ASTM E1409-97
(Test Method)Standard Test Method for Determination of Oxygen in Titanium and Titanium Alloys by the Inert Gas Fusion Technique
Standard Test Method for Determination of Oxygen in Titanium and Titanium Alloys by the Inert Gas Fusion Technique
SCOPE
1.1 This test method covers the determination of oxygen in titanium and titanium alloys in concentrations from 0.04 and 0.3%.
1.2 The values stated in both inch-pound and SI units are to be regarded separately as the standard. The values given in parentheses are for information only.
1.3 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. Specific precautionary statements are given in Note 2.
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Designation: E 1409 – 97
Standard Test Method for
Determination of Oxygen in Titanium and Titanium Alloys by
1
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
1.1 This test method covers the determination of oxygen in
titanium and titanium alloys in concentrations from 0.04 and
0.3 %.
1.2 The values stated in both inch-pound and SI units are to
be regarded separately as the standard. The values given in
parentheses are for information only.
1.3 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 appro-
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. Specific precau-
tionary statements are given in Note 2.
2. Referenced Documents
FIG. 1 Apparatus for Determination of Oxygen by the Inert Gas
2.1 ASTM Standards:
Fusion-Thermal Conductivity Method
E 50 Practices for Apparatus, Reagents, and Safety Precau-
2
tions for Chemical Analysis of Metals
with helium through heated rare earth/copper oxide that
E 173 Practice for Conducting Interlaboratory Studies of
2
converts CO to CO . The water produced during fusion is
2
Methods for Chemical Analysis of Metals
absorbed by magnesium perchlorate and the remaining nitro-
3. Summary of Test Method
gen and carbon dioxide are separated chromatographically. The
oxygen, as CO , enters the measuring cell and the thermistor
3.1 This test method is intended for use with automated, 2
bridge output is integrated and processed to display percent
commercially available, inert gas fusion analyzers.
oxygen.
3.2 The test sample, plus flux, is fused in a graphite crucible
3.4 In a typical instrument based on infrared detection (see
under a flowing inert gas stream (Ar, He, or N)ata
2
Fig. 2) the test sample is fused in a stream of nitrogen or argon
temperature sufficient to release oxygen. The released oxygen
and the evolved gases are passed directly into an infrared cell
combines with carbon to form CO. Depending on instrument
through which infrared energy is transmitted. The CO in the
design, the CO is oxidized to CO or left as CO and swept by
2
sample gases absorbs some of the transmitted infrared energy
the inert gas stream into either an infrared or thermal conduc-
and the decrease in energy reaching the detector is processed
tivity detector. The detector output is compared to that of
and displayed directly as percent oxygen. Some instruments
calibration standards and the result is displayed as percent
utilize helium carrier gas and oxidize the CO to CO before it
oxygen. 2
is passed into the infrared cell.
3.3 In a typical instrument whose detection is based upon
thermal conductivity (see Fig. 1) the sample gases are swept
4. Significance and Use
4.1 This test method is primarily intended as a referee test
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for compliance with compositional specifications. It is assumed
This test method is under the jurisdiction of ASTM Committee E-1 on
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
that all who use this test method will be trained analysts
responsibility of Subcommittee E01.06 on Ti, Zr, W, Mo, Ta, Nb, Hf.
capable of performing common laboratory procedures skill-
Current edition approved April 10, 1997. Published June 1997. Originally
fully and safely. It is expected that the work will be performed
published as E 1409 – 91. Last previous edition E 1409 – 96.
2
Annual Book of ASTM Standards, Vol 03.05. in a properly equipped laboratory.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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E1409–97
7.3 Inert Gas—Use the purity and type (Ar, N ,orHe)
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specified by the instrument manufacturer.
3
7.4 Magnesium Perchlorate, Anhydrous —Used in the in-
strument to absorb water. Use the purity specified by the
instrument manufacturer.
7.5 Nickel Flux Cleaning Solution—Prepare a fresh solution
of nickel cleaning solution by combining 75 mL of acetic acid,
25 mL of HNO and 2 mL of HCl.
3
7.6 Rare Earth/Copper Oxide—Reagent used in some in-
struments to oxidize CO to CO for thermal conductivity
2
detection. Use the purity specified by the instrument manufac-
turer.
4
7.7 Sodium Hydroxide on Clay —Reagent used in some
instruments to absorb CO . Use a purity specified by the
2
instrument manufacturer.
7.8 Titanium Sample Pickle Solution—Prepare a fresh solu-
FIG. 2
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