ASTM F1710-08(2016)
(Test Method)Standard Test Method for Trace Metallic Impurities in Electronic Grade Titanium by High Mass-Resolution Glow Discharge Mass Spectrometer (Withdrawn 2023)
Standard Test Method for Trace Metallic Impurities in Electronic Grade Titanium by High Mass-Resolution Glow Discharge Mass Spectrometer (Withdrawn 2023)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 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.
5.3 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.
5.4 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.
WITHDRAWN RATIONALE
This test method covers the determination of concentrations of trace metallic impurities in high purity titanium.
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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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: F1710 − 08 (Reapproved 2016)
Standard Test Method for
Trace Metallic Impurities in Electronic Grade Titanium by
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
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
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.
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 May 1, 2016. Published May 2016. Originally
approved in 1996. Last previous edition approved in 2008 as F1710–08. DOI:
discharge cell. Atoms subsequently sputtered from the speci-
10.1520/F1710-08R16.
men surface are ionized, and then focused as an ion beam
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
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
F1710 − 08 (2016)
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 current of an isotope at mass M is the total is cooled by liquid nitrogen, Peltier cooled, or cooled by an
i
measured current, less contributions from all other interfering equivalent method.
sources. Portions of the measured current may originate from
6.2 Machining Apparatus, capable of preparing specimens
the ion detector alone (detector noise). Portions may be due to
and reference samples in the required geometry and with
incompletelymassresolvedionsofanisotopeormoleculewith
smooth surfaces.
mass close to, but not identical with, M. In all such instances
i
7. Reagents and Materials
the interfering contributions must be estimated and subtracted
from the measured signal.
7.1 Reagent and High Purity Grade Reagents, as required
4.2.1 If the source of interfering contributions to the mea-
(MeOH, HNO,HF,H O ).
3 2 2
sured ion current at M cannot be determined unambiguously,
i
7.2 Demineralized Water.
the measured current less the interfering contributions from
identified sources constitutes an upper bound of the detection 7.3 Tantalum Reference Sample.
limit for the current due to the isotope.
7.4 Titanium Reference Sample.
4.3 The composition of the test specimen is calculated from 7.4.1 To the extent available, titanium reference materials
shall be used to produce the GDMS relative sensitivity factors
the mass spectrum by applying a relative sensitivity factor
(RSF(X/M)) for each contaminant element, X, compared to the for the various elements being determined (Table 1).
7.4.2 Asnecessary,non-titaniumreferencematerialsmaybe
matrixelement, M. RSF’saredeterminedinaseparateanalysis
of a reference material performed under the same analytical used to produce the GDMS relative sensitivity factors for the
various elements being determined.
conditions, source configuration, and operating protocol as for
7.4.3 Reference materials should be homogeneous and free
the test specimen.
of cracks or porosity.
4.4 The relative concentrations of elements X and Y are
7.4.4 At least two reference materials are required to estab-
calculatedfromtherelativeisotopicioncurrents I(X)and I(Y)
i j
lish the relative sensitivity factors, including one nominally
in the mass spectrum, adjusted for the appropriate isotopic
99.999% pure (5N-grade) or better titanium metal to establish
abundancefactors (A(X), A(Y))and RSF’s. I(X)and I(Y)refer
i j i j
the background contribution in analyses.
to the measured ion current from isotopes X and Y,
i j
7.4.5 The concentration of each analyte for relative sensi-
respectively, of atomic species X and Y as follows:
tivity factor determination should be a factor of 100 greater
X / Y 5 RSF X/M /RSF Y/M 3A Y /A X 3I X /I Y , (1)
@ # @ # ~ ! ~ ! ~ ! ~ ! ~ ! ~ !
j i i j
than the detection limit determined using a nominally
99.999%pure(5N-grade)orbettertitaniumspecimen,butless
where (X)/(Y) is the concentration ratio of atomic species X
than 100 ppmw.
to species Y. If species Y is taken to be the titanium matrix
7.4.6 To meet expected analysis precision, it is necessary
(RSF(M/M) =1.0), (X) is (with only very small error for pure
that specimens of reference and test material present the same
metal matrices) the absolute impurity concentration of X.
size and configuration (shape and exposed length) in the glow
5. Significance and Use
discharge ion source, with a tolerance of 0.2 mm in diameter
and 0.5 mm in the distance of specimen to cell ion exit slit.
5.1 This test method is intended for application in the
semiconductor industry for evaluating the purity of materials
8. Preparation of Reference Standards and Test
(for example, sputtering targets, evaporation sources) used in
Specimens
thin film metallization processes. This test method may be
8.1 The surface of the parent material must not be included
usefulinadditionalapplications,notenvisionedbytherespon-
in the specimen.
sible technical committee, as agreed upon between the parties
concerned.
8.2 The machined surface of the specimen must be cleaned
by chemical etching immediately prior to mounting the speci-
5.2 This test method is intended for use by GDMS analysts
men and inserting it into the glow discharge ion source.
invariouslaboratoriesforunifyingtheprotocolandparameters
8.2.1 Inordertoobtainarepresentativebulkcompositionin
fordeterminingtraceimpuritiesinpuretitanium.Theobjective
a reasonable analysis time, surface cleaning must remove all
is to improve laboratory to laboratory agreement of analysis
contaminantswithoutalteringthecompositionofthespecimen
data. This test method is also directed to the users of GDMS
surface.
analyses as an aid to understanding the determination method,
8.2.2 To minimize the possibility of contamination, clean
and the significance and reliability of reported GDMS data.
eachspecimenseparatelyimmediatelypriortomountinginthe
5.3 For most metallic species the detection limit for routine
glow discharge ion source.
analysis is on the order of 0.01 weight ppm. With special
8.2.3 Prepare and use etching solutions in a clean container
precautions detection limits to sub-ppb levels are possible.
insoluble in the contained solution.
5.4 This test method may be used as a referee method for 8.2.4 Useful etching solutions are HNO :HF::3:1 or
producers and users of electronic-grade titanium materials. HNO :HF:H O : :1:1:1 or H O:HNO :HF:H O ::20:5:5:4
3 2 2 2 3 2 2
F1710 − 08 (2016)
TABLE 1 Suite of Impurity Elements to be Analyzed, with
(double etched), etching until smooth, clean metal is exposed
Appropriate Isotope Selection
over the entire surface.
NOTE 1—Establish RSFs for the following suite of elements, using the
8.2.5 Immediately after cleaning, wash the specimen with
indicated isotopes for establishing RSF values and for performing
high purity rinses and thoroughly dry the specimen in the
analyses of test specimens.
laboratory environment.
NOTE 2—This selection of isotopes minimizes significant interferences
NOTE1—Examplesofacceptablehighpurityrinsesareverylargescale
(see Annex A1.). Additional species may be determined and reported, as
integration (VLSI) grade methanol and distilled water.
agreeduponbyallpartiesconcernedwiththeanalyses.Otherisotopescan
be selected to assist mass spectrum peak identification or for other
8.3 Immediately mount and insert the specimen into the
purposes.
glow discharge ion source, minimizing exposure of the
Lithium Li
9 cleaned, rinsed, specimen surface to the laboratory environ-
Beryllium Be
Boron B
ment.
Carbon C
14 8.3.1 As necessary, use a noncontacting gage when mount-
Nitrogen N
Oxygen O ing specimens in the analysis cell specimen holder to ensure
Fluorine F
thepropersampleconfigurationintheglowdischargecell(see
Sodium Na
7.4.6).
Magnesium Mg
Aluminum Al
8.4 Sputter etch the specimen surface in the glow discharge
Silicon Si
Phophorus P
plasma for a period of time before data acquisition (12.3)to
Sulfur S
ensure the cleanliness of the surface. Pre-analysis sputtering
Chlorine Cl
conditions can be limited by the need to maintain sample
Potassium K
Calcium Ca
integrity. If sputter cleaning and analysis are carried out under
Scandium Sc
differentplasmaconditions,accuracyshouldbeestablishedfor
Titanium Ti
the analytical protocol adopted and elements measured.
Vanadium V
Chromium Cr
Manganese Mn
56 9. Preparation of the GDMS Apparatus
Iron Fe
Cobalt Co
60 9.1 The ultimate background pressure in the ion source
Nickel Ni
−6
Copper Cu chambershouldbelessthan1×10 torrbeforeoperation.The
66 68
Zinc Zn or Zn
background pressure in the mass analyzer should be less than
69 71
Gallium Ga or Ga
−7
70 73
5×10 torr during operation.
Germanium Ge or Ge
Arsenic As
9.2 The glow discharge ion source must be cooled to near
Selenium Se
Bromine Br
liquid nitrogen temperature.
Rubidium Rb
Y
Yttrium
9.3 The GDMS instrument must be accurately mass cali-
Zirconium Zr
brated prior to measurements.
Niobium Nb
Molybdenum Mo
9.4 The GDMS instrument must be adjusted to the appro-
Ruthenium Ru
Rhodium Rh priate mass peak shape and mass resolving power for the
Silver Ag
required analysis.
106 108
Palladium Pd or Pd
Cadmium Cd
9.5 Iftheinstrumentusesdifferentioncollectorstomeasure
Indium In
117 119 ion currents during the same analysis, the measurement effi-
Tin Sn or Sn
Antimony Sb
ciency of each detector relative to the others should be
Iodine I
determined at least weekly.
125 130
Tellurium Te or Te
Cesium Cs 9.5.1 If both Faraday cup collector for ion current measure-
Barium Ba
ment and ion counting detectors are used during the same
Lanthanum La
140 analysis, the ion counting efficiency (ICE) must be determined
Cerium Ce
Neodymium Nd
prior to each campaign of specimen analyses using the follow-
176 178
Hafnium Hf or Hf
ing or equivalent procedures:
Tantalum Ta
Tungsten W 9.5.1.1 Using a specimen of tantalum, measure the ion
Rhenium Re
current from the major isotope ( Ta) using the ion current
190 192
Osmium Os or Os
Faraday cup detector, and measure the ion current from the
Iridium Ir
194 196
Platinum Pt or Pt minorisotope( Ta)usingtheioncountingdetector,withcare
Gold Au
to avoid ion counting losses due to ion-counting system dead
201 202
Hg or Hg
Mercury
times. The counting loss should be 1% or less.
Thallium Tl
Lead Pb
9.5.1.2 The ion counting efficiency is calculated by multi-
Bismuth Bi
180 181
232 plyingtheratioofthe Taioncurrenttothe Taioncurrent
Thorium Th
181 180
Uranium U
by the Ta/ Ta isotopic ratio. The result of this calculation
is the ion counting detector efficiency (ICE).
F1710 − 08 (2016)
TABLE 2 Required Relative Standard Deviation (RSD) for RSF
ini
...
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: F1710 − 08 (Reapproved 2016)
Standard Test Method for
Trace Metallic Impurities in Electronic Grade Titanium by
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. 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 Chemical Analysis of Metals (Withdrawn
1998)
1.1 This test method covers the determination of concentra-
E180 Practice 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 This test method pertains to analysis by magnetic-sector
cialty Chemicals (Withdrawn 2009)
glow discharge mass spectrometer (GDMS).
E691 Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method
1.3 The titanium matrix must be 99.9 weight % (3N-grade)
pure, or purer, with respect to metallic impurities. There must E1257 Guide for Evaluating Grinding Materials Used for
Surface Preparation in Spectrochemical Analysis
be no major alloy constituent, for example, aluminum or iron,
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:
This test method does cover the particular factors (for example,
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.
ion source specimen cell is often the boundary event separating
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
source, and analyzed.
2.1 ASTM Standards:
E135 Terminology Relating to Analytical Chemistry for
3.2.4 test sample—material titanium to be analyzed for trace
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
from a larger batch (lot, casting) of product and is intended to
be representative of the batch.
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 May 1, 2016. Published May 2016. Originally
approved in 1996. Last previous edition approved in 2008 as F1710 – 08. DOI:
discharge cell. Atoms subsequently sputtered from the speci-
10.1520/F1710-08R16.
men surface are ionized, and then focused as an ion beam
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
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
F1710 − 08 (2016)
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.
The GDMS must be fitted with an ion source specimen cell that
4.2 The ion current of an isotope at mass M is the total is cooled by liquid nitrogen, Peltier cooled, or cooled by an
i
measured current, less contributions from all other interfering equivalent method.
sources. Portions of the measured current may originate from
6.2 Machining Apparatus, capable of preparing specimens
the ion detector alone (detector noise). Portions may be due to
and reference samples in the required geometry and with
incompletely mass resolved ions of an isotope or molecule with
smooth surfaces.
mass close to, but not identical with, M . In all such instances
i
7. Reagents and Materials
the interfering contributions must be estimated and subtracted
from the measured signal.
7.1 Reagent and High Purity Grade Reagents, as required
4.2.1 If the source of interfering contributions to the mea-
(MeOH, HNO , HF, H O ).
3 2 2
sured ion current at M cannot be determined unambiguously,
i
7.2 Demineralized Water.
the measured current less the interfering contributions from
7.3 Tantalum Reference Sample.
identified sources constitutes an upper bound of the detection
limit for the current due to the isotope.
7.4 Titanium Reference Sample.
7.4.1 To the extent available, titanium reference materials
4.3 The composition of the test specimen is calculated from
the mass spectrum by applying a relative sensitivity factor shall be used to produce the GDMS relative sensitivity factors
for the various elements being determined (Table 1).
(RSF(X/M)) for each contaminant element, X, compared to the
matrix element, M . RSF’s are determined in a separate analysis 7.4.2 As necessary, non-titanium reference materials may be
used to produce the GDMS relative sensitivity factors for the
of a reference material performed under the same analytical
various elements being determined.
conditions, source configuration, and operating protocol as for
7.4.3 Reference materials should be homogeneous and free
the test specimen.
of cracks or porosity.
4.4 The relative concentrations of elements X and Y are
7.4.4 At least two reference materials are required to estab-
calculated from the relative isotopic ion currents I(X ) and I(Y )
i j
lish the relative sensitivity factors, including one nominally
in the mass spectrum, adjusted for the appropriate isotopic
99.999 % pure (5N-grade) or better titanium metal to establish
abundance factors (A(X ), A(Y )) and RSF’s. I(X ) and I(Y ) refer
i j i j
the background contribution in analyses.
to the measured ion current from isotopes X and Y ,
i j
7.4.5 The concentration of each analyte for relative sensi-
respectively, of atomic species X and Y as follows:
tivity factor determination should be a factor of 100 greater
@X#/@Y# 5 RSF~X/M!/RSF~Y/M! 3A~Y !/A~X ! 3I~X !/I~Y !, (1)
j i i j
than the detection limit determined using a nominally
99.999 % pure (5N-grade) or better titanium specimen, but less
where (X)/(Y) is the concentration ratio of atomic species X
than 100 ppmw.
to species Y. If species Y is taken to be the titanium matrix
7.4.6 To meet expected analysis precision, it is necessary
(RSF(M/M) = 1.0), (X) is (with only very small error for pure
that specimens of reference and test material present the same
metal matrices) the absolute impurity concentration of X.
size and configuration (shape and exposed length) in the glow
5. Significance and Use
discharge ion source, with a tolerance of 0.2 mm in diameter
and 0.5 mm in the distance of specimen to cell ion exit slit.
5.1 This test method is intended for application in the
semiconductor industry for evaluating the purity of materials
8. Preparation of Reference Standards and Test
(for example, sputtering targets, evaporation sources) used in
Specimens
thin film metallization processes. This test method may be
8.1 The surface of the parent material must not be included
useful in additional applications, not envisioned by the respon-
in the specimen.
sible technical committee, as agreed upon between the parties
concerned.
8.2 The machined surface of the specimen must be cleaned
by chemical etching immediately prior to mounting the speci-
5.2 This test method is intended for use by GDMS analysts
men and inserting it into the glow discharge ion source.
in various laboratories for unifying the protocol and parameters
8.2.1 In order to obtain a representative bulk composition in
for determining trace impurities in pure titanium. The objective
a reasonable analysis time, surface cleaning must remove all
is to improve laboratory to laboratory agreement of analysis
contaminants without altering the composition of the specimen
data. This test method is also directed to the users of GDMS
surface.
analyses as an aid to understanding the determination method,
8.2.2 To minimize the possibility of contamination, clean
and the significance and reliability of reported GDMS data.
each specimen separately immediately prior to mounting in the
5.3 For most metallic species the detection limit for routine
glow discharge ion source.
analysis is on the order of 0.01 weight ppm. With special
8.2.3 Prepare and use etching solutions in a clean container
precautions detection limits to sub-ppb levels are possible.
insoluble in the contained solution.
5.4 This test method may be used as a referee method for 8.2.4 Useful etching solutions are HNO :HF::3:1 or
producers and users of electronic-grade titanium materials. HNO :HF:H O : :1:1:1 or H O:HNO :HF:H O ::20:5:5:4
3 2 2 2 3 2 2
F1710 − 08 (2016)
TABLE 1 Suite of Impurity Elements to be Analyzed, with
(double etched), etching until smooth, clean metal is exposed
Appropriate Isotope Selection
over the entire surface.
NOTE 1—Establish RSFs for the following suite of elements, using the
8.2.5 Immediately after cleaning, wash the specimen with
indicated isotopes for establishing RSF values and for performing
high purity rinses and thoroughly dry the specimen in the
analyses of test specimens.
laboratory environment.
NOTE 2—This selection of isotopes minimizes significant interferences
NOTE 1—Examples of acceptable high purity rinses are very large scale
(see Annex A1.). Additional species may be determined and reported, as
integration (VLSI) grade methanol and distilled water.
agreed upon by all parties concerned with the analyses. Other isotopes can
be selected to assist mass spectrum peak identification or for other
8.3 Immediately mount and insert the specimen into the
purposes.
glow discharge ion source, minimizing exposure of the
Lithium Li
cleaned, rinsed, specimen surface to the laboratory environ-
Beryllium Be
Boron B ment.
Carbon C
14 8.3.1 As necessary, use a noncontacting gage when mount-
Nitrogen N
Oxygen O ing specimens in the analysis cell specimen holder to ensure
Fluorine F
the proper sample configuration in the glow discharge cell (see
Sodium Na
26 7.4.6).
Magnesium Mg
Aluminum Al
28 8.4 Sputter etch the specimen surface in the glow discharge
Silicon Si
Phophorus P
plasma for a period of time before data acquisition (12.3) to
Sulfur S
ensure the cleanliness of the surface. Pre-analysis sputtering
Chlorine Cl
conditions can be limited by the need to maintain sample
Potassium K
Calcium Ca
integrity. If sputter cleaning and analysis are carried out under
Scandium Sc
different plasma conditions, accuracy should be established for
Titanium Ti
the analytical protocol adopted and elements measured.
Vanadium V
Chromium Cr
Manganese Mn
56 9. Preparation of the GDMS Apparatus
Iron Fe
Cobalt Co
60 9.1 The ultimate background pressure in the ion source
Nickel Ni
−6
Copper Cu chamber should be less than 1 × 10 torr before operation. The
66 68
Zinc Zn or Zn
background pressure in the mass analyzer should be less than
69 71
Gallium Ga or Ga
−7
70 73 5 × 10 torr during operation.
Germanium Ge or Ge
Arsenic As
9.2 The glow discharge ion source must be cooled to near
Selenium Se
Bromine Br
liquid nitrogen temperature.
Rubidium Rb
Yttrium Y
9.3 The GDMS instrument must be accurately mass cali-
Zirconium Zr
brated prior to measurements.
Niobium Nb
Molybdenum Mo
101 9.4 The GDMS instrument must be adjusted to the appro-
Ruthenium Ru
Rhodium Rh priate mass peak shape and mass resolving power for the
Silver Ag
required analysis.
106 108
Palladium Pd or Pd
Cadmium Cd
9.5 If the instrument uses different ion collectors to measure
Indium In
117 119
ion currents during the same analysis, the measurement effi-
Tin Sn or Sn
Antimony Sb
ciency of each detector relative to the others should be
Iodine I
determined at least weekly.
125 130
Tellurium Te or Te
Cesium Cs 9.5.1 If both Faraday cup collector for ion current measure-
Barium Ba
ment and ion counting detectors are used during the same
Lanthanum La
analysis, the ion counting efficiency (ICE) must be determined
Cerium Ce
Neodymium Nd prior to each campaign of specimen analyses using the follow-
176 178
Hafnium Hf or Hf
ing or equivalent procedures:
Tantalum Ta
Tungsten W 9.5.1.1 Using a specimen of tantalum, measure the ion
Rhenium Re
current from the major isotope ( Ta) using the ion current
190 192
Osmium Os or Os
191 Faraday cup detector, and measure the ion current from the
Iridium Ir
194 196 180
Platinum Pt or Pt
minor isotope ( Ta) using the ion counting detector, with care
Gold Au
to avoid ion counting losses due to ion-counting system dead
201 202
Mercury Hg or Hg
times. The counting loss should be 1 % or less.
Thallium Tl
Lead Pb
9.5.1.2 The ion counting efficiency is calculated by multi-
Bismuth Bi
180 181
plying the ratio of the Ta ion current to the Ta ion current
Thorium Th
181 180
Uranium U
by the Ta/ Ta isotopic ratio. The result of this calculation
is the ion counting detector efficiency (ICE).
F1710 − 08 (2
...
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