ASTM F1374-92(1999)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: F 1374 – 92 (Reapproved 1999)
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 F 1374; 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 (e) 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 2. Referenced Documents
1.1 This test method establishes a procedure for testing 2.1 ASTM Standards:
components used in ultra-high-purity gas distribution systems E1151 Practice for Ion Chromatography Terms and Rela-
for ionic and organic surface residues. tionships
1.2 This test method applies to in-line components contain- 2.2 Union Carbide Standard:
ing electronics grade materials in the gaseous form. Techniques for Measuring Trace Gas Impurities in High
1.3 Limitations: Purity Gases
1.3.1 This test method is limited by the sensitivity of the
3. Terminology
detection instruments and by the available levels of purity in
extracting solvents. While the ion and gas chromatographic 3.1 Definitions of Terms Specific to This Standard:
3.1.1 spool piece—a null component, consisting of a
methods are quantitative, the Fourier transform infrared spec-
troscopy (FTIR) method can be used as either a qualitative or straightpieceofelectropolishedtubingandappropriatefittings,
used in place of the test component to establish the baseline.
a quantitative tool. In addition, the gas chromatography (GC)
and FTIR methods are used to detect hydrocarbons and 3.1.2 standard conditions—101.3 kPa, 0.0°C (14.73 psia,
32.0°F).
halogenated substances that remain as residues on component
internal surfaces. This eliminates those materials with high 3.1.3 test component—any device being tested, such as a
valve, regulator, or filter.
vaporpressures,whichareanalyzedperthetotalhydrocarbons
test, from this test method. 3.1.4 test fluid blank—a volume of test solvent adequate for
analysis.
1.3.2 This test method is intended for use by operators who
understand the use of the apparatus at a level equivalent to 3.1.4.1 Discussion—This is used to determine the back-
ground impurity concentrations in the test fluid. This fluid is
twelve months of experience.
1.4 The values stated in SI units are to be regarded as the 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
standards. The inch-pound units given in parentheses are for
does not contaminate the fluid blank.
information only.
1.5 This standard does not purport to address all of the 3.2 Abbreviations:Abbreviations:
3.2.1 FTIR—Fourier transform infrared spectroscopy.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro- 3.2.2 GC—gas chromatography.
3.2.3 IC—ion chromatography.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. Specific hazard 3.2.4 IPA—isopropanol (2-propanol).
3.2.5 MS—mass spectrometry.
statements are given in Section 6.
3.2.6 ppbv—parts per billion by volume (such as nL/L).
This test method is under the jurisdiction of ASTM Committee F-1 on
Electronics and is the direct responsibility of Subcommittee F01.10 on Processing Annual Book of ASTM Standards, Vol 14.02.
Environments. Available from Linde Division Union Carbide, 175 E. Park Drive,Tonawanda,
Current edition published Feb. 15, 1992. Approved April 1992. NY 14151.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
F 1374 – 92 (1999)
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:
FIG. 2 Ionic/Organic Contribution Data Table Illustration
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 MV
water [corrected for 18°C (64°F)] must be used for the ionic
extractables determination. Total oxidizable carbon must be
lessthan50ppbw.Thewatermustbefilteredthrougha0.2-µm
(or finer) filter. Electronics grade (or better) IPA is to be used
for the organic extractables determination.
5.1.2 Spool Piece— a straight run of electropolished 316-L
stainless steel tubing with no restrictions. The length of the
spool piece shall be approximately 200 mm. The spool piece
should be the same diameter as the test component.
5.1.3 Caps—usedtosealtheendsofthetestcomponentand
spool piece are to be of 316-L stainless steel. For stub end
components, 316-L stainless steel compression fittings with
nylon or polytetraflouroethylene ferrules are to be used. For
face seal fittings, stainless steel gaskets must be used.
5.1.4 Gloves—made of powder free latex or natural rubber
and resistant to the test fluids used in this test method.
5.2 Instrumentation:
5.2.1 Ion Chromatograph—The IC is an analytical instru-
ment that detects ionic species in deionized (DI) water. The
eluant is passed through a column containing ion exchange
resin. A conductivity detector is used to detect the ionic
species. The retention times of the various ionic species are
usedtoidentifythespecies.Theareaundertherespectivepeak
FIG. 1 Ionic/Organic Contribution Data Table Illustration yieldsthequantityofthespeciesintheeluant.Thistestmethod
F 1374 – 92 (1999)
uses a column for mono- and polyvalent anions and a column 6.3 Gloves are to be worn at all times.After use, the gloves
formono-andpolyvalentcations.Asuppressorcolumnmaybe are to be rinsed in the appropriate test fluid.
used to increase sensitivity.
NOTE 2—An alternative could be the use of disposable gloves, using a
5.2.2 Gas chromatograph—The GC is an analytical instru-
new glove for each test.
ment that detects organic species in the gas phase. A liquid
sample is injected and heated to the vapor phase. The sample
7. Calibration
is then passed through a column containing an adsorbent. A
7.1 Calibrate instruments using standard laboratory prac-
carrier gas is used as the mobile phase. The retention times of
tices and manufacturer’s recommendations.
the various peaks help to identify the organic species.The area
under the respective peak yields the quantity of the species in
8. Test Procedure
the mobile phase.
8.1 Temperature— The test component and the spool piece
NOTE 1—Since the peak of the solvent will be large, it will obscure
aretobetestedataconstanttemperature 62°Cintherangeof
thosespeciesthathaveacarbonnumberorretentiontimebelowthatofthe
26°C (18 to 78°F). Solvents used must be at the same
solvent.
temperature.
5.2.3 Fourier transform infrared spectrometer—The FTIR
8.2 Rinse t
...