Name: ASTM E1447-04 - Standard Test Method for Determination of Hydrogen in Titanium and Titanium Alloys by the Inert Gas Fusion Thermal Conductivity Method
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Abstract

Standard Test Method for Determination of Hydrogen in Titanium and Titanium Alloys by the Inert Gas Fusion Thermal Conductivity Method

SCOPE
1.1 This test method applies to the determination of hydrogen in titanium and titanium alloys in concentrations from 0.0010 to 0.0200 %.
1.2 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. For specific precautionary statements, see Section 8.

General Information

Status

Historical

Publication Date

30-Nov-2004

ICS

77.120.50 - Titanium and titanium alloys

Technical Committee

E01 - Analytical Chemistry for Metals, Ores, and Related Materials

Drafting Committee

E01.06 - Ti, Zr, W, Mo, Ta, Nb, Hf, Re

Current Stage

Ref Project

Relations

Replaces

ASTM E1447-01 - Standard Test Method for Determination of Hydrogen in Titanium and Titanium Alloys by the Inert Gas Fusion Thermal Conductivity Method

Effective Date

01-Dec-2004

Replaced By

ASTM E1447-05 - Standard Test Method for Determination of Hydrogen in Titanium and Titanium Alloys by the Inert Gas Fusion Thermal Conductivity/Infrared Detection Method

Effective Date

01-May-2005

Referred By

ASTM F1713-08(2021)e1 - Standard Specification for Wrought Titanium-13Niobium-13Zirconium Alloy for Surgical Implant Applications (UNS R58130)

Effective Date

01-Dec-2004

Referred By

ASTM F2885-17(2023) - Standard Specification for Metal Injection Molded Titanium-6Aluminum-4Vanadium Components for Surgical Implant Applications

Effective Date

01-Dec-2004

Referred By

ASTM B863-19 - Standard Specification for Titanium and Titanium Alloy Wire

Effective Date

01-Dec-2004

Referred By

ASTM F1108-21 - Standard Specification for Titanium-6Aluminum-4Vanadium Alloy Castings for Surgical Implants (UNS R56406)

Effective Date

01-Dec-2004

Referred By

ASTM A1001-18 - Standard Specification for High-Strength Steel Castings in Heavy Sections

Effective Date

01-Dec-2004

Referred By

ASTM F1813-21 - Standard Specification for Wrought Titanium-12Molybdenum-6Zirconium-2Iron Alloy for Surgical Implant (UNS R58120)

Effective Date

01-Dec-2004

Referred By

ASTM B862-19 - Standard Specification for Titanium and Titanium Alloy Welded Pipe

Effective Date

01-Dec-2004

Referred By

ASTM B1009-20 - Standard Specification for Titanium Alloy Bars for Near Surface Mounts in Civil Structures

Effective Date

01-Dec-2004

Referred By

ASTM B861-19 - Standard Specification for Titanium and Titanium Alloy Seamless Pipe

Effective Date

01-Dec-2004

Referred By

ASTM F620-20 - Standard Specification for Titanium Alloy Forgings for Surgical Implants in the Alpha Plus Beta Condition

Effective Date

01-Dec-2004

Referred By

ASTM F1295-23 - Standard Specification for Wrought Titanium-6Aluminum-7Niobium Alloy for Surgical Implant Applications (UNS R56700)

Effective Date

01-Dec-2004

Referred By

ASTM B265-20a - Standard Specification for Titanium and Titanium Alloy Strip, Sheet, and Plate

Effective Date

01-Dec-2004

Referred By

ASTM F136-13(2021)e1 - Standard Specification for Wrought Titanium-6Aluminum-4Vanadium ELI (Extra Low Interstitial) Alloy for Surgical Implant Applications (UNS R56401)

Effective Date

01-Dec-2004

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ASTM E1447-04 - Standard Test Method for Determination of Hydrogen in Titanium and Titanium Alloys by the Inert Gas Fusion Thermal Conductivity Method

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ASTM E1447-04 - Standard Test ...

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:E1447–04
Standard Test Method for
Determination of Hydrogen in Titanium and Titanium Alloys
1
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 compositionalspeciﬁcations.Itisassumedthatallwhousethis
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
2
6. Apparatus
2.1 ASTM Standards:
6.1 Fusion and Measurement Apparatus—Automatic hy-
C 696 Test Methods for Chemical, Mass Spectrometeric,
and Spectrochemical Analysis of Nuclear-Grade Uranium drogen determinator, consisting of an electrode furnace or
induction furnace; analytical gas stream impurity removal
Dioxide Powders and Pellets
E50 Practices forApparatus, Reagents, and Safety Consid- systems; thermal conductivity cell hydrogen measurement
system; and auxiliary puriﬁcation systems (Note 1).
erations for Chemical Analysis of Metals, Ores, and
Related Materials
NOTE 1—The apparatus and analysis system have been previously
E 173 Practice for Conducting Interlaboratory Studies of
described in Test Methods C 696, Sections 142 to 149. Several models of
Methods for Chemical Analysis of Metals
commercial analyzers are available and presently in use in industry. Each
has its own unique design characteristics and operational requirements.
3. Summary of Test Method
Consult the instrument manufacturer’s instructions for operational details.
3.1 The specimen, contained in a small, single-use graphite
6.2 Graphite Crucibles—The crucibles are machined from
crucible, is fused under a ﬂowing carrier gas atmosphere.
high-purity graphite. Use the size crucibles recommended by
Hydrogen present in the sample is released as molecular
the manufacturer of the instrument.
hydrogen into the ﬂowing gas stream. The hydrogen is sepa-
6.3 Crucible Tongs—Capable of handling recommended
rated from other liberated gases such as carbon monoxide and
crucibles.
ﬁnally measured in a thermal conductivity cell.
7. Reagents and Materials
3.2 This test method is written for use with commercial
analyzers equipped to carry out the above operations automati-
7.1 Acetone, low-residue.
cally and is calibrated using standard samples of known
7.2 Sodium Hydroxide on Clay Base, commonly known as
hydrogen content.
Ascarite II.
7.3 High-Purity Carrier Gas (99.99 %)—Argon, nitrogen
(Note 2).
1
This test method is under the jurisdiction of ASTM Committee E01 on
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
NOTE 2—Carrier gases vary by instrument model and include both
responsibility of Subcommittee E01.06 on Ti, Zr, W, Mo, Ta, Nb, Hf.
high-purity argon and nitrogen. Consult instrument manufacturer’s in-
Current edition approved Dec. 1, 2004. Published January 2005. Originally
structions for proper gas selection.
approved in 1992. Last previous editon approved in 2001 as E 1447–01.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
7.4 High-Purity Tin Metal (Low Hydrogen)—Use the purity
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
speciﬁed by the instrument manufacturer.
Standards volume information, refer to the standard’s Document Summary page on
7.5 Magnesium Perchlorate, Anhydrone.
the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
E1447–04
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 wil
...

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SIGNIFICANCE AND USE
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1.1 This test method applies to the determination of hydrogen in reactive metals and reactive metal alloys, particularly titanium and zirconium, with mass fractions from 9 mg/kg to 320 mg/kg.
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Standard Test Method for Determination of Oxygen and Nitrogen in Titanium and Titanium Alloys by Inert Gas Fusion

SIGNIFICANCE AND USE
5.1 This test method is primarily intended as a test for compliance with compositional specifications. It is assumed that all who use this test method will be trained analysts capable of performing common laboratory procedures skillfully and safely. It is expected that the work will be performed in a properly equipped laboratory.
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1.1 This test method covers the determination of oxygen in titanium and titanium alloys in mass fractions from 0.01 % to 0.5 % and the determination of nitrogen in titanium and titanium alloys in mass fractions from 0.003 % to 0.11 %.
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ASTM E2994-21(Test Method)

Standard Test Method for Analysis of Titanium and Titanium Alloys by Spark Atomic Emission Spectrometry and Glow Discharge Atomic Emission Spectrometry (Performance-Based Method)

SIGNIFICANCE AND USE
5.1 This test method for the chemical analysis of titanium alloys is primarily intended to test material for compliance to compositional requirements of specifications such as those under jurisdiction of ASTM Committee B10. It may also be used to test compliance with other specifications that are compatible with the test method.
5.2 This is a performance-based test method that relies more on the demonstrated quality of the test result than on strict adherence to specific procedural steps. It is assumed that all who use this test method will be trained analysts capable of performing common laboratory procedures skillfully and safely, and that the work will be performed in a properly equipped laboratory.
5.3 It is expected that laboratories using this test method will prepare their own work instructions. These work instructions will include detailed operating instructions for the specific laboratory, the specific reference materials employed, and performance acceptance criteria.
SCOPE
1.1 This test method describes the analysis of titanium and its alloys by spark atomic emission spectrometry (Spark-AES) and glow discharge atomic emission spectrometry (GD-AES). The titanium specimen to be analyzed may be in the form of a disk, casting, foil, sheet, plate, extrusion, or some other wrought form or shape. The elements and ranges covered in the scope by spark-AES of this test method are listed below.
Element
Tested Mass Fraction Range (%)
Aluminum
0.008 to 7.0
Chromium
0.006 to 0.1
Copper
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Iron
0.043 to 0.3
Manganese
0.005 to 0.1
Molybdenum
0.014 to 0.1
Nickel
0.006 to 0.1
Silicon
0.018 to 0.1
Tin
0.02 to 0.1
Vanadium
0.015 to 5.0
Zirconium
0.013 to 0.1
1.1.1 The elements oxygen, nitrogen, carbon, niobium, boron, yttrium, palladium, and ruthenium, were included in the ILS but the data did not contain the required six laboratories. Precision tables were provided for informational use only.
1.2 The elements and ranges covered in the scope by GD-AES of this test method are listed below.
Element
Tested Mass Fraction Range (%)
Aluminum
0.02 to 7.0
Carbon
0.02 to 0.1
Chromium
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Copper
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Iron
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Molybdenum
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Nickel
0.006 to 0.1
Silicon
0.018 to 0.1
Tin
0.022 to 0.1
Vanadium
0.054 to 5.0
Zirconium
0.026 to 0.1
1.2.1 The elements boron, manganese, oxygen, nitrogen, niobium, yttrium, palladium, and ruthenium were included in the ILS, but the data did not contain the required six laboratories. Precision tables were provided for informational use only.
1.3 The elements and mass fractions given in the above scope tables are the ranges validated through the interlaboratory study. However, it is known that the techniques used in this standard allow the useable range, for the elements listed, to be extended higher or lower based on individual instrument capability, available reference materials, laboratory capabilities, and the spectral characteristics of the specific element wavelength being used. It is also acceptable to analyze elements not listed in 1.1 or 1.2 and still meet compliance to this standard test method. Laboratories must provide sufficient evidence of method validation when extending the analytical range or when analyzing elements not reported in Section 18 (Precision and Bias), as described in Guide E2857.
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SIGNIFICANCE AND USE
5.1 This test method for the chemical analysis of titanium and titanium alloys is primarily intended to test material for compliance with specifications of chemical composition such as those under the jurisdiction of ASTM Committee B10. It may also be used to test compliance with other specifications that are compatible with the test method.
5.2 It is assumed that all who use this test method will be trained analysts capable of performing common laboratory procedures skillfully and safely and that the work will be performed in a properly equipped laboratory.
5.3 This is a performance-based test method that relies more on the demonstrated quality of the test result than on strict adherence to specific procedural steps. It is expected that laboratories using this test method will prepare their own work instructions. These work instructions will include detailed operating instructions for the specific laboratory, the specific reference materials used, and performance acceptance criteria. It is also expected that, when applicable, each laboratory will participate in proficiency test programs, such as described in Practice E2027, and that the results from the participating laboratory will be satisfactory.
SCOPE
1.1 This method describes the analysis of titanium and titanium alloys, such as specified by committee B10, by inductively coupled plasma atomic emission spectrometry (ICP-AES) and direct current plasma atomic emission spectrometry (DCP-AES) for the following elements:
Element
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Range (wt.%)
Quantitative
Range (wt.%)
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Boron
0–0.04
0.0008 to 0.01
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0.005 to 4.0
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0–0.6
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Iron
0–3
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Yttrium
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Zirconium
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5.1 This procedure is suitable for manufacturing control and for verifying that the product meets specifications. It provides rapid, multi-element determinations with sufficient accuracy to assure product quality. The analytical performance data included may be used as a benchmark to determine if similar X-ray spectrometers provide equivalent precision and accuracy, or if the performance of a particular spectrometer has changed.
SCOPE
1.1 This test method covers the analysis of Ni-base alloys by wavelength dispersive X-ray Fluorescence Spectrometry for the determination of the following elements:
Element
Composition Range
Manganese
0.06 % to 1.6 %
Phosphorus
0.008 % to 0.015 %
Silicon
0.08 % to 0.6 %
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Iron
0.17 % to 46 %
Tungsten
0.06 % to 0.50 %
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1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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Standard Test Method for Analysis of Titanium Alloys by Wavelength Dispersive X-Ray Fluorescence Spectrometry

SIGNIFICANCE AND USE
5.1 This method is suitable for providing data on the chemical composition of titanium alloys having compositions within the scope of the standard. It is intended for routine production control and for determination of chemical composition for the purpose of certifying material specification compliance. Additionally, the analytical performance data included with this method may be used as a benchmark to determine if similar X-ray spectrometers provide equivalent precision and accuracy.
5.2 Compositions outside the ranges in 1.1 may be reported if proper method validation is performed. Refer to Guide E2857 for information on method validation.
SCOPE
1.1 This test method2 covers the X-ray fluorescence analysis of titanium alloys for the following elements in the ranges indicated:
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Aluminum
0.041 to 8.00
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0.015 to 0.60
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0.023 to 2.00
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0.003 to 9.50
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Standard Test Method for Determination of Transformation Temperature of Nickel-Titanium Shape Memory Alloys by Bend and Free Recovery

SIGNIFICANCE AND USE
5.1 This test method provides a rapid, economical method for determination of transformation temperatures.
5.2 Measurement of the specimen motion closely parallels many shape memory applications and provides a result that is applicable to the function of the material.
5.3 This test method uses a wire, tube, strip specimen, or a wire, tube, or strip specimen extracted from a component; thus, it provides an assessment of a nickel titanium product in its semifinished or finished form.
5.4 This test method may be used on annealed samples to determine the transformation temperatures and ensure the alloy formulation, since chemical analysis is not precise enough to adequately determine the nickel-to-titanium ratio of shape memory alloys.
5.5 In general, the transformation temperatures measured by this method will not be the same as those measured by the DSC method defined in Test Method F2004. Therefore, the results of DSC and BFR cannot be compared directly.
5.5.1 The BFR method measures the transformation temperatures by tracking shape recovery of stress-induced martensite deformed below the R′s temperature or the As temperature. In contrast, the DSC method measures the start, peak, and finish temperatures of the thermal transformation of martensite to R-phase or to austenite. See Refs (1-4).
5.6 The test method is applicable to shape memory alloys with Af temperatures in the range of approximately –25 to 90 °C.
SCOPE
1.1 This test method describes a procedure for quantitatively determining the martensite-to-austenite or the martensite to R-phase transformation temperature of annealed, aged, shape-set, or tempered nickel-titanium alloy specimens by deforming the specimen in bending and measuring the deformation recovered during heating through the thermal transformation (BFR method). See 3.1.1.
Note 1: For aged, shape-set, or tempered specimens the transformation may be from martensite to austenite or from martensite to R-phase. See Reference (1)2 for details.
1.2 The test specimen may be wire, tube, or strip or a specimen extracted from a semifinished or finished component.
1.2.1 For specimens not in the form of a wire, tube, or strip that are extracted from semifinished or finished components, a wire, tube, or strip shaped test specimen shall be made from the component such that the deformation mode in the test specimen is pure bending.
1.2.2 Other specimen geometries or displacements resulting in a more complex strain state, such as bending with torsion or buckling, are beyond the scope of this standard.
1.3 Ruggedness tests have demonstrated that sample Af must be limited to obtain good test results. See 5.6 for details. Ruggedness tests have demonstrated that deformation strain, deformation temperature, and equilibration time at the deformation temperature must be controlled to obtain good test results. See 9.1, 9.2, and 9.4 for details.
1.4 The values stated in either SI units or inch-pound units are to be regarded separately as standard. The values stated in each system may not be exact equivalents; therefore, each system shall be used independently of the other. Combining values from the two systems may result in nonconformance with this standard.
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.
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.