ASTM E1409-13

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.
SCOPE
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 %.  
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. Specific warning statements are given in 8.8.

General Information

• Status: Historical
• Publication Date: 30-Sep-2013
• 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

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: E1409 − 13
Standard Test Method for
Determination of Oxygen and Nitrogen in Titanium and
1
Titanium Alloys by Inert Gas Fusion
This standard is issued under the fixed designation E1409; 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 analyzers typically measure both oxygen and nitrogen simul-
taneously or sequentially utilizing parallel measurement sys-
1.1 This test method covers the determination of oxygen in
tems.
titanium and titanium alloys in mass fractions from 0.01 % to
0.5 % and the determination of nitrogen in titanium and 4.2 The test sample, plus flux, is fused in a graphite crucible
under a flowing inert gas stream at a temperature sufficient to
titanium alloys in mass fractions from 0.003 % to 0.11 %.
release oxygen and nitrogen. Oxygen combines with carbon to
1.2 This standard does not purport to address all of the
form carbon monoxide (CO) and nitrogen is released as N .
2
safety concerns, if any, associated with its use. It is the
Depending on instrument design, the CO may be oxidized to
responsibility of the user of this standard to establish appro-
carbon dioxide (CO ). The CO or CO , or both, are swept by
2 2
priate safety and health practices and determine the applica-
the inert gas stream into either an infrared or thermal conduc-
bility of regulatory limitations prior to use. Specific warning
tivity detector. The detector response generated by analysis of
statements are given in 8.8.
the test sample is compared to the response generated by
2. Referenced Documents analysis of reference materials and the result is displayed as
2 percent oxygen. The nitrogen is swept by the inert gas stream
2.1 ASTM Standards:
into a thermal conductivity detector. The detector response
E50 Practices for Apparatus, Reagents, and Safety Consid-
generated by analysis of the test sample is compared to the
erations for Chemical Analysis of Metals, Ores, and
response generated by analysis of reference materials and the
Related Materials
result is displayed as percent nitrogen.
E135 Terminology Relating to Analytical Chemistry for
4.3 Inatypicalinstrumentforthedeterminationofnitrogen,
Metals, Ores, and Related Materials
the sample gases are swept with inert gas through heated rare
E173 Practice for Conducting Interlaboratory Studies of
earth/copper oxide that converts CO to CO and hydrogen (H )
Methods for Chemical Analysis of Metals (Withdrawn
2 2
3
to water (H O). The CO is absorbed on sodium hydroxide
1998)
2 2
impregnated on clay, and the H O is removed with magnesium
E1601 Practice for Conducting an Interlaboratory Study to
2
perchlorate. The nitrogen, as N , enters the measuring cell and
Evaluate the Performance of an Analytical Method
2
the thermistor bridge output is integrated and processed to
3. Terminology
display percent nitrogen.
3.1 Definitions—For definitions of terms used in this
5. Significance and Use
method, refer to Terminology E135.
5.1 This test method is primarily intended as a test for
4. Summary of Test Method compliance with compositional specifications. It is assumed
that all who use this test method will be trained analysts
4.1 This test method is intended for use with automated,
capable of performing common laboratory procedures skill-
commercially available, inert gas fusion analyzers. These
fully and safely. It is expected that the work will be performed
in a properly equipped laboratory.
1
E01 on 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, Re. 6. Interferences
Current edition approved Oct. 1, 2013. Published November 2013. Originally
6.1 The elements usually present in titanium and its alloys
approved in 1991. Last previous edition approved in 2008 as E1409 – 08. DOI:
do not interfere but there is some evidence to suggest that low
10.1520/E1409-13.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
purity flux can cause some adsorption of the released oxygen.
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
7. Apparatus
the ASTM website.
3
7.1 Instrument—Fusion and measurement apparatus, auto-
The last approved version of this historical standard is referenced on
www.astm.org. matic oxygen and nitrogen determinator consisting of an
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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E1409 − 13
NOTE 3—In 2004,
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: E1409 − 08 E1409 − 13
Standard Test Method for
Determination of Oxygen and Nitrogen in Titanium and
1
Titanium Alloys by the Inert Gas Fusion Technique
This standard is issued under the fixed designation E1409; 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
1.1 This test method covers the determination of oxygen in titanium and titanium alloys in concentrations mass fractions from
0.01 % to 0.5 % and the determination of nitrogen in titanium and titanium alloys in concentrations mass fractions from 0.003 %
to 0.11 %.
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.
1.2 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. Specific warning statements are given in 8.8.
2. Referenced Documents
2
2.1 ASTM Standards:
E50 Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials
E135 Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
3
E173 Practice for Conducting Interlaboratory Studies of Methods for Chemical Analysis of Metals (Withdrawn 1998)
E882 Guide for Accountability and Quality Control in the Chemical Analysis Laboratory
E1019 Test Methods for Determination of Carbon, Sulfur, Nitrogen, and Oxygen in Steel, Iron, Nickel, and Cobalt Alloys by
Various Combustion and Fusion Techniques
E1601 Practice for Conducting an Interlaboratory Study to Evaluate the Performance of an Analytical Method
E1914 Practice for Use of Terms Relating to the Development and Evaluation of Methods for Chemical Analysis
3. Terminology
3.1 Definitions—For definitions of terms used in this method, refer to Terminology E135 and Practice E1914.
4. Summary of Test Method
4.1 This test method is intended for use with automated, commercially available, inert gas fusion analyzers. These analyzers
typically measure both oxygen and nitrogen simultaneously or sequentially utilizing parallel measurement systems.
4.2 The test sample, plus flux, is fused in a graphite crucible under a flowing inert gas stream (argon, helium) at a temperature
sufficient to release oxygen and nitrogen. Oxygen combines with carbon to form carbon monoxide (CO) and nitrogen is released
as N . Depending on instrument design, the CO is may be oxidized to carbon dioxide (CO ) or left). The CO or CO as CO and,
2 2 2
or both, are swept by the inert gas stream into either an infrared or thermal conductivity detector. The detector output response
generated by analysis of the test sample is compared to that the response generated by analysis of reference materials and the result
is displayed as percent oxygen. The nitrogen is swept by the inert gas stream (helium gas) into a thermal conductivity detector.
The detector response generated by analysis of the test sample is compared to that the response generated by analysis of reference
materials and the result is displayed as percent nitrogen.
1
E01 on 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, Re.
Current edition approved June 15, 2008Oct. 1, 2013. Published July 2008November 2013. Originally approved in 1991. Last previous edition approved in 20052008 as
E1409 – 05.E1409 – 08. DOI: 10.1520/E1409-08.10.1520/E1409-13.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
3
The last approved version of this historical standard is referenced on www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

---------------------- Page: 1 ----------------------
E1409 − 13
4.3 In a typical instrument for the determination of nitrogen, the sample gases are swept with inert gas through heated rare
earth/copper oxide that converts CO to CO and h
...