ASTM E2594-09
(Test Method)Standard Test Method for Analysis of Nickel Alloys by Inductively Coupled Plasma Atomic Emission Spectrometry (Performance-Based Method)
Standard Test Method for Analysis of Nickel Alloys by Inductively Coupled Plasma Atomic Emission Spectrometry (Performance-Based Method)
SIGNIFICANCE AND USE
This test method for the chemical analysis of nickel alloys is primarily intended to test material for compliance with specifications such as those under jurisdiction of ASTM Committee B02. It may also be used to test compliance with other specifications that are compatible with the test method.
It is assumed that all who use this test 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.
This is a performance-based test method that relies more on the demonstrated quality of the test result than on strict adherence to specific procedural steps. It is expected that laboratories using this test method will prepare their own work instructions. These work instructions will include detailed operating instructions for the specific laboratory, the specific reference materials employed, and performance acceptance criteria. It is also expected that, when applicable, each laboratory will participate in proficiency test programs, such as described in Practice E 2027, and that the results from the participating laboratory will be satisfactory.
SCOPE
1.1 This test method describes the inductively coupled plasma atomic emission spectrometric analysis of nickel alloys, such as specified by Committee B02, and having chemical compositions within the following limits: ElementApplication
Range (%) Aluminum0.01–1.00 Boron0.001–0.050 Calcium0.001–0.05 Carbon0.10–0.20 Chromium0.01–33.0 Cobalt0.10–20.0 Copper0.01–3.00 Iron0.01–50.0 Lead0.001–0.01 Magnesium0.0001–0.100 Manganese0.01–3.0 Molybdenum0.01–30.0 Niobium0.01–6.0 Nickel25.0–80.0 Nitrogen0.001–0.20 Oxygen0.0001–0.003 Phosphorous0.001–0.030 Sulfur0.0001–0.010 Silicon0.01–1.50 Tantalum0.005–0.10 Tin0.001–0.020 Titanium0.001–6.0 Tungsten0.01–5.0 Vanadium0.01–1.0 Zirconium0.01–0.10
1.2 The following elements may be determined using this test method. The test method user should carefully evaluate the precision and bias statements of this test method to determine applicability of the test method for the intended use. ElementQuantification
Range (%) Aluminum0.060–1.40 Boron0.002–0.020 Calcium0.001–0.003 Copper0.010–0.52 Magnesium0.001–0.10 Manganese0.002–0.65 Niobium0.020–5.5 Phosphorous0.004–0.030 Tantalum0.010–0.050 Tin0.002–0.018 Titanium0.020–3.1 Tungsten0.007–0.11 Vanadium0.010–0.50 Zirconium0.002–0.10
1.3 This test method has only been interlaboratory tested for the elements and ranges specified. It may be possible to extend this test method to other elements or different concentration ranges provided that method validation is performed that includes evaluation of method sensitivity, precision, and bias as described in this document. Additionally, the validation study must evaluate the acceptability of sample preparation methodology using reference materials or spike recoveries, or both. The user is cautioned to carefully evaluate the validation data against the laboratory’s data quality objectives. Method validation of scope extensions is also a requirement of ISO/IEC 17025.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
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. Specific warning statements are given in 8.2.6.3 and safety hazard statements are given in Section 9.
General Information
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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: E2594 − 09
StandardTest Method for
Analysis of Nickel Alloys by Inductively Coupled Plasma
Atomic Emission Spectrometry (Performance-Based
Method)
This standard is issued under the fixed designation E2594; 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
Quantification
Element
Range (%)
1.1 This test method describes the inductively coupled
Manganese 0.002–0.65
plasma atomic emission spectrometric analysis of nickel Niobium 0.020–5.5
Phosphorous 0.004–0.030
alloys, such as specified by Committee B02, and having
Tantalum 0.010–0.050
chemical compositions within the following limits:
Tin 0.002–0.018
Titanium 0.020–3.1
Application
Element
Tungsten 0.007–0.11
Range (%)
Vanadium 0.010–0.50
Aluminum 0.01–1.00
Zirconium 0.002–0.10
Boron 0.001–0.050
Calcium 0.001–0.05
1.3 Thistestmethodhasonlybeeninterlaboratorytestedfor
Carbon 0.10–0.20
the elements and ranges specified. It may be possible to extend
Chromium 0.01–33.0
Cobalt 0.10–20.0 this test method to other elements or different concentration
Copper 0.01–3.00
ranges provided that method validation is performed that
Iron 0.01–50.0
includesevaluationofmethodsensitivity,precision,andbiasas
Lead 0.001–0.01
Magnesium 0.0001–0.100
described in this document. Additionally, the validation study
Manganese 0.01–3.0
must evaluate the acceptability of sample preparation method-
Molybdenum 0.01–30.0
ology using reference materials or spike recoveries, or both.
Niobium 0.01–6.0
Nickel 25.0–80.0 The user is cautioned to carefully evaluate the validation data
Nitrogen 0.001–0.20
against the laboratory’s data quality objectives. Method vali-
Oxygen 0.0001–0.003
dation of scope extensions is also a requirement of ISO/
Phosphorous 0.001–0.030
Sulfur 0.0001–0.010
IEC 17025.
Silicon 0.01–1.50
1.4 The values stated in SI units are to be regarded as
Tantalum 0.005–0.10
Tin 0.001–0.020
standard. No other units of measurement are included in this
Titanium 0.001–6.0
standard.
Tungsten 0.01–5.0
Vanadium 0.01–1.0
1.5 This standard does not purport to address all of the
Zirconium 0.01–0.10
safety concerns, if any, associated with its use. It is the
1.2 The following elements may be determined using this
responsibility of the user of this standard to establish appro-
test method.The test method user should carefully evaluate the
priate safety and health practices and determine the applica-
precision and bias statements of this test method to determine
bility of regulatory limitations prior to use. Specific warning
applicability of the test method for the intended use.
statementsaregivenin8.2.6.3andsafetyhazardstatementsare
Quantification
given in Section 9.
Element
Range (%)
Aluminum 0.060–1.40
2. Referenced Documents
Boron 0.002–0.020
Calcium 0.001–0.003
2.1 ASTM Standards:
Copper 0.010–0.52
Magnesium 0.001–0.10 D1193 Specification for Reagent Water
This test method is under the jurisdiction of ASTM Committee E01 on
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct For referenced ASTM standards, visit the ASTM website, www.astm.org, or
responsibility of Subcommittee E01.08 on Ni and Co and HighTemperatureAlloys. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Current edition approved March 15, 2009. Published April 2009. DOI: 10.1520/ Standards volume information, refer to the standard’s Document Summary page on
E2594-09. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E2594 − 09
E50 Practices for Apparatus, Reagents, and Safety Consid- criteria. It is also expected that, when applicable, each labora-
erations for Chemical Analysis of Metals, Ores, and tory will participate in proficiency test programs, such as
Related Materials described in Practice E2027, and that the results from the
E55 Practice for Sampling Wrought Nonferrous Metals and participating laboratory will be satisfactory.
Alloys for Determination of Chemical Composition
E88 Practice for Sampling Nonferrous Metals and Alloys in 6. Interferences
Cast Form for Determination of Chemical Composition
6.1 Practice E1479 describes the typical interferences en-
E135 Terminology Relating to Analytical Chemistry for
countered during the inductively coupled plasma spectrometric
Metals, Ores, and Related Materials
analysis of metal alloys. The user is responsible for ensuring
E1329 Practice for Verification and Use of Control Charts in
the absence of or for compensating for interferences that may
Spectrochemical Analysis
bias test results obtained using their particular spectrometer.
E1479 Practice for Describing and Specifying Inductively-
6.2 The use of an internal standard may compensate for the
Coupled Plasma Atomic Emission Spectrometers
physical interferences resulting from differences between
E1601 Practice for Conducting an Interlaboratory Study to
sample and calibration solutions transport efficiencies.
Evaluate the Performance of an Analytical Method
E2027 Practice for Conducting Proficiency Tests in the
6.3 Shifts in background intensity levels because of, for
ChemicalAnalysis of Metals, Ores, and Related Materials
example, recombination effects or molecular band
contributions, or both, may be corrected by the use of an
2.2 ISO Standards:
ISO/IEC 17025 General Requirements for the Competence appropriate background correction technique. Direct spectral
overlaps are best addressed by selecting alternative wave-
of Calibration and Testing Laboratories
ISO Guide 31 ReferenceMaterials—ContentsofCertificates lengths. Spectral interference studies should be conducted on
all new matrices to determine the interference correction
and Labels
ISO Guide 34 General Requirements for the Competence of factor(s) that must be applied to concentrations obtained from
certain spectral line intensities to minimize biases. Some
Reference Material Producers
ISO Guide 98-3 Uncertainty of Measurement Part 3: Guide instrument manufacturers offer software options which math-
ematically correct for direct spectral overlaps, but the user is
to the Expression of Uncertainty in Measurement
(GUM:1995), First Edition cautioned to carefully evaluate this approach to spectral
correction.
3. Terminology
6.4 Modern instruments have software that allows compari-
3.1 Definitions—For definitions of terms used in this test
son of a sample spectrum to the spectrum obtained from a
method, refer to Terminology E135.
blank solution. The user of this test method must examine this
information to ascertain the need for background correction
4. Summary of Test Method
and the correct placement of background points.
4.1 Samples are dissolved in a mixture of mineral acids and
6.5 Table 1 suggests wavelengths that the user may use for
the resulting solutions are measured using inductively coupled
analysis of nickel alloys. Each line was used by at least one
plasma atomic emission spectrometry.
laboratory during the interlaboratory phase of test method
development and provided statistically valid results. Informa-
5. Significance and Use
tion for the suggested analytical wavelengths was collected
5.1 This test method for the chemical analysis of nickel
fromeachlaboratoryandhasbeenconvertedtowavelengthsas
alloysisprimarilyintendedtotestmaterialforcompliancewith
annotated in the National Institute of Standards and Technol-
specifications such as those under jurisdiction of ASTM
ogy (NIST) Atomic Spectra Database. In this database,
Committee B02. It may also be used to test compliance with
wavelengths of less than 200 nm were measured in vacuum
other specifications that are compatible with the test method.
and wavelengths greater than or equal to 200 nm were mea-
sured in air. Software tables for individual instruments may list
5.2 It is assumed that all who use this test method will be
wavelengths somewhat differently, as instrument optical path
trained analysts capable of performing common laboratory
atmospheric conditions may vary.
procedures skillfully and safely, and that the work will be
performed in a properly equipped laboratory.
6.6 Information on potential spectral interfering elements
was provided by the laboratories participating in the interlabo-
5.3 Thisisaperformance-basedtestmethodthatreliesmore
ratory study and may have originated from sources such as
on the demonstrated quality of the test result than on strict
recognized wavelength reference tables, instrument manufac-
adherence to specific procedural steps. It is expected that
turer’s software wavelength tables, or an individual laborato-
laboratories using this test method will prepare their own work
ry’s wavelength research studies, or combinations thereof.
instructions. These work instructions will include detailed
operating instructions for the specific laboratory, the specific
reference materials employed, and performance acceptance
Ralchenko, Yu, Kramida,A. E., Reader, J., and NISTASD Team (2008). NIST
Atomic Spectra Database (version 3.1.5), National Institute of Standards and
Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St., Technology,Gaithersburg,MD.Availableonline:http://physics.nist.gov/asd3[2008,
4th Floor, New York, NY 10036, http://www.ansi.org. October 28].
E2594 − 09
TABLE 1 Suggested Wavelengths/Interferences
Suitability of a specific instrument for testing to this test
Wavelength method will be established using the performance criteria
Element Potential Interference
(nm)
described in 12.1. The sample introduction system shall be
Aluminum 396.152
capable of handling solutions containing up to 5 % HF.
Aluminum 394.401 Nickel
Aluminum 237.312
7.2 Sample Preparation Equipment—Machine tools capable
Aluminum 176.638
of removing surface oxides and other contamination from the
Aluminum 167.079
as-received sample shall be used to produce chips or millings
Boron 182.641 Molybdenum, Cobalt, Chromium
Boron 182.591 Molybdenum, Cobalt, Chromium
for analysis.
Boron 136.246 Cobalt
Calcium 396.847
8. Reagents and Materials
Calcium 393.366 Cobalt
Copper 327.396 Titanium, Niobium, Gadolinium
8.1 Reagents:
Copper 224.700 Molybdenum, Iron
8.1.1 Purity of Reagents—Reagent grade chemicals shall be
Copper 219.958 Tantalum
used in all tests. Unless otherwise indicated, it is intended that
Copper 218.172
Copper 217.894
all reagents conform to the specifications of the Committee on
Copper 213.598
Analytical Reagents of the American Chemical Society where
Magnesium 383.829
such specifications are available. Other grades may be used,
Magnesium 280.270 Cobalt
Magnesium 279.553
provided it is first ascertained that the reagent is of sufficiently
Manganese 283.930
high purity to permit its use without lessening the accuracy of
Manganese 257.610 Cerium, Cobalt, Tungsten
the determination.
Niobium 319.498
Niobium 309.418 Chromium, Vanadium
8.1.2 Purity of Water—Unless otherwise indicated, refer-
Niobium 294.154 Vanadium
ences to water shall be understood to mean reagent water as
Niobium 269.706
defined by Type II of Specification D1193. The water purifi-
Niobium 210.942
Phosphorous 178.766
cation method used must be capable of removal of all elements
Phosphorous 178.284 Cobalt
in concentrations that might bias the test results.
Phosphorous 177.495 Nickel, Copper
8.1.3 Internal Standard—The use of an internal standard is
Tantalum 263.558 Molybdenum
Tantalum 240.063 Cobalt, Chromium, Vanadium
optional. However, the use of an internal standard may
Tantalum 226.230
compensate for the physical interferences resulting from dif-
Tin 189.991 Titanium
ferences in sample and calibration solutions transport effi-
Tin 175.800
Tin 140.052
ciency.
Titanium 350.489
Titanium 338.376 8.2 Calibration Solutions:
Titanium 337.280 Niobium
8.2.1 In this test method, calibration is based on laboratory-
Titanium 323.228
prepared, alloy matrix-matched calibration solutions. Alloy
Titanium 321.827
Tungsten 207.912
matrix-matched calibration solutions are solutions that contain
Tungsten 202.999
the approximate amounts of the major alloying elements
Vanadium 437.924
nickel, chromium, cobalt, molybdenum, and iron found in
Vanadium 375.087
Vanadium 309.311 typical sample solutions. They are intended to model the
Vanadium 292.464
physical behavior of sample solutions in the plasma. The
Vanadium 292.402
matrix solutions are prepared with starting materials of known
Zirconium 357.247
Zirconium 343.823 Niobium purity and are then spiked with aliquots of single element
Zirconium 327.305 Chromium, Europium
certified reference material (CRM) solutions that contain the
Zirconium 256.887
analytes to be quantified. The CRMs shall be compliant with
ISO Guide 31 and ISO Guide 34. It may be possible to analyze
different alloys using common matrix-matched calibration
solutions provided method validation studies demonstrate ac-
6.7 The user must verify that the selected wavelength
ceptable data.
performs acceptably in their lab, preferably during method
8.2.2 Steps 8.2.3 and following describe the preparation of
validation (see Section 15). The user also may choose to use
alloy matrix-matched calibration solutions for analysis of
multiple wavelengths to help verify that line selection is
sample solutions that contain 1 g alloy/100 mLfinal dilution. It
optimized for the particular alloy being determined. It is
is acceptable to vary the sample weight and final volume as
recommended that when wavelengths and appropriate spectral
corrections are determined, the user of this test method should long as the user’s method demonstrates adequate sensitivity
and precision (see 12.1).
specify this information or reference instrument programs that
include this information in their laboratory analysis proce- 8.2.3 Calculate the nominal amounts of the alloying metals
nickel, chromium, cobalt, molybdenum, and iron in 1 g of the
dures.
7. Apparatus 5
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC, www.chemistry.org. For suggestions on the
7.1 Inductively Coupled Plasma Atomic Emission
testing of reagents not listed by the American Chemical Society, see the United
Spectrometers—Used to perform analysis by this test method
States Pharmacopeia and National Formulary, U.S. Pharmacopeial Convention,
may conform to the specifications given in Practice E1479. Inc. (USPC), Rockville, MD, http://www.usp.org.
E2594 − 09
alloy to be analyzed. Use a source of each metal that contains 8.2.7.
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