ASTM E1409-04

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation:E1409–04
Standard Test Method for
Determination of Oxygen in Titanium and Titanium Alloys by
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the Inert Gas Fusion Technique
This standard is issued under the fixed designation E 1409; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope design, the CO is oxidized to CO or left as CO and swept by
2
the inert gas stream into either an infrared or thermal conduc-
1.1 This test method covers the determination of oxygen in
tivity detector. The detector output is compared to that of
titanium and titanium alloys in concentrations from 0.04 and
calibration standards and the result is displayed as percent
0.3 %.
oxygen.
1.2 The values stated in both inch-pound and SI units are to
3.3 In a typical instrument whose detection is based upon
be regarded separately as the standard. The values given in
thermal conductivity (see Fig. 1) the sample gases are swept
parentheses are for information only.
with helium through heated rare earth/copper oxide that
1.3 This standard does not purport to address all of the
converts CO to CO . The water produced during fusion is
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safety concerns, if any, associated with its use. It is the
absorbed by magnesium perchlorate and the remaining nitro-
responsibility of the user of this standard to establish appro-
genandcarbondioxideareseparatedchromatographically.The
priate safety and health practices and determine the applica-
oxygen, as CO , enters the measuring cell and the thermistor
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bility of regulatory limitations prior to use. Specific precau-
bridge output is integrated and processed to display percent
tionary statements are given in Note 2.
oxygen.
2. Referenced Documents
3.4 In a typical instrument based on infrared detection (see
2
Fig. 2) the test sample is fused in a stream of nitrogen or argon
2.1 ASTM Standards:
and the evolved gases are passed directly into an infrared cell
E 50 Practices for Apparatus, Reagents, and Safety Precau-
through which infrared energy is transmitted. The CO in the
tions for Chemical Analysis of Metals
sample gases absorbs some of the transmitted infrared energy
E 173 Practice for Conducting Interlaboratory Studies of
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and the decrease in energy reaching the detector is processed
Methods for Chemical Analysis of Metals
and displayed directly as percent oxygen. Some instruments
E 1601 Practice for Conducting an Interlaboratory Study to
utilize helium carrier gas and oxidize the CO to CO before it
Evaluate the Performance of an Analytical Method 2
is passed into the infrared cell.
3. Summary of Test Method
4. Significance and Use
3.1 This test method is intended for use with automated,
4.1 This test method is primarily intended as a referee test
commercially available, inert gas fusion analyzers.
forcompliancewithcompositionalspecifications.Itisassumed
3.2 The test sample, plus flux, is fused in a graphite crucible
that all who use this test method will be trained analysts
under a flowing inert gas stream (Ar, He, or N)ata
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capable of performing common laboratory procedures skill-
temperature sufficient to release oxygen. The released oxygen
fully and safely. It is expected that the work will be performed
combines with carbon to form CO. Depending on instrument
in a properly equipped laboratory.
1 5. Interferences
This test method is under the jurisdiction of ASTM Committee E01 on
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
5.1 The elements usually present in titanium and its alloys
responsibility of Subcommittee E01.06 on Ti, Zr, W, Mo, Ta, Nb, Hf.
do not interfere but there is some evidence to suggest that low
Current edition approved May 1, 2004. Published June 2004. Originally
purity flux can cause some adsorption of the released oxygen.
approved in 1991. Last previous edition approved in 1997 as E 1409 – 97.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM 6. Apparatus
Standards volume information, refer to the standard’s Document Summary page on
6.1 Instrument—The general features of the instruments are
the ASTM website.
3
shown in Figs. 1 and 2.
Withdrawn.
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E1409–04
6.4 Tweezers—Six inches (152 millimetres), solvent and
acid-resistant plastic (used during the sample preparation
process).
7. Reagents
7.1 Acetone—Residue after evaporation must be<
0.0005 %.
7.2 Graphite Powder—High-purity graphite powder speci-
fied
...