ASTM F1710-08
(Test Method)Standard Test Method for Trace Metallic Impurities in Electronic Grade Titanium by High Mass-Resolution Glow Discharge Mass Spectrometer
Standard Test Method for Trace Metallic Impurities in Electronic Grade Titanium by High Mass-Resolution Glow Discharge Mass Spectrometer
SIGNIFICANCE AND USE
This test method is intended for application in the semiconductor industry for evaluating the purity of materials (for example, sputtering targets, evaporation sources) used in thin film metallization processes. This test method may be useful in additional applications, not envisioned by the responsible technical committee, as agreed upon between the parties concerned.
This test method is intended for use by GDMS analysts in various laboratories for unifying the protocol and parameters for determining trace impurities in pure titanium. The objective is to improve laboratory to laboratory agreement of analysis data. This test method is also directed to the users of GDMS analyses as an aid to understanding the determination method, and the significance and reliability of reported GDMS data.
For most metallic species the detection limit for routine analysis is on the order of 0.01 weight ppm. With special precautions detection limits to sub-ppb levels are possible.
This test method may be used as a referee method for producers and users of electronic-grade titanium materials.
SCOPE
1.1 This test method covers the determination of concentrations of trace metallic impurities in high purity titanium.
1.2 This test method pertains to analysis by magnetic-sector glow discharge mass spectrometer (GDMS).
1.3 The titanium matrix must be 99.9 weight % (3N-grade) pure, or purer, with respect to metallic impurities. There must be no major alloy constituent, for example, aluminum or iron, greater than 1000 weight ppm in concentration.
1.4 This test method does not include all the information needed to complete GDMS analyses. Sophisticated computer-controlled laboratory equipment skillfully used by an experienced operator is required to achieve the required sensitivity. This test method does cover the particular factors (for example, specimen preparation, setting of relative sensitivity factors, determination of sensitivity limits, etc.) known by the responsible technical committee to effect the reliability of high purity titanium analyses.
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 and health practices and determine the applicability of regulatory limitations prior to use.
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Designation: F1710 − 08
StandardTest Method for
Trace Metallic Impurities in Electronic Grade Titanium by
1
High Mass-Resolution Glow Discharge Mass Spectrometer
This standard is issued under the fixed designation F1710; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope Methods for Chemical Analysis of Metals (Withdrawn
3
1998)
1.1 This test method covers the determination of concentra-
E180Practice for Determining the Precision of ASTM
tions of trace metallic impurities in high purity titanium.
Methods for Analysis and Testing of Industrial and Spe-
1.2 Thistestmethodpertainstoanalysisbymagnetic-sector 3
cialty Chemicals (Withdrawn 2009)
glow discharge mass spectrometer (GDMS).
E691Practice for Conducting an Interlaboratory Study to
1.3 The titanium matrix must be 99.9 weight % (3N-grade) Determine the Precision of a Test Method
E1257Guide for Evaluating Grinding Materials Used for
pure, or purer, with respect to metallic impurities. There must
be no major alloy constituent, for example, aluminum or iron, Surface Preparation in Spectrochemical Analysis
greater than 1000 weight ppm in concentration.
3. Terminology
1.4 This test method does not include all the information
3.1 Terminology in this test method is consistent with
needed to complete GDMS analyses. Sophisticated computer-
Terminology E135. Required terminology specific to this test
controlled laboratory equipment skillfully used by an experi-
method, not covered in Terminology E135, is indicated in 3.2.
enced operator is required to achieve the required sensitivity.
3.2 Definitions:
Thistestmethoddoescovertheparticularfactors(forexample,
3.2.1 campaign—a series of analyses of similar specimens
specimen preparation, setting of relative sensitivity factors,
performed in the same manner in one working session, using
determination of sensitivity limits, etc.) known by the respon-
one GDMS setup.
sible technical committee to effect the reliability of high purity
3.2.1.1 Discussion—As a practical matter, cleaning of the
titanium analyses.
ionsourcespecimencellisoftentheboundaryeventseparating
1.5 This standard does not purport to address all of the
one analysis campaign from the next.
safety concerns, if any, associated with its use. It is the
3.2.2 reference sample—material accepted as suitable for
responsibility of the user of this standard to establish appro-
use as a calibration/sensitivity reference standard by all parties
priate safety and health practices and determine the applica-
concerned with the analyses.
bility of regulatory limitations prior to use.
3.2.3 specimen—a suitably sized piece cut from a reference
2. Referenced Documents
or test sample, prepared for installation in the GDMS ion
2
source, and analyzed.
2.1 ASTM Standards:
E135Terminology Relating to Analytical Chemistry for
3.2.4 test sample—materialtitaniumtobeanalyzedfortrace
Metals, Ores, and Related Materials
metallic impurities by this GDMS method.
E173Practice for Conducting Interlaboratory Studies of
3.2.4.1 Discussion—Generally the test sample is extracted
from a larger batch (lot, casting) of product and is intended to
be representative of the batch.
1
This test method is under the jurisdiction of ASTM Committee F01 on
Electronics and is the direct responsibility of Subcommittee F01.17 on Sputter
4. Summary of the Test Method
Metallization.
4.1 A specimen is mounted as the cathode in a plasma
Current edition approved June 15, 2008. Published July 2008. Originally
approved in 1996. Last previous edition approved in 2002 as F1710–97(02). DOI:
discharge cell. Atoms subsequently sputtered from the speci-
10.1520/F1710-08.
men surface are ionized, and then focused as an ion beam
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
3
Standards volume information, refer to the standard’s Document Summary page on The last approved version of this historical standard is referenced on
the ASTM website. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1
---------------------- Page: 1 ----------------------
F1710 − 08
through a double-focusing magnetic-sector mass separation 6. Apparatus
apparatus. The mass spectrum, that is, the ion current, is
6.1 Glow Discharge Mass Spectrometer, with mass resolu-
collected as magnetic field or acceleration voltage, or both, is
tion greater than 3500, and associated equipment and supplies.
scanned.
TheGDMSmustbefittedwithanionsourcespecimencellthat
4.2 The ion
...
This document is not anASTM standard and is intended only to provide the user of anASTM 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:F 1710–97 (Reapproved 2002) Designation: F 1710 – 08
Standard Test Method for
Trace Metallic Impurities in Electronic Grade Titanium by
1
High Mass-Resolution Glow Discharge Mass Spectrometer
This standard is issued under the fixed designation F 1710; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber 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 concentrations of trace metallic impurities in high purity titanium.
1.2 This test method pertains to analysis by magnetic-sector glow discharge mass spectrometer (GDMS).
1.3 The titanium matrix must be 99.9 weight % (3N-grade) pure, or purer, with respect to metallic impurities. There must be
no major alloy constituent, for example, aluminum or iron, greater than 1000 weight ppm in concentration.
1.4 This test method does not include all the information needed to complete GDMS analyses. Sophisticated computer-
controlled laboratory equipment skillfully used by an experienced operator is required to achieve the required sensitivity.This test
method does cover the particular factors (for example, specimen preparation, setting of relative sensitivity factors, determination
of sensitivity limits, etc.) known by the responsible technical committee to effect the reliability of high purity titanium analyses.
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 and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2
2.1 ASTM Standards:
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
E180 PracticeforDeterminingthePrecisionofASTMMethodsforAnalysisandTestingofIndustrialandSpecialtyChemicals
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
E1257 Guide for Evaluating Grinding Materials Used for Surface Preparation in Spectrochemical Analysis
3. Terminology
3.1 Terminology in this test method is consistent with Terminology E135. Required terminology specific to this test method,
not covered in Terminology E135, is indicated in 3.2.
3.2 Definitions:
3.2.1 campaign—a series of analyses of similar specimens performed in the same manner in one working session, using one
GDMS setup.
3.2.1.1 Discussion—As a practical matter, cleaning of the ion source specimen cell is often the boundary event separating one
analysis campaign from the next.
3.2.2 reference sample—material accepted as suitable for use as a calibration/sensitivity reference standard by all parties
concerned with the analyses.
3.2.3 specimen—a suitably sized piece cut from a reference or test sample, prepared for installation in the GDMS ion source,
and analyzed.
3.2.4 test sample—material titanium to be analyzed for trace metallic impurities by this GDMS method.
3.2.4.1 Discussion—Generally the test sample is extracted from a larger batch (lot, casting) of product and is intended to be
representative of the batch.
1
This test method is under the jurisdiction of ASTM Committee F01 on Electronics and is the direct responsibility of Subcommittee F01.17 on Sputter Metallization.
Current edition approved Dec. 10, 2002. Published May 2003. Originally approved in 1996. Last previous edition approved in 1997 as F1710–97.
Current edition approved June 15, 2008. Published July 2008. Originally approved in 1996. Last previous edition approved in 2002 as F1710–97(02).
2
ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,orcontactASTMCustomerServiceatservice@astm.org.For Annual Book of ASTM Standards
, Vol 03.05.volume information, refer to the standard’s Document Summary page on the ASTM website.
3
Discontinued. See 1996 Annual Book of ASTM Standards , Vol 03.05.
3
Withdrawn.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
---------------------- Page: 1 ----------------------
F 1710 – 08
4. Summary of the Test Method
4.1 Aspecimen is mounted as the cathode in a plasma discharge cell.Atoms subsequently sputtered from the specimen surface
are ionized, and then focused as
...
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