ASTM E2371-04
(Test Method)Standard Test Method for Analysis of Titanium and Titanium Alloys by Atomic Emission Plasma Spectrometry (Withdrawn 2013)
Standard Test Method for Analysis of Titanium and Titanium Alloys by Atomic Emission Plasma Spectrometry (Withdrawn 2013)
SIGNIFICANCE AND USE
This method for the chemical analysis of titanium and titanium alloys is primarily intended to test material for compliance with specifications of chemical composition.
It is assumed that all who use this method will be trained analysts capable of performing common laboratory procedures skillfully and safely, and that the work will be performed in a properly equipped laboratory.
The method is designed to give the maximum flexibility analyzing elements in the titanium matrix. Thus options are given in calibration and analysis to accommodate the variety of ICP and DCP spectrometers and their auxiliary systems.
SCOPE
1.1 This method describes the analysis of titanium and titanium alloys by ICP-AES (Inductively Coupled Plasma) and DCP-AES (Direct Current Plasma) for the following elements:ElementApplicationRange (wt.%)QuantitativeRange (wt.%)Aluminum0-80.001 to 8.0Boron0-0.040.0008 to 0.01Chromium0-50.005 to 4.0Copper0-0.60.002 to 0.5Iron0-30.004 to 3.0Manganese0-0.040.001 to 0.01Molybdenum0-80.004 to 6.0Nickel0-10.001 to 1.0Silicon0-0.50.02 to 0.4Tin0-40.02 to 3.0Vanadium0-150.01 to 15.0Yttrium0-0.040.001 to 0.004Zirconium0-50.003 to 4.0
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 safety hazards statements are given in Section 9.
WITHDRAWN RATIONALE
Formerly under the jurisdiction of Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials, this test method was withdrawn in January 2013 in accordance with section 10.5.3.1 of the Regulations Governing ASTM Technical Committees, which requires that standards shall be updated by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
Relations
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: E2371 − 04
StandardTest Method for
Analysis of Titanium and Titanium Alloys by Atomic
Emission Plasma Spectrometry
This standard is issued under the fixed designation E2371; 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 E1479 Practice for Describing and Specifying Inductively-
Coupled Plasma Atomic Emission Spectrometers
1.1 This method describes the analysis of titanium and
E1601 Practice for Conducting an Interlaboratory Study to
titanium alloys by ICP-AES (Inductively Coupled Plasma) and
Evaluate the Performance of an Analytical Method
DCP-AES (Direct Current Plasma) for the following elements:
E1763 Guide for Interpretation and Use of Results from
Application Quantitative
Element
Interlaboratory Testing of Chemical Analysis Methods
Range (wt.%) Range (wt.%)
Aluminum 0–8 0.001 to 8.0 E1832 Practice for Describing and Specifying a Direct
Boron 0–0.04 0.0008 to 0.01
Current Plasma Atomic Emission Spectrometer
Chromium 0–5 0.005 to 4.0
E1914 Practice for Use of Terms Relating to the Develop-
Copper 0–0.6 0.002 to 0.5
Iron 0–3 0.004 to 3.0 ment and Evaluation of Methods for Chemical Analysis
Manganese 0–0.04 0.001 to 0.01
Molybdenum 0–8 0.004 to 6.0
3. Terminology
Nickel 0–1 0.001 to 1.0
Silicon 0–0.5 0.02 to 0.4
3.1 For definitions of terms used in this method, refer to
Tin 0–4 0.02 to 3.0
Terminology E135 and Terminology section in E1914.
Vanadium 0–15 0.01 to 15.0
Yttrium 0–0.04 0.001 to 0.004
4. Summary of Test Method
Zirconium 0–5 0.003 to 4.0
1.2 This standard does not purport to address all of the
4.1 Amineralacidsolutionofthesampleisaspiratedintoan
safety concerns, if any, associated with its use. It is the inductively coupled plasma or a direct current plasma spec-
responsibility of the user of this standard to establish appro-
trometer. The intensities of emission lines from the spectra of
priate safety and health practices and determine the applica- the analytes are measured and compared with calibration
bility of regulatory limitations prior to use. Specific safety
curves obtained from solutions containing known amounts of
hazards statements are given in Section 9. pure elements.
5. Significance and Use
2. Referenced Documents
5.1 This method for the chemical analysis of titanium and
2.1 ASTM Standards:
titanium alloys is primarily intended to test material for
D1193 Specification for Reagent Water
compliance with specifications of chemical composition.
E50 Practices for Apparatus, Reagents, and Safety Consid-
erations for Chemical Analysis of Metals, Ores, and
5.2 Itisassumedthatallwhousethismethodwillbetrained
Related Materials
analysts capable of performing common laboratory procedures
E135 Terminology Relating to Analytical Chemistry for
skillfully and safely, and that the work will be performed in a
Metals, Ores, and Related Materials
properly equipped laboratory.
E882 Guide for Accountability and Quality Control in the
5.3 The method is designed to give the maximum flexibility
Chemical Analysis Laboratory
analyzing elements in the titanium matrix. Thus options are
givenincalibrationandanalysistoaccommodatethevarietyof
ICP and DCP spectrometers and their auxiliary systems.
This test method is under the jurisdiction of ASTM Committee E01 on
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
6. Interferences
responsibility of Subcommittee E01.06 on Ti, Zr, W, Mo, Ta, Nb, Hf, Re.
6.1 Potential interferences for analytes (see 1.2) are listed in
Current edition approved June 1, 2004. Published June 2004. DOI: 10.1520/
E2371-04.
Table 1 for this method’s analytical wavelengths. The analyti-
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
cal wavelengths of Table 1 were selected for their freedom
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
from interference by the elements included in this method and
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. the titanium base (see Note 1).
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E2371 − 04
TABLE 1 Analytical Lines and Potential Interferences
commercial suppliers.The NISTStandard Reference Materials
Wavelength Potential (SRM) 3100 series are available as 10 mg/g (5 mg/g for some
Element Notes
(nm) Interferences
elements) solutions. See Notes 2 and 3.
Al 394.401
8.5.2 Reference solutions from other sources may be used if
B 249.678
they have a documented link of traceability to primary refer-
Cr 267.716
Cu 327.396 ence materials or CRMs from a national metrology institute
Fe 259.940
and the concentrations of impurities are known or determined
Mn 257.610
(see Note 4).
Mo 202.030
Ni 231.604
NOTE 2—To use solution standards of concentration less than the
Si 288.160 Cr
originalconcentration,preparethesolutionbydilutionoftheconcentrated
Sn 175.790 2
referencesolution.Maintaintheacidconcentrationasrecommendedinthe
242.949 Mo, Fe 3
V 292.402 Mo, Fe NIST or other certificate. NIST certificates provide instructions for
Y 360.073 Mo dilution by mass or by volume. Dilution by mass may be preferable to
Zr 343.823
pipetting, especially for solutions containing HF.
NOTE 3—The user should establish internal laboratory procedures that
Note—Sn 175.790 – Low UV Capable
specify a maximum shelf life for a working standard solution. It has been
Sn 242.949 – DCP; non-Low UV capable alternative
observedthatpolytetrafluoroethylene(PTFE)bottlespreservetheintegrity
of the solutions stored in them for a long period of time.
NOTE 4—If single element solutions are not provided with values for
NOTE 1—Elements outside the scope of this method may be present in
trace impurities, it is necessary to either determine the concentrations of
production materials or experimental titanium alloys. These potential
elementsthatareinthescopeofthismethodor,iftheycannotbedetected,
interferences must be tested for their effect as an interference on analyte
ensure that the method detection limit is sufficiently low that the
wavelengths and corrections made as necessary as a part of method
impurities cannot be detected in solutions prepared for calibration of this
development according to manufacturer’s instructions.
method.
7. Apparatus
8.5.3 Calibrants Prepared from Pure Metals or their Salts
(see Notes 5 and 6):
7.1 Direct Current Plasma Atomic Emission Spectrometers
used in this method may conform to the specifications given in
NOTE 5—Elemental solutions of 10.0 mg/mL or 1.00 mg/mL can be
Practice E1832.Adifferently designed instrument may provide stored in HDPE or polytetrafluoroethylene (PTFE) for one (1) year. The
0.100 mg/mL solutions must be made fresh before each use.
equivalent measurements. Suitability for use is determined by
NOTE 6—Elements and compounds for the solutions below are usually
comparing the results obtained with the precision and bias
supplied on a “metals basis” assay. The concentration of the element
statements contained in this method.
sought, as percent in the present usage, is the total metallic content of the
compound less the assayed metallic impurities (including B, Si, Y).
7.2 Inductively Coupled Plasma Atomic Emission Spec-
trometers used in this method may conform to the specifica- 8.5.3.1 Aluminum Standard Solution A (1 mL = 10.0 mg
tions given in Practice E1479. A differently designed instru-
Al)—Dissolve 10.000 g aluminum wire (purity 99.99 %, min)
mentmayprovideequivalentmeasurements.Suitabilityforuse
in 200 mL of HCl (1+1) with gentle heating. Cool, transfer to
is determined by comparing the results obtained with the a 1 L volumetric flask, dilute to the mark and mix. (A small
precision and bias statements contained in this method.
crystal of mercuric nitrate may be added to catalyze the
dissolution reaction.)
7.3 The sample introduction system shall be constructed of
8.5.3.2 Boron Standard Solution A (1 mL = 1.00 mg
materials resistant to all mineral acids including HF.
B)—Dissolve 5.720 g of boric acid, H BO (purity 99.99 %,
3 3
7.4 Each instrument shall be set up according to the manu-
min) in 500 mL of water. Transfer toa1L volumetric flask,
facturer’s instructions.
dilute to the mark and mix. Store in a plastic bottle.
8.5.3.3 Chromium Standard Solution A (1 mL = 10.0 mg
8. Reagents and Materials
Cr)—Dissolve 10.00 g of chromium (purity 99.99 %, min.)
8.1 Purity of reagents utilized in this procedure shall con-
chips in 200 mL of HCl (1+1) with gentle heating. Cool,
form to the requirements prescribed in Practice E50.
transfer to a 1 L volumetric flask, dilute to the mark and mix.
8.2 The purity of water used shall conform to the require- 8.5.3.4 Copper Standard Solution A (1 ML = 10.0 MG
CU)—Dissolve10.00gofcopperwire(purity99.99 %,min.)in
ments in Specification D1193 for reagent water, Type II.
100 mL of HNO (1+1) with gentle heating. Continue heating
8.3 The argon supply for the ICPor DCPplasma shall be of
until brown fumes cease to evolve. Cool, transfer toa1L
99.998 % minimum purity; for purging the ICP Optical path,
volumetric flask, and add 50 mL of HNO , dilute to the mark
99.999 % minimum purity.
and mix.
8.4 The nitrogen supply for purging the ICP Optical path
8.5.3.5 Copper Standard Solution B (1 mL = 1.00 mg
shall be 99.995 % minimum purity.
Cu)—Pipet 10 mL of Copper Standard Solution A into a 100
mL volumetric flask, add 10 mL of HNO , dilute to the mark
8.5 Reference solutions are available for purchase as an
and mix.
alternative to the preparation of solutions from pure metals or
compounds.
8.5.1 Single element reference solutions in the form of
Certified Reference Materials are available from the National
Available from National Institute of Standards and Technology, 100 Bureau
Institute of Standards and Technology (NIST) and a number of Drive, Gaithersburg, MD 20899, USA.
E2371 − 04
8.5.3.6 Iron Standard Solution A (1 mL = 10.0 mg Fe)— 8.8 Asurfactant may be used to control droplet formation in
Dissolve 10.00 g of iron rod (purity 99.99 %, min, that has the spray chamber and sample tubes of the DCP spectrometer.
been cleaned to remove oxidation) in 100 mL of HNO by A maximum 0.1 % Vol/Vol of a surfactant such as
heating to boiling. Continue gentle boiling until brown fumes Polyoxyethyene(10)isooctylphenyl ether is recommended.
cease to evolve. Cool, transfer toa1Lvolumetric flask, dilute
8.9 Calibration Solutions:
to the mark and mix.
8.9.1 Standard Solution A:
8.5.3.7 Manganese Standard Solution A (1 mL = 1.00 mg
8.9.1.1 Add5.00g(ICPsystem)or10.00g(DCPsystem)of
Mn)—Dissolve 1.000 g of manganese (purity 99.98 %, min) in
titanium (purity 99.99 %, min) toa1Lplastic volumetric flask
100 mL of HNO (1+1) with gentle heating. Boil gently to
(see Note 8).
expelbrownfumesandcool.Transfertoa1Lvolumetricflask,
NOTE 8—The ICP procedure and DCP procedure require differing
add 50 mL of HNO , dilute to the mark and mix.
sample sizes. This is maintained consistently throughout the method in
8.5.3.8 Molybdenum Standard Solution A (1 mL = 10.0 mg
terms of sample weights and analyte additions for samples, calibration
Mo)—Transfer 5.00 g of molybdenum rod (purity 99.98 %,
solutions and quality control solutions.
min) to a 600 mL beaker. Add 200 mL of an acid mixture of
8.9.1.2 Add150mLofHCl,then20mLofHF(seewarning
HCl, HNO and water (3+2+1) and heat gently to dissolve.
note below in 8.9.1.4).
Cool, transfer to a 500 mL volumetric flask, dilute to the mark
8.9.1.3 After all titanium has dissolved, add 10 mL of
and mix.
HNO (ICP) or 15 mL of HNO (DCP) to oxidize.
3 3
8.5.3.9 Nickel Standard Solution A (1 mL = 10.0 mg
8.9.1.4 Cool, add internal standard solution and/or surfac-
Ni)—Dissolve 10.00 g of nickel wire (purity 99.99 %, min) in
tant if desired, dilute to the mark and mix. (Warning—HF
100 mL of HNO with gentle heating. Continue heating until
causes burns that require immediate medical attention even
brown fumes are no longer evolved. Cool, transfer toa1L
though they are not immediately painful; refer to the paragraph
volumetric flask, dilute to the mark and mix.
about HF in the Safety Precautions of Practice E50.)
8.5.3.10 Nickel Standard Solution B (1 mL = 1.00 mg
8.9.1.5 Store in a polytetrafluoroethylene (PTFE) bottle.
Ni)—Pipet10mLofNickelStandardSolutionAintoa100mL
Label the bottle and mark with the date of preparation. This
volumetric flask, add 10 mL of HNO , dilute to the mark and
solution’s shelf life is six (6) months.
mix.
8.9.1.6 Adjust the “0” values of Standard A to reflect the
8.5.3.11 Silicon Standard Solution A (1 mL = 1.00 mg
actual concentration of the analytes in the titanium base
Si)—Fuse 0.2139 g of silicon dioxide (purity 99.99 %, min)
material before calibration.
with 2.00 g of sodium carbonate (purity 99.995 %, min) in a
8.9.2 Standard Solutions B-G:
platinum crucible. Dissolve the melt in water, transfer to a 100
8.9.2.1 Weigh quantities of titanium (purity 99.99 % min)
mL flask, dilute to the mark and mix. Store in a plastic bottle.
into 1 Lplastic volumetric flasks in accordance with Appendix
8.5.3.12 Tin Standard Solution A (1 mL = 10.0 mg Sn)—
X1 for ICP and Appendix X2 for DCP.
Dissolve 10.00 g of tin wire (purity 99.99 %, min) in 100 mL
8.9.2.2 To each, add the specified volumes of HCl and HF
of HCl with gentle heating. Cool, transfer toa1L volumetric
(see warning in 8.9.1.4) in accordance with Appendix X1 for
flask, and add 400 mL of HCl, dilute to the mark and mix.
ICP and Appendix X2 for DCP.
8.5.3.13 Vanadium Standard Solution A (1 mL = 10.0 mg
8.9.2.3 After the titanium dissolves completely, add the
V)—Dissolve 17.852 g of vanadium (V) oxide (V O ) (purity
2 5
specified volumes of HNO in accordance with Appendix X1
99.99 %, min) ina1L volumetric flask by adding 300 mL of
for ICP and Appendix X2 for DCP.
HCl and warm (≤ 75°C) to complete dissolution. Cool, dilute
8.9.2.4 Cool, add volumes of standard solutions in accor-
to the mark and mix.
dance with Appendix X1 for ICP and Appendix X2 for DCP.
8.5.3.14 Yttrium Standard Solution A (1 mL = 1.00 mg
8.9.2.5 Add internal standard solution and/or surfactant if
Y)—Dissolve1.270gofyttriumoxide(Y O )(purity99.99 %,
2 3
desired. Dilute to volume and mix. Store in a polytetrafluoro-
min) in 30 mLof HCl (1+1).Transfer toalLvolumetric flask,
ethylene (PTFE) bottle. Shelf life is three (3) months.
dilute to the mark and mix.
8.9.2.6 Adjust the concentration values of Standard Solu-
8.5.3.15 Zirconium Standard Solution A (1 mL = 10.0 mg
tio
...
Questions, Comments and Discussion
Ask us and Technical Secretary will try to provide an answer. You can facilitate discussion about the standard in here.