data among components tested for pur-
poses of qualification for this installation.
4. Apparatus
4.1 Materials:
4.1.1 Nitrogen or Argon, clean and dry, as specified in 7.5.
4.1.2 Spool Piece, that can be installed in place of the test
component is required. This piece is to be a straight section of
316L electropolished stainless steel tubing with no restrictions.
The length of the spool piece shall be 200 mm. The spool piece
has the same end connections as the test component.
4.1.2.1 Components With Stub Ends—Use compression fit-
tings with nylon or teflon ferrules to connect the spool piece
and test component to the test loop. Keep the purged glove bag FIG. 1 Test Schematic
F1396 − 93 (2020)
5. Hazards of the test apparatus during the installation and removal of the
spool piece and the test piece.
5.1 It is required that the user have a working knowledge of
the respective instrumentation and that the user practice proper 8.3 A trace oxygen analyzer capable of detecting oxygen
handling of test components for trace oxygen analysis. Good concentration levels down to 2 ppb is connected to the test
laboratory practices must also be understood. stand to sample the gas flowing through the test piece. The
purified and filtered base gas from the test stand containing <
5.2 It is required that the user be familiar with proper
10 ppb oxygen is used as the zero oxygen gas source for the
component installation, and that the test components be in-
analyzer. Since the analyzer is sensitive to the sample flow rate,
stalled on the test stand in accordance with manufacturer’s
the metering valves within the analyzer should be adjusted to
instructions.
yield the flow rates required by the specification for an inlet
5.3 Do not exceed ratings (such as pressure, temperature,
pressure of 30 psig. The gas flow rate Q is set to 1 L/min.
s
and flow) of component.
8.4 Inlet gas pressure is controlled by a pressure regulator
5.4 Gloves are to be worn for all steps.
and measured immediately upstream of the purifier by an
5.5 Limit exposure of the instrument and test component to electronic grade pressure gage. Flow measurement is carried
out by a mass flow controller (MFC) located downstream of the
atmospheric contamination before and during the test.
analyzer. The outlet pressure of the gas is measured immedi-
6. Calibration
ately downstream of the analyzer by another electronic grade
pressure gage. The MFC along with its digital readout should
6.1 Calibrate instruments using standard laboratory prac-
be calibrated before use to control and display the gas flow rate
tices and manufacturer’s recommendations.
Q .
7. Conditioning
8.5 The temperature of the spool piece, test specimen,
7.1 Ensure that adequate mixing of the test gas is attained.
analyzer cell compartment, and the oxygen concentration
measured by the analyzer can either be recorded continuously
7.2 Pressure—Test component at 200 kPa gage (30 psig)
by a 25 channel data logger or collected and stored in a
measured at P .
computer using a data acquisition program.
7.3 Temperature— T is to be in the ambient temperature
s
range of 18 to 26°C (64 to 78°F) and in the higher mean
9. Procedure (see Fig. 2)
temperature range of 69 to 71°C (156 to 160°F). T must not
a
9.1 Bake-Out—With the spool piece installed and valves
deviate more than 6 2°C (4°F) from the time of calibration to
V-1, V-2, V-3, and V-4 open, bake out the system (downstream
the termination of the test. T must either be within the range
a
of purifier to upstream of analyzer, exclusive of the exhaust
of 18 to 26°C (64 to 78°F) or be consistent with the analytical
leg) at 94°C (200°F) until outlet oxygen concentration is stable
systems manufacturer’s specifications, whichever is more
below <20 ppbv. Flow of the gas is specified in 7.4. Cool to
stringent.
lower T . Close valves V-1 and V-2.
s
7.4 The flow rate Q for components is 1 standard L/min
s
9.2 Baseline—Flow gas through the test stand with the spool
with 6 2 % tolerance.
piece installed on the test stand. Use the flow rate as defined in
7.5 The test gas shall be purified nitrogen or argon with a
7.4. Flow for 30 min after the oxygen concentration has
maximum oxygen concentration not exceeding an oxygen
attained a level of <20 ppbv. Utilizing heat tape, heat the spool
concentration of 10 ppb. Gas quality must be maintained at
piece and upstream tubing to within 80 mm of the upstream
flow specified in 7.4. The test gas must be passed through a
valve. Monitor the oxygen of the outlet and the T , as specified
s
filter having a pore size rating of 0.02 µm or finer. the filter
in 7.3. The time required to reach the higher T must be less
s
must be compatible with the 94°C (200°F) bake-out.
than or equal to 10 min. Continue testing for 30 min after a
stable baseline is reestablished (<20 ppbv) as specified in 9.1.
8. Preparation of Apparatus
Cool until the lower T is reached.
s
8.1 A schematic drawing of a recommended test apparatus
located inside a clean laboratory is shown in Fig. 1. Deviations
from this design are acceptable as long as baseline levels
consistent with 4.2.1 can be maintained. Nitrogen or argon gas
is purified to remove water and hydrocarbons. The base gas is
then filtered by an electronics grade, high purity, point of use
filter (pore size rating ≤ 0.02 µm) before it is delivered to the
test component.
8.2 A bypass loop may be used to divert gas flow through
the test stand and the analyzer whenever the spool piece or a
test component is installed or removed from the test stand. This
prevents the ambient air from contaminating the test apparatus
and the oxygen analyzer; thus, the analyzer baseline remains
the same. A glove bag is used to enclose test component lines FIG. 2 Test Procedure Sequence
F1396 − 93 (2020)
9.3 Place the spool piece, test component (in original
bagging), and fittings into a glove bag or nitrogen tent without
disconnecting. Purge the glove bag with approximately five
glove bag volumes of inert gas. Disconnect the spool piece
while maintaining the flow through the system. Maintain the
spool piece in the proximity of the positive
...
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