ASTM E1447-92(1996)

NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: E 1447 – 92 (Reapproved 1996)
Standard Test Method for
Determination of Hydrogen in Titanium and Titanium Alloys
by the Inert Gas Fusion Thermal Conductivity Method
This standard is issued under the fixed designation E 1447; 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 4. Significance and Use
1.1 This test method applies to the determination of hydro- 4.1 This test method is intended to test for compliance with
gen in titanium and titanium alloys in concentrations from compositional specifications. It is assumed that all who use this
0.0010 to 0.0200 %. test method will be trained analysts capable of performing
1.2 This standard does not purport to address all of the common laboratory procedures skillfully and safely. It is
safety concerns, if any, associated with its use. It is the expected that the work will be performed in a properly
responsibility of the user of this standard to establish appro- equipped laboratory.
priate safety and health practices and determine the applica-
5. Interferences
bility of regulatory limitations prior to use. For specific
precautionary statements, see Section 8. 5.1 The elements ordinarily present in titanium and its
alloys do not interfere.
2. Referenced Documents
6. Apparatus
2.1 ASTM Standards:
6.1 Fusion and Measurement Apparatus—Automatic hy-
C 696 Method for Chemical, Mass Spectrometeric, and
Spectrochemical Analysis of Nuclear-Grade Uranium Di- drogen determinator, consisting of an electrode furnace or
induction furnace; analytical gas stream impurity removal
oxide Powders and Pellets
E 29 Practice for Using Significant Digits in Test Data to systems; thermal conductivity cell hydrogen measurement
system; and auxiliary purification systems (Note 1).
Determine Conformance with Specifications
E 50 Practices for Apparatus, Reagents, and Safety Precau-
NOTE 1—The apparatus and analysis system have been previously
tions for Chemical Analysis of Metals
described in Method C 696, Sections 142 to 149. Several models of
E 173 Practice for Conducting Interlaboratory Studies of
commercial analyzers are available and presently in use in industry. Each
Methods for Chemical Analysis of Metals has its own unique design characteristics and operational requirements.
Consult the instrument manufacturer’s instructions for operational details.
E 178 Practice for Dealing with Outlying Observations
6.2 Graphite Crucibles—The crucibles are machined from
3. Summary of Test Method
high-purity graphite. Use the size crucibles recommended by
3.1 The specimen, contained in a small, single-use graphite
the manufacturer of the instrument.
crucible, is fused under a flowing carrier gas atmosphere.
6.3 Crucible Tongs—Capable of handling recommended
Hydrogen present in the sample is released as molecular
crucibles.
hydrogen into the flowing gas stream. The hydrogen is sepa-
7. Reagents and Materials
rated from other liberated gases such as carbon monoxide and
finally measured in a thermal conductivity cell.
7.1 Acetone, low-residue.
3.2 This test method is written for use with commercial
7.2 Sodium Hydroxide on Clay Base, commonly known as
analyzers equipped to carry out the above operations automati-
Ascarite II.
cally and is calibrated using standard samples of known
7.3 High-Purity Carrier Gas (99.99 %)—Argon, nitrogen
hydrogen content.
(Note 2).
NOTE 2—Carrier gases vary by instrument model and include both
high-purity argon and nitrogen. Consult instrument manufacturer’s in-
This test method is under the jurisdiction of ASTM Committee E-1 on
structions for proper gas selection.
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
responsibility of Subcommittee E01.06 on Ti, Zr, W, Mo, Ta, Nb, Hf. 7.4 High-Purity Tin Metal (Low Hydrogen)—Use the purity
Current edition approved Jan. 15, 1992. Published June 1992.
specified by the instrument manufacturer.
Annual Book of ASTM Standards, Vol 12.01.
7.5 Magnesium Perchlorate, Anhydrone.
Annual Book of ASTM Standards, Vol 14.02.
Annual Book of ASTM Standards, Vol 03.05.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
E 1447
7.6 Molecular Sieve—Characteristics specified by the in- 11.2.4 Enter the average blank value in the appropriate
strument manufacturer. mechanism of the analyzer (Note 6), and refer to the manufac-
7.7 Schutze Reagent—Iodine pentoxide over silica gel. turer’s instruction. This mechanism will electronically com-
pensate for the blank value.
8. Hazards
NOTE 6—If the unit does not have this function, the average blank must
8.1 For hazards to be observed in the use of this test method,
be subtracted from the total result (see Note 9).
refer to Practices E 50.
11.3 Calibration Procedure:
8.2 Use care when handling hot crucibles and operating
11.3.1 Prepare at least four 0.15 to 0.30-g specimens of a
electrical equipment to avoid personal injury by either burn or
titanium hydrogen calibration standard as directed in 10.2.
electrical shock.
This titanium hydrogen calibration standard should have a
hydrogen content greater than or approximately equal to the
9. Preparation of Apparatus
unknown samples within the scope of this test method (0.0010
9.1 Assemble the apparatus as recommended by the manu-
to 0.0200 %).
facturer.
11.3.2 Follow the calibration procedure recommended by
9.2 Test the furnace and analyzer to ensure the absence of
the manufacturer. Analyze at least three standard specimens to
gas leaks and make the required electrical power and water
determine calibration slope. Treat each specimen as directed in
connections. Prepare the apparatus for operation in accordance
12.2 before proceeding to the next one.
with the manufacturer’s instructions. Make a minimum of two
11.3.3 Confirm the calibration by analyzing the fourth
determinations using a specimen as directed in 12.2 before
titanium hydrogen standard (Note 7). The value should be
attempting to calibrate the system or to determine the blank.
within the allowable limits of the certified value. If not,
determine and correct the cause, and repeat 11.3.1 and 11.3.2
10. Sample Preparation
(Note 8).
10.1 U
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