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ASTM E1447-01

(Test Method)

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

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 problems, 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
09-May-2001
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 E1447-92(1996) - Standard Test Method for Determination of Hydrogen in Titanium and Titanium Alloys by the Inert Gas Fusion Thermal Conductivity Method
Effective Date
10-May-2001
Replaced By
ASTM E1447-04 - 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
Referred By
ASTM B338-17(2021) - Standard Specification for Seamless and Welded Titanium and Titanium Alloy Tubes for Condensers and Heat Exchangers
Effective Date
10-May-2001
Referred By
ASTM B348/B348M-21 - Standard Specification for Titanium and Titanium Alloy Bars and Billets
Effective Date
10-May-2001
Referred By
ASTM F2063-18 - Standard Specification for Wrought Nickel-Titanium Shape Memory Alloys for Medical Devices and Surgical Implants
Effective Date
10-May-2001
Referred By
ASTM B863-19 - Standard Specification for Titanium and Titanium Alloy Wire
Effective Date
10-May-2001
Referred By
ASTM F90-23 - Standard Specification for Wrought Cobalt-20Chromium-15Tungsten-10Nickel Alloy for Surgical Implant Applications (UNS R30605)
Effective Date
10-May-2001
Referred By
ASTM B988-18(2022) - Standard Specification for Powder Metallurgy (PM) Titanium and Titanium Alloy Structural Components
Effective Date
10-May-2001
Referred By
ASTM F1713-08(2021)e1 - Standard Specification for Wrought Titanium-13Niobium-13Zirconium Alloy for Surgical Implant Applications (UNS R58130)
Effective Date
10-May-2001
Referred By
ASTM F3001-14(2021) - Standard Specification for Additive Manufacturing Titanium-6 Aluminum-4 Vanadium ELI (Extra Low Interstitial) with Powder Bed Fusion
Effective Date
10-May-2001
Referred By
ASTM F1108-21 - Standard Specification for Titanium-6Aluminum-4Vanadium Alloy Castings for Surgical Implants (UNS R56406)
Effective Date
10-May-2001
Referred By
ASTM B381-21 - Standard Specification for Titanium and Titanium Alloy Forgings
Effective Date
10-May-2001
Referred By
ASTM F2146-22 - Standard Specification for Wrought Titanium-3Aluminum-2.5Vanadium Alloy Seamless Tubing for Surgical Implant Applications (UNS R56320)
Effective Date
10-May-2001
Referred By
ASTM B265-20a - Standard Specification for Titanium and Titanium Alloy Strip, Sheet, and Plate
Effective Date
10-May-2001
Referred By
ASTM F3046-21 - Standard Specification for Wrought Titanium-3Aluminum-2.5Vanadium Alloy for Surgical Implant Applications (UNS R56320)
Effective Date
10-May-2001

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ASTM E1447-01 - Standard Test Method for Determination of Hydrogen in Titanium and Titanium Alloys by the Inert Gas Fusion Thermal Conductivity MethodASTM E1447-01 - 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 E1447-01 - Standard Test Method for Determination of Hydrogen in Titanium and Titanium Alloys by the Inert Gas Fusion Thermal Conductivity Method
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Standards Content (Sample)

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:E1447–01
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
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
2
induction furnace; analytical gas stream impurity removal
Dioxide Powders and Pellets
E 50 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
3
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
4
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
1 (Note 2).
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 May 10, 2001. Published July 2001. Originally
structions for proper gas selection.
published as E 1447–92. Last previous editon E 1447–92 (1996)
2
Annual Book of ASTM Standards, Vol 12.01.
7.4 High-Purity Tin Metal (Low Hydrogen)—Use the purity
3
Annual Book of ASTM Standards, Vol 03.05.
4 specified by the instrument manufacturer.
Discontinued; see 1997 Annual Book of ASTM Standards, Vol 03.05.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
E1447
meeting the above criterion.
7.5 Magnesium Perchlorate, Anhydrone.
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
...

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ASTM E2994-21(Test Method)
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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.  
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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  
0.014 to 0.1  
Iron  
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Manganese  
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Molybdenum  
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Nickel  
0.006 to 0.1  
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0.018 to 0.1  
Tin  
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Vanadium  
0.015 to 5.0  
Zirconium  
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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  
0.006 to 0.1  
Copper  
0.028 to 0.1  
Iron  
0.09 to 0.3  
Molybdenum  
0.016 to 0.1  
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.  
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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.  
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SCOPE
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Application
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Quantitative
Range (wt.%)  
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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:    
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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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0.017 to 15.50  
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ASTM F2082/F2082M-23(Test Method)
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.  
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ASTM E1447-22(Test Method)
Standard Test Method for Determination of Hydrogen in Reactive Metals and Reactive Metal Alloys by Inert Gas Fusion with Detection by Thermal Conductivity or Infrared Spectrometry

SIGNIFICANCE AND USE
5.1 This test method is intended for the routine analysis of reactive metals and reactive metal alloys to verify compliance with compositional specifications such as those specified by Committees B09 and B10. It is expected 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.
SCOPE
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.  
1.2 This method has been interlaboratory tested for titanium and zirconium and alloys of these metals and can provide quantitative results in the range specified in 1.1. It may be possible to extend the quantitative range of this method provided a method validation study, as described in Guide E2857, is performed and the results of the study show the method extension meets laboratory data quality objectives. This method may also be extended to alloys other than titanium and zirconium provided a method validation study, as described in Guide E2857, is performed.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific hazards, see Section 9.  
1.4 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.

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ASTM
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  
0.014 to 0.1  
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  
0.006 to 0.1  
Copper  
0.028 to 0.1  
Iron  
0.09 to 0.3  
Molybdenum  
0.016 to 0.1  
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.  
1.4 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. Specific safety hazard statements are given in Section 9.  
1.5 This international standard was developed in accordance with internationally recognized pri...

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ASTM
ASTM E2371-21a(Test Method)
Standard Test Method for Analysis of Titanium and Titanium Alloys by Direct Current Plasma and Inductively Coupled Plasma Atomic Emission Spectrometry (Performance-Based Test Methodology)

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  
Application
Range (wt.%)  
Quantitative
Range (wt.%)  
Aluminum  
0–8  
0.009 to 8.0  
Boron  
0–0.04  
0.0008 to 0.01  
Cobalt  
0-1  
0.006 to 0.1  
Chromium  
0–5  
0.005 to 4.0  
Copper  
0–0.6  
0.004 to 0.5  
Iron  
0–3  
0.004 to 3.0  
Manganese  
0–0.04  
0.003 to 0.01  
Molybdenum  
0–8  
0.004 to 6.0  
Nickel  
0–1  
0.001 to 1.0  
Niobium  
0-6  
0.008 to 0.1  
Palladium  
0-0.3  
0.02 to 0.20  
Ruthenium  
0-0.5  
0.004 to 0.10  
Silicon  
0–0.5  
0.02 to 0.4  
Tantalum  
0-1  
0.01 to 0.10  
Tin  
0–4  
0.02 to 3.0  
Tungsten  
0-5  
0.01 to 0.10  
Vanadium  
0–15  
0.01 to 15.0  
Yttrium  
0–0.04  
0.001 to 0.004  
Zirconium  
0–5  
0.003 to 4.0  
1.2 This test method has been interlaboratory tested for the elements and ranges specified in the quantitative range part of the table in 1.1. It may be possible to extend this test method to other elements or broader mass fraction ranges as shown in the application range part of the table above provided that test method validation is performed that includes evaluation of method sensitivity, precision, and bias. Additionally, the validation study shall evaluate the acceptability of sample preparation methodology using reference materials or spike recoveries, or both. Guide E2857 provides information on validation of analytical methods for alloy analysis.  
1.3 Because of the lack of certified reference materials (CRMs) containing bismuth, hafnium, and magnesium, these elements were not included in the scope or the interlaboratory study (ILS). It may be possible to extend the scope of this test method to include these elements provided that method validation includes the evaluation of method sensitivity, precision, and bias during the development of the testing method.  
1.4 Units—The values stated in SI units are to be regarded as the standard. No other units of measurement are included in 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. Specific safety hazards statements are given in Section 9.  
1.6 This international standard was developed in accordance with internationally recognized principle...

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