ASTM F1845-08(2016)
(Test Method)Standard Test Method for Trace Metallic Impurities in Electronic Grade Aluminum-Copper, Aluminum-Silicon, and Aluminum-Copper-Silicon Alloys by High-Mass-Resolution Glow Discharge Mass Spectrometer (Withdrawn 2023)
Standard Test Method for Trace Metallic Impurities in Electronic Grade Aluminum-Copper, Aluminum-Silicon, and Aluminum-Copper-Silicon Alloys by High-Mass-Resolution Glow Discharge Mass Spectrometer (Withdrawn 2023)
SIGNIFICANCE AND USE
5.1 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.
5.2 This test method is intended for use by GDMS analysts in various laboratories for unifying the protocol and parameters for determining trace impurities in aluminum-copper, aluminum-silicon, and aluminum-copper-silicon alloys. 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.
5.3 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.
5.4 This test method may be used as a referee method for producers and users of electronic-grade aluminum-copper, aluminum-silicon and aluminum-copper-silicon materials.
SCOPE
1.1 This test method determines the concentrations of trace metallic impurities in high purity (99.99 wt. % pure, or purer, with respect to metallic trace impurities) aluminum-copper, aluminum-silicon and aluminum-copper-silicon alloys with major alloy constituents as follows:
aluminum
Greater than 95.0 %
copper
Less or equal than 5.0 %
silicon
Less or equal than 5.0 %
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, etc.) known by the responsible technical committee to effect the reliability of high purity aluminum 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 determines the concentrations of trace metallic impurities in high purity (99.99 wt. % pure, or purer, with respect to metallic trace impurities) aluminum-copper, aluminum-silicon and aluminum-copper-silicon alloys.
Formerly under the jurisdiction of Committee F01 on Electronics, this test method was withdrawn in November 2023. This standard is being withdrawn without replacement because Committee F01 was disbanded.
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Standards Content (Sample)
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.
Designation: F1845 − 08 (Reapproved 2016)
Standard Test Method for
Trace Metallic Impurities in Electronic Grade Aluminum-
Copper, Aluminum-Silicon, and Aluminum-Copper-Silicon
Alloys by High-Mass-Resolution Glow Discharge Mass
Spectrometer
This standard is issued under the fixed designation F1845; 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 Metals, Ores, and Related Materials
E1593 GuideforAssessingtheEfficacyofAirCareProducts
1.1 This test method determines the concentrations of trace
in Reducing the Perception of Indoor Malodor
metallic impurities in high purity (99.99 wt. % pure, or purer,
with respect to metallic trace impurities) aluminum-copper,
3. Terminology
aluminum-silicon and aluminum-copper-silicon alloys with
major alloy constituents as follows: 3.1 Terminology in this test method is consistent with
Terminology E135. Required terminology specific to this test
aluminum Greater than 95.0 %
copper Less or equal than 5.0 %
method, not covered in Terminology E135, is indicated in 3.2.
silicon Less or equal than 5.0 %
3.2 Definitions:
1.2 This test method pertains to analysis by magnetic-sector
3.2.1 campaign—a test procedure to determine the accuracy
glow discharge mass spectrometer (GDMS).
of the instrument, which was normally performed at the
1.3 This test method does not include all the information
beginning of the day or after the instrument modification, or
needed to complete GDMS analyses. Sophisticated computer-
both.
controlled laboratory equipment, skillfully used by an experi-
3.2.2 reference sample—material accepted as suitable for
enced operator, is required to achieve the required sensitivity.
use as a calibration/sensitivity reference standard by all parties
Thistestmethoddoescovertheparticularfactors(forexample,
concerned with the analyses.
specimen preparation, setting of relative sensitivity factors,
3.2.3 specimen—a suitably sized piece cut from a reference
determination of detection limits, etc.) known by the respon-
or test sample, prepared for installation in the GDMS ion
sible technical committee to effect the reliability of high purity
source, and analyzed.
aluminum analyses.
3.2.4 test sample—material(aluminumalloy)tobeanalyzed
1.4 This standard does not purport to address all of the
for trace metallic impurities by this GDMS method.
safety concerns, if any, associated with its use. It is the
3.2.4.1 Discussion—Generally the test sample is extracted
responsibility of the user of this standard to establish appro-
from a larger batch (lot, casting) of product and is intended to
priate safety and health practices and determine the applica-
be representative of the batch.
bility of regulatory limitations prior to use.
4. Summary of Test Method
2. Referenced Documents
4.1 A specimen is mounted in a plasma discharge cell.
2.1 ASTM Standards:
Atoms subsequently sputtered from the specimen surface are
E135 Terminology Relating to Analytical Chemistry for
ionized, and then focused as an ion beam through a double-
focusing magnetic-sector mass separation apparatus. The mass
spectrum (the ion current) is collected as magnetic field or
This test method is under the jurisdiction of ASTM Committee F01 on
acceleration voltage, (or both) is scanned.
Electronics and is the direct responsibility of Subcommittee F01.17 on Sputter
Metallization.
4.2 The ion current of an isotope at mass M is the total
i
Current edition approved May 1, 2016. Published May 2016. Originally
measured current, less contributions from all other interfering
approved in 1997. Last previous edition approved in 2008 as F1845 – 08. DOI:
10.1520/F1845-08R16.
sources. Portions of the measured current may originate from
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
the ion detector alone (detector noise). Portions may be due to
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
incompletelymassresolvedionsofanisotopeormoleculewith
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. mass close to, but not identical with, M. In all such instances
i
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
F1845 − 08 (2016)
the interfering contributions must be estimated and subtracted 6. Apparatus
from the measured signal.
6.1 Glow Discharge Mass Spectrometer , with mass resolu-
4.2.1 If the source of interfering contributions to the mea-
tion greater than 3500, and associated equipment and supplies.
sured ion current at M cannot be determined unambiguously,
i
TheGDMSmustbefittedwithanionsourcespecimencellthat
the measured current less the interfering contributions from
is cooled by liquid nitrogen, Peltier cooled, or cooled by an
identified sources constitutes an upper bound of the detection
equivalent method.
limit for the current due to the isotope.
6.2 Machining Apparatus, capable of preparing specimens
4.3 The composition of the test specimen is calculated from
andreferencesamplesinthedesiredgeometryandwithsmooth
the mass spectrum by applying a relative sensitivity factor
surfaces.
(RSF(X/M)) for each contaminant element, X, compared to the
6.3 Electro-Polishing Apparatus , capable of removing the
matrixelement, M.RSF’saredeterminedinaseparateanalysis
contaminants from the surfaces of specimens.
of a reference material performed under the same analytical
conditions, source configuration, and operating protocol as for
7. Reagents and Materials
the test specimen.
7.1 Reagents—Reagent and high purity grade reagents as
4.4 The relative concentrations of elements X and Y are
required (MeOH, HNO and HCl).
calculated from the relative isotopic ion currents I(X) and I(Y) 3
i j
in the mass spectrum, adjusted for the appropriate isotopic
7.2 Demineralized Water.
abundance factors (A(X), A(Y) and RSF’s. I(X) and I(Y) refer
i j i j
7.3 Tantalum Reference Sample.
to the measured ion current from isotopes X and Y ,
i j
7.4 Aluminum Reference Sample.
respectively, of atomic species X and Y as follows:
7.4.1 To the extent available, aluminum reference materials
~X!/~Y! 5 RSF~X/M!/RSF~Y/M! 3A~Y !/A~X ! 3I~X !/I~Y ! (1)
j i i j
shall be used to produce the GDMS relative sensitivity factors
where (X)/(Y) is the concentration ratio of atomic species X
for the various elements being determined (see Table 1).
to species Y. If species Y is taken to be the aluminum matrix
7.4.1.1 As necessary, non-aluminum reference materials
(RSF(M/M) = 1.0), (X) is (with only very small error for pure
may be used to produce the GDMS relative sensitivity factors
metal matrices) the absolute impurity concentration of X.
for the various elements being determined.
7.4.2 Reference materials should be homogeneous (see
5. Significance and Use
11.1) and free of cracks or porosity.
5.1 This test method is intended for application in the
7.4.3 At least two reference materials are required to estab-
semiconductor industry for evaluating the purity of materials
lish the relative sensitivity factors, including a 99.9999 % pure
(for example, sputtering targets, evaporation sources) used in
aluminum metal to establish the background contribution in
thin film metallization processes. This test method may be
analyses.
useful in additional applications, not envisioned by the respon-
7.4.4 The concentration of each analyte for relative sensi-
sible technical committee, as agreed upon between the parties
tivity factor determination should be at a factor of 100 greater
concerned.
than the detection limit determined using a 99.9999 % pure
aluminum specimen, but less than 100 ppmw.
5.2 This test method is intended for use by GDMS analysts
7.4.5 To meet expected analysis precision, it is necessary
invariouslaboratoriesforunifyingtheprotocolandparameters
that specimens of reference and test material present the same
for determining trace impurities in aluminum-copper,
size and configuration (shape and exposed length) in the glow
aluminum-silicon, and aluminum-copper-silicon alloys. The
discharge ion source, with a tolerance of 0.2 mm in diameter
objective is to improve laboratory-to-laboratory agreement of
and 0.5 mm in the distance of sample to cell ion exit slit.
analysis data. This test method is also directed to the users of
GDMS analyses as an aid to understanding the determination
8. Preparation of Reference Standards and Test
method, and the significance and reliability of reported GDMS
data. Specimens
5.3 For most metallic species the detection limit for routine 8.1 The surface of the parent material must not be included
analysis is on the order of 0.01 wt. ppm. With special in the specimen.
precautions, detection limits to sub-ppb levels are possible.
8.2 The machined surface of the specimen must be cleaned
5.4 This test method may be used as a referee method for by electropolishing or etching immediately prior to mounting
producers and users of electronic-grade aluminum-copper, the specimen and inserting it into the glow discharge ion
aluminum-silicon and aluminum-copper-silicon materials. source.
A
TABLE 1 Suite of Impurity Elements to Be Analyzed
NOTE 1—Establish RSFs for the following suite of elements:
silver arsenic gold boron beryllium calcium cerium chromium cesium copper iron
potassium lithium magnesium manganese sodium nickel phosphorus antimony silicon tin thorium
titanium uranium vanadium zinc zirconium
...
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: F1845 − 08 (Reapproved 2016)
Standard Test Method for
Trace Metallic Impurities in Electronic Grade Aluminum-
Copper, Aluminum-Silicon, and Aluminum-Copper-Silicon
Alloys by High-Mass-Resolution Glow Discharge Mass
Spectrometer
This standard is issued under the fixed designation F1845; 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 Metals, Ores, and Related Materials
E1593 Guide for Assessing the Efficacy of Air Care Products
1.1 This test method determines the concentrations of trace
in Reducing the Perception of Indoor Malodor
metallic impurities in high purity (99.99 wt. % pure, or purer,
with respect to metallic trace impurities) aluminum-copper,
3. Terminology
aluminum-silicon and aluminum-copper-silicon alloys with
major alloy constituents as follows: 3.1 Terminology in this test method is consistent with
Terminology E135. Required terminology specific to this test
aluminum Greater than 95.0 %
copper Less or equal than 5.0 %
method, not covered in Terminology E135, is indicated in 3.2.
silicon Less or equal than 5.0 %
3.2 Definitions:
1.2 This test method pertains to analysis by magnetic-sector
3.2.1 campaign—a test procedure to determine the accuracy
glow discharge mass spectrometer (GDMS).
of the instrument, which was normally performed at the
1.3 This test method does not include all the information
beginning of the day or after the instrument modification, or
needed to complete GDMS analyses. Sophisticated computer-
both.
controlled laboratory equipment, skillfully used by an experi-
3.2.2 reference sample—material accepted as suitable for
enced operator, is required to achieve the required sensitivity.
use as a calibration/sensitivity reference standard by all parties
This test method does cover the particular factors (for example,
concerned with the analyses.
specimen preparation, setting of relative sensitivity factors,
3.2.3 specimen—a suitably sized piece cut from a reference
determination of detection limits, etc.) known by the respon-
or test sample, prepared for installation in the GDMS ion
sible technical committee to effect the reliability of high purity
source, and analyzed.
aluminum analyses.
3.2.4 test sample—material (aluminum alloy) to be analyzed
1.4 This standard does not purport to address all of the
for trace metallic impurities by this GDMS method.
safety concerns, if any, associated with its use. It is the
3.2.4.1 Discussion—Generally the test sample is extracted
responsibility of the user of this standard to establish appro-
from a larger batch (lot, casting) of product and is intended to
priate safety and health practices and determine the applica-
be representative of the batch.
bility of regulatory limitations prior to use.
4. Summary of Test Method
2. Referenced Documents
4.1 A specimen is mounted in a plasma discharge cell.
2.1 ASTM Standards:
Atoms subsequently sputtered from the specimen surface are
E135 Terminology Relating to Analytical Chemistry for
ionized, and then focused as an ion beam through a double-
focusing magnetic-sector mass separation apparatus. The mass
spectrum (the ion current) is collected as magnetic field or
This test method is under the jurisdiction of ASTM Committee F01 on
acceleration voltage, (or both) is scanned.
Electronics and is the direct responsibility of Subcommittee F01.17 on Sputter
Metallization.
4.2 The ion current of an isotope at mass M is the total
i
Current edition approved May 1, 2016. Published May 2016. Originally
measured current, less contributions from all other interfering
approved in 1997. Last previous edition approved in 2008 as F1845 – 08. DOI:
10.1520/F1845-08R16.
sources. Portions of the measured current may originate from
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
the ion detector alone (detector noise). Portions may be due to
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
incompletely mass resolved ions of an isotope or molecule with
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. mass close to, but not identical with, M . In all such instances
i
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
F1845 − 08 (2016)
the interfering contributions must be estimated and subtracted 6. Apparatus
from the measured signal.
6.1 Glow Discharge Mass Spectrometer , with mass resolu-
4.2.1 If the source of interfering contributions to the mea-
tion greater than 3500, and associated equipment and supplies.
sured ion current at M cannot be determined unambiguously,
i
The GDMS must be fitted with an ion source specimen cell that
the measured current less the interfering contributions from
is cooled by liquid nitrogen, Peltier cooled, or cooled by an
identified sources constitutes an upper bound of the detection
equivalent method.
limit for the current due to the isotope.
6.2 Machining Apparatus, capable of preparing specimens
4.3 The composition of the test specimen is calculated from
and reference samples in the desired geometry and with smooth
the mass spectrum by applying a relative sensitivity factor
surfaces.
(RSF(X/M)) for each contaminant element, X, compared to the
6.3 Electro-Polishing Apparatus , capable of removing the
matrix element, M. RSF’s are determined in a separate analysis
contaminants from the surfaces of specimens.
of a reference material performed under the same analytical
conditions, source configuration, and operating protocol as for
7. Reagents and Materials
the test specimen.
7.1 Reagents—Reagent and high purity grade reagents as
4.4 The relative concentrations of elements X and Y are
required (MeOH, HNO and HCl).
calculated from the relative isotopic ion currents I(X ) and I(Y ) 3
i j
in the mass spectrum, adjusted for the appropriate isotopic
7.2 Demineralized Water.
abundance factors (A(X ), A(Y ) and RSF’s. I(X ) and I(Y ) refer
i j i j
7.3 Tantalum Reference Sample.
to the measured ion current from isotopes X and Y ,
i j
7.4 Aluminum Reference Sample.
respectively, of atomic species X and Y as follows:
7.4.1 To the extent available, aluminum reference materials
X / Y 5 RSF X/M /RSF Y/M 3A Y /A X 3I X /I Y (1)
~ ! ~ ! ~ ! ~ ! ~ ! ~ ! ~ ! ~ !
j i i j
shall be used to produce the GDMS relative sensitivity factors
where (X)/(Y) is the concentration ratio of atomic species X
for the various elements being determined (see Table 1).
to species Y. If species Y is taken to be the aluminum matrix
7.4.1.1 As necessary, non-aluminum reference materials
(RSF(M/M) = 1.0), (X) is (with only very small error for pure
may be used to produce the GDMS relative sensitivity factors
metal matrices) the absolute impurity concentration of X.
for the various elements being determined.
7.4.2 Reference materials should be homogeneous (see
5. Significance and Use
11.1) and free of cracks or porosity.
5.1 This test method is intended for application in the
7.4.3 At least two reference materials are required to estab-
semiconductor industry for evaluating the purity of materials
lish the relative sensitivity factors, including a 99.9999 % pure
(for example, sputtering targets, evaporation sources) used in
aluminum metal to establish the background contribution in
thin film metallization processes. This test method may be
analyses.
useful in additional applications, not envisioned by the respon-
7.4.4 The concentration of each analyte for relative sensi-
sible technical committee, as agreed upon between the parties
tivity factor determination should be at a factor of 100 greater
concerned.
than the detection limit determined using a 99.9999 % pure
aluminum specimen, but less than 100 ppmw.
5.2 This test method is intended for use by GDMS analysts
7.4.5 To meet expected analysis precision, it is necessary
in various laboratories for unifying the protocol and parameters
that specimens of reference and test material present the same
for determining trace impurities in aluminum-copper,
size and configuration (shape and exposed length) in the glow
aluminum-silicon, and aluminum-copper-silicon alloys. The
discharge ion source, with a tolerance of 0.2 mm in diameter
objective is to improve laboratory-to-laboratory agreement of
analysis data. This test method is also directed to the users of and 0.5 mm in the distance of sample to cell ion exit slit.
GDMS analyses as an aid to understanding the determination
method, and the significance and reliability of reported GDMS 8. Preparation of Reference Standards and Test
Specimens
data.
5.3 For most metallic species the detection limit for routine 8.1 The surface of the parent material must not be included
analysis is on the order of 0.01 wt. ppm. With special in the specimen.
precautions, detection limits to sub-ppb levels are possible.
8.2 The machined surface of the specimen must be cleaned
5.4 This test method may be used as a referee method for by electropolishing or etching immediately prior to mounting
producers and users of electronic-grade aluminum-copper, the specimen and inserting it into the glow discharge ion
aluminum-silicon and aluminum-copper-silicon materials. source.
A
TABLE 1 Suite of Impurity Elements to Be Analyzed
NOTE 1—Establish RSFs for the following suite of elements:
silver arsenic gold boron beryllium calcium cerium chromium cesium copper iron
potassium lithium magnesium manganese sodium nickel phosphorus antimony silicon tin thorium
titanium uranium vanadium zinc zirconium
A
Additional species may be determined and reported, as agreed u
...
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