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ASTM F2405-04(2011)

(Test Method)

Standard Test Method for Trace Metallic Impurities in High Purity Copper by High-Mass-Resolution Glow Discharge Mass Spectrometer (Withdrawn 2020)

Standard Test Method for Trace Metallic Impurities in High Purity Copper by High-Mass-Resolution Glow Discharge Mass Spectrometer (Withdrawn 2020)

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 copper. 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 wt. 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 copper materials.
SCOPE
1.1 This test method covers the concentrations of trace metallic impurities in high purity (99.95 wt. % pure, or purer, with respect to metallic trace impurities) electronic grade copper.
1.2 This test method pertains to analysis by magnetic-sector glow discharge mass spectrometer (GDMS).
1.3 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 detection limits, and the like) known by the responsible technical committee to effect the reliability of high purity copper analyses.
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.
WITHDRAWN RATIONALE
This test method covers the concentration of trace metallic impurities in high purity (99.05 wt. % pure, or purer, with respect to metallic trace impurities) electronic grade copper.
Formerly under the jurisdiction of Committee F01 on Electronics, this test method was withdrawn in January 2020 in accordance with section 10.6.3 of the Regulations Governing ASTM Technical Committees, which requires that standards shall be updated by the end of the eighth year since the last approval date.

General Information

Status
Withdrawn
Publication Date
31-May-2011
Withdrawal Date
09-Jan-2020
ICS
77.120.30 - Copper and copper alloys
Technical Committee
F01 - Electronics
Drafting Committee
F01.17 - Sputter Metallization
Current Stage
Ref Project

Relations

Referred By
ASTM F3192-16 - Standard Specification for High-Purity Copper Sputtering Target Used for Through-Silicon Vias (TSV) Mettalization
Effective Date
01-Jun-2011

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ASTM F2405-04(2011) - Standard Test Method for Trace Metallic Impurities in High Purity Copper by High-Mass-Resolution Glow Discharge Mass Spectrometer (Withdrawn 2020)ASTM F2405-04(2011) - Standard Test Method for Trace Metallic Impurities in High Purity Copper by High-Mass-Resolution Glow Discharge Mass Spectrometer (Withdrawn 2020)
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ASTM F2405-04(2011) - Standard Test Method for Trace Metallic Impurities in High Purity Copper by High-Mass-Resolution Glow Discharge Mass Spectrometer (Withdrawn 2020)
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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: F2405 − 04 (Reapproved 2011)
Standard Test Method for
Trace Metallic Impurities in High Purity Copper by High-
1
Mass-Resolution Glow Discharge Mass Spectrometer
This standard is issued under the fixed designation F2405; 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 Methods for Analysis and Testing of Industrial and Spe-
3
cialty Chemicals (Withdrawn 2009)
1.1 This test method covers the concentrations of trace
E691 Practice for Conducting an Interlaboratory Study to
metallic impurities in high purity (99.95 wt. % pure, or purer,
Determine the Precision of a Test Method
with respect to metallic trace impurities) electronic grade
E876 Practice for Use of Statistics in the Evaluation of
copper.
3
Spectrometric Data (Withdrawn 2003)
1.2 This test method pertains to analysis by magnetic-sector
F1593 Test Method for Trace Metallic Impurities in Elec-
glow discharge mass spectrometer (GDMS).
tronic Grade Aluminum by High Mass-Resolution Glow-
1.3 This test method does not include all the information Discharge Mass Spectrometer
needed to complete GDMS analyses. Sophisticated computer-
3. Terminology
controlled laboratory equipment, skillfully used by an experi-
enced operator, is required to achieve the required sensitivity.
3.1 Terminology in this test method is consistent with
Thistestmethoddoescovertheparticularfactors(forexample,
Terminology E135. Required terminology specific to this test
specimen preparation, setting of relative sensitivity factors,
method, not covered in Terminology E135, is indicated in 3.2.
determination of detection limits, and the like) known by the
3.2 Definitions:
responsible technical committee to effect the reliability of high
3.2.1 campaign—a test procedure to determine the accuracy
purity copper analyses.
of the instrument, which was normally performed at the
1.4 This standard does not purport to address all of the
beginning of the day or after the instrument modification, or
safety concerns, if any, associated with its use. It is the
both.
responsibility of the user of this standard to establish appro-
3.2.2 reference sample—material accepted as suitable for
priate safety and health practices and determine the applica-
use as a calibration/sensitivity reference standard by all parties
bility of regulatory limitations prior to use.
concerned with the analyses.
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
2.1 ASTM Standards:
source, and analyzed.
E135 Terminology Relating to Analytical Chemistry for
3.2.4 test sample—material(copper)tobeanalyzedfortrace
Metals, Ores, and Related Materials
metallic impurities by this GDMS method.
E173 Practice for Conducting Interlaboratory Studies of
3.2.4.1 Discussion—Generally the test sample is extracted
Methods for Chemical Analysis of Metals (Withdrawn
3
from a larger batch (lot, casting) of product and is intended to
1998)
be representative of the batch.
E180 Practice for Determining the Precision of ASTM
4. Summary of Test Method
1
This test method is under the jurisdiction of ASTM Committee F01 on
4.1 A specimen is mounted in a plasma discharge cell.
Electronics and is the direct responsibility of Subcommittee F01.17 on Sputter
Atoms subsequently sputtered from the specimen surface are
Metallization.
ionized, and then focused as an ion beam through a double-
Current edition approved June 1, 2011. Published June 2011. Originally
approved in 2004. Last previous edition approved in 2004 as F2405–04. DOI:
focusing magnetic-sector mass separation apparatus. The mass
10.1520/F2405-04R11.
spectrum (the ion current) is collected as magnetic field or
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
acceleration voltage, or both, and is scanned.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on
4.2 The ion current of an isotope at mass M is the total
i
the ASTM website.
3
measured current, less contributions from all other interfering
The last approved version of this historical standard is referenced on
www.astm.org. sources. Portions of the measured current may originate from
Copyright ©ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA19428-2959. United States
1

---------------------- Page: 1 ----------------------
F2405 − 04 (2011)
the ion detector alone (detector noise). Portions may be due to 5.3 For most metallic species, the detection limit for routine
incomple
...

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4.1 This test environment is believed to give an accelerated ranking of the relative or absolute degree of stress-corrosion cracking susceptibility for different brasses. It has been found to correlate well with the corresponding service ranking in environments that cause stress-corrosion cracking which is thought to be due to the combined presence of traces of moisture and ammonia vapor. The extent to which the accelerated ranking correlates with the ranking obtained after long-term exposure to environments containing corrodents other than ammonia is not at present known. Examples of such environments may be severe marine atmospheres (Cl−), severe industrial atmospheres (predominantly SO2), and super-heated ammonia-free steam.  
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4.3 Mattsson's solution of pH 7.2 may also cause stress independent general and intergranular corrosion of brasses to some extent. This leads to the possibility of confusing stress-corrosion failures with mechanical failures induced by corrosion-reduced net cross sections. This danger is particularly great with small cross section specimens, high applied stress levels, long exposure periods and stress-corrosion resistant alloys. Careful metallographic examination is recommended for correct diagnosis of the cause of failure. Alternatively, unstressed control specimens may be exposed to evaluate the extent to which stress independent corrosion degrades mechanical properties.
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1.1 This practice covers the preparation and use of Mattsson’s solution of pH 7.2 as an accelerated stress-corrosion cracking test environment for brasses (copper-zinc base alloys). The variables (to the extent that these are known at present) that require control are described together with possible means for controlling and standardizing these variables.  
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1.4 This practice relates solely to the preparation and control of the test environment. No attempt is made to recommend surface preparation or finish, or both, as this may vary with the test objectives. Similarly, no attempt is made to recommend particular stress-corrosion test specimen configurations or methods of applying the stress. Test specimen configurations that may be used are referenced in Practice G30 and STP 425.2  
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included ...

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Standard Terminology for Copper and Copper Alloys

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3.1 This terminology is not intended to apply to any standard, test method, practice, or other document not within the jurisdiction of Committee B05 on Copper and Copper Alloys.
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1.1 The terms defined in this terminology standard are applicable to copper and copper alloy products specifications, test methods, practices, and other documents within the jurisdiction of Committee B05 on Copper and Copper Alloys.  
1.2 The values stated in inch-pound units are to be regarded as standard. The values given in parentheses are mathematical conversions to SI units that are provided for information only and are not considered standard.  
1.3 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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