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ASTM E2994-16

(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)

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 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 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 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 method are listed below.    
Element  
Tested Mass Fraction Range (%)  
Aluminum  
0.02 to 7.0  
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  
1.3 The 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 to be extended higher or lower based on individual instrument and laboratory capabilities, and the spectral characteristics of the specific element wavelength being used. Laboratories must provide sufficient evidence of method validation when extending the analytical range as described in Guide E2857 Validating Analytical Methods.  
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 and health practices and determine the applicability of regulatory limitations prior to use. Specific safety hazard statements are given in Section 9.

General Information

Status
Historical
Publication Date
14-Apr-2016
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

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ASTM E2994-16 - Standard Test Method for Analysis of Titanium and Titanium Alloys by Spark Atomic Emission Spectrometry and Glow Discharge Atomic Emission Spectrometry (Performance-Based Method)ASTM E2994-16 - Standard Test Method for Analysis of Titanium and Titanium Alloys by Spark Atomic Emission Spectrometry and Glow Discharge Atomic Emission Spectrometry (Performance-Based Method)
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ASTM E2994-16 - Standard Test Method for Analysis of Titanium and Titanium Alloys by Spark Atomic Emission Spectrometry and Glow Discharge Atomic Emission Spectrometry (Performance-Based Method)
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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: E2994 − 16
Standard Test Method for
Analysis of Titanium and Titanium Alloys by Spark Atomic
Emission Spectrometry and Glow Discharge Atomic
1
Emission Spectrometry (Performance-Based Method)
This standard is issued under the fixed designation E2994; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope
Tested Mass
Element Fraction
1.1 This test method describes the analysis of titanium and
Range (%)
Zirconium 0.026 to 0.1
its alloys by spark atomic emission spectrometry (Spark-AES)
and glow discharge atomic emission spectrometry (GD-AES).
1.3 The mass fractions given in the above scope tables are
The titanium specimen to be analyzed may be in the form of a
the ranges validated through the interlaboratory study.
disk,casting,foil,sheet,plate,extrusionorsomeotherwrought
However, it is known that the techniques used in this standard
form or shape. The elements and ranges covered in the scope
allow the useable range to be extended higher or lower based
by spark-AES of this method are listed below.
on individual instrument and laboratory capabilities, and the
Tested Mass spectral characteristics of the specific element wavelength
Element Fraction
being used. Laboratories must provide sufficient evidence of
Range (%)
method validation when extending the analytical range as
Aluminum 0.008 to 7.0
Chromium 0.006 to 0.1 described in Guide E2857 Validating Analytical Methods.
Copper 0.014 to 0.1
1.4 This standard does not purport to address all of the
Iron 0.043 to 0.3
Manganese 0.005 to 0.1 safety concerns, if any, associated with its use. It is the
Molybdenum 0.014 to 0.1
responsibility of the user of this standard to establish appro-
Nickel 0.006 to 0.1
priate safety and health practices and determine the applica-
Silicon 0.018 to 0.1
Tin 0.02to0.1 bility of regulatory limitations prior to use. Specific safety
Vanadium 0.015 to 5.0
hazard statements are given in Section 9.
Zirconium 0.013 to 0.1
1.1.1 The elements oxygen, nitrogen, carbon, niobium,
2. Referenced Documents
boron, yttrium, palladium, and ruthenium, were included in the
2
2.1 ASTM Standards:
ILS but the data did not contain the required six laboratories.
E135 Terminology Relating to Analytical Chemistry for
Precision tables were provided for informational use only.
Metals, Ores, and Related Materials
1.2 The elements and ranges covered in the scope by
E177 Practice for Use of the Terms Precision and Bias in
GD-AES of this method are listed below.
ASTM Test Methods
Tested Mass
E305 Practice for Establishing and Controlling Atomic
Element Fraction
Emission Spectrochemical Analytical Curves
Range (%)
E406 Practice for Using Controlled Atmospheres in Spec-
Aluminum 0.02 to 7.0
Chromium 0.006 to 0.1
trochemical Analysis
Copper 0.028 to 0.1
E691 Practice for Conducting an Interlaboratory Study to
Iron 0.09 to 0.3
Determine the Precision of a Test Method
Molybdenum 0.016 to 0.1
Nickel 0.006 to 0.1
E1329 Practice for Verification and Use of Control Charts in
Silicon 0.018 to 0.1
Spectrochemical Analysis
Tin 0.022 to 0.1
Vanadium 0.054 to 5.0 E1507 Guide for Describing and Specifying the Spectrom-
eter of an Optical Emission Direct-Reading Instrument
1
This test method is under the jurisdiction of ASTM Committee E01 on
2
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct For referenced ASTM standards, visit the ASTM website, www.astm.org, or
responsibility of Subcommittee E01.06 on Ti, Zr, W, Mo, Ta, Nb, Hf, Re. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Current edition approved April 15, 2016. Published May 2016. DOI: 10.1520/ Standards volume information, refer to the standard’s Document Summary page on
E2994-16. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
E2994 − 16
E1601 Practice for Conducting an Interlaboratory Study to the elements composing the sample and is converted into
Evaluate the Performance of an Analytical Method electrical signals by either photomultiplier tubes (PMTs) or a
E2857 Guide for Validating Analytical Methods suitable solid state detector. The detected analyte signals are
E2972 Guide for Production, Testing, and ValueAssignment integrated and converted to an intensity value. A ratio of the
of In-House Reference Materials for Metals, Ores, and detected analyte intensity and the internal standard signal may
Other Related Materials be made. A calibration is made using a suite of reference
3
materials with co
...

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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.  
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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  
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Chromium  
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Copper  
0.014 to 0.1  
Iron  
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Manganese  
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Molybdenum  
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Nickel  
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Silicon  
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Tin  
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Vanadium  
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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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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.
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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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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.  
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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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