ASTM E2823-17
(Test Method)Standard Test Method for Analysis of Nickel Alloys by Inductively Coupled Plasma Mass Spectrometry (Performance-Based)
Standard Test Method for Analysis of Nickel Alloys by Inductively Coupled Plasma Mass Spectrometry (Performance-Based)
SIGNIFICANCE AND USE
5.1 This test method for the chemical analysis of nickel and 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.
5.2 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.
5.3 This is a performance-based 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 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 E2027, and that the results from the participating laboratory will be satisfactory.
SCOPE
1.1 This test method describes the inductively coupled plasma mass spectrometric analysis of nickel and nickel allys, as specified by Committee B02, and having chemical compositions within the following limits:
Element
Application Range (Mass Fraction %)
Aluminum
0. 01–6.00
Boron
0. 01–0.10
Carbon
0. 01–0.15
Chromium
0. 01–33.00
Copper
0.01–35.00
Cobalt
0. 01–20.00
Iron
0.05–50.00
Magnesium
0. 01–0.020
Molybdenum
0. 01–30.0
Niobium
0. 01–6.0
Nickel
25.00–100.0
Phosphorous
0.001–0.025
Silicon
0.01–1.50
Sulfur
0.0001–0.01
Titanium
0.0001–6.0
Tungsten
0.01–5.0
Vanadium
0.0005–1.0
1.2 The following elements may be determined using this method.
Element
Quantification Range (μg/g)
Antimony
0.5–50
Bismuth
0.1–11
Gallium
2.9–54
Lead
0.4–21
Silver
1–35
Tin
2.2–97
Thallium
0.5–3.0
1.3 This method has only been interlaboratory tested for the elements and ranges specified. It may be possible to extend this method to other elements or different composition ranges provided that method validation that includes evaluation of method sensitivity, precision, and bias as described in this document is performed. Additionally, the validation study must evaluate the acceptability of sample preparation methodology using reference materials and/or spike recoveries. The user is cautioned to carefully evaluate the validation data as to the intended purpose of the analytical results. Guide E2857 provides additional guidance on method validation.
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. Specific safety hazard statements are given in Section 9.
General Information
- Status
- Published
- Publication Date
- 31-Dec-2016
- Technical Committee
- E01 - Analytical Chemistry for Metals, Ores, and Related Materials
- Drafting Committee
- E01.08 - Ni and Co and High Temperature Alloys
Relations
- Effective Date
- 01-Jan-2017
- Effective Date
- 01-Jan-2020
- Effective Date
- 01-Nov-2019
- Effective Date
- 01-Oct-2019
- Effective Date
- 15-May-2019
- Effective Date
- 15-Nov-2017
- Effective Date
- 01-Sep-2017
- Effective Date
- 01-Sep-2017
- Effective Date
- 01-Nov-2016
- Effective Date
- 01-Aug-2016
- Effective Date
- 15-May-2016
- Effective Date
- 01-Jul-2015
- Effective Date
- 15-May-2015
- Effective Date
- 15-Feb-2015
- Effective Date
- 15-Aug-2014
Overview
ASTM E2823-17 is the internationally recognized standard test method for the chemical analysis of nickel and nickel alloys using Inductively Coupled Plasma Mass Spectrometry (ICP-MS). Developed by ASTM International, this performance-based method is vital for verifying alloy composition and compliance with relevant specifications, such as those under ASTM Committee B02. The standard provides guidance for laboratories on setting up analytic protocols, validating results, and achieving a high level of accuracy and reliability when determining the concentration of major and trace elements in nickel alloys.
Key Topics
- Performance-Based Testing: This method emphasizes the performance and quality of the analytic outcome over strict procedural steps. Laboratories are responsible for developing internal work instructions tailored to their specific equipment, reference materials, and quality criteria.
- Material Compliance: Primarily used to confirm that nickel and nickel alloys meet material specifications, especially those defined by ASTM Committee B02.
- Element Coverage: The method applies to a wide range of elements and concentration levels. Major elements include aluminum, boron, carbon, chromium, copper, cobalt, iron, magnesium, molybdenum, niobium, nickel, phosphorus, silicon, sulfur, titanium, tungsten, and vanadium. Trace elements such as antimony, bismuth, gallium, lead, silver, tin, and thallium can also be quantified.
- Laboratory Requirements: Users of ASTM E2823-17 must be skilled analytical chemists operating in properly equipped laboratories. Safety and regulatory compliance are emphasized, especially when handling hazardous substances like hydrofluoric acid.
- Method Validation & Quality Control: Method validation, including sensitivity, precision, and bias studies, is required for both standard and extended applications of the method. Ongoing proficiency testing is recommended to ensure continued measurement reliability.
Applications
Adoption of ASTM E2823-17 brings consistency, precision, and trust to the chemical analysis of nickel alloys in a variety of industries, including:
- Aerospace and Automotive: Accurate elemental analysis is crucial for ensuring that high-performance components meet critical safety and regulatory standards.
- Manufacturing and Metallurgy: Quality control in the production of nickel alloy materials relies on precise confirmation of both major and trace element content.
- Research and Development: Laboratories developing new alloy compositions depend on reliable analytical data to optimize properties for specialized applications.
- Compliance Testing: Conformance with international and customer material specifications is validated through the standardized use of ICP-MS as outlined in this method.
The flexibility of this performance-based test method also allows for method extension to elements and concentration ranges beyond those explicitly covered, provided that sufficient method validation is performed.
Related Standards
Several standards and guides are referenced within ASTM E2823-17 to ensure best practices and analytic consistency, including:
- ASTM D1193: Specification for Reagent Water quality.
- ASTM E29: Guidelines for rounding and reporting significant digits in test data.
- ASTM E50, E55, E88: Practices for sampling and laboratory safety in the analysis of metals and alloys.
- ASTM E691, E1329: Procedures for conducting interlaboratory studies and using control charts for data quality.
- ASTM E177, E1601: Use of precision, bias, and interlaboratory performance evaluation.
- ASTM E2027: Conducting proficiency tests in metals analysis.
- ASTM E2857: Method validation requirements for analytical testing.
- ISO/IEC 17025: General requirements for competence of testing and calibration laboratories.
- ISO Guides 31, 34, 98-3: Certification and quality guidance for reference materials and measurement uncertainty.
Integrating ASTM E2823-17 into laboratory procedures ensures global alignment and technical excellence in nickel alloy analysis using ICP-MS, supporting high standards of quality, safety, and reliability across industries.
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Frequently Asked Questions
ASTM E2823-17 is a standard published by ASTM International. Its full title is "Standard Test Method for Analysis of Nickel Alloys by Inductively Coupled Plasma Mass Spectrometry (Performance-Based)". This standard covers: SIGNIFICANCE AND USE 5.1 This test method for the chemical analysis of nickel and 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. 5.2 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. 5.3 This is a performance-based 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 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 E2027, and that the results from the participating laboratory will be satisfactory. SCOPE 1.1 This test method describes the inductively coupled plasma mass spectrometric analysis of nickel and nickel allys, as specified by Committee B02, and having chemical compositions within the following limits: Element Application Range (Mass Fraction %) Aluminum 0. 01–6.00 Boron 0. 01–0.10 Carbon 0. 01–0.15 Chromium 0. 01–33.00 Copper 0.01–35.00 Cobalt 0. 01–20.00 Iron 0.05–50.00 Magnesium 0. 01–0.020 Molybdenum 0. 01–30.0 Niobium 0. 01–6.0 Nickel 25.00–100.0 Phosphorous 0.001–0.025 Silicon 0.01–1.50 Sulfur 0.0001–0.01 Titanium 0.0001–6.0 Tungsten 0.01–5.0 Vanadium 0.0005–1.0 1.2 The following elements may be determined using this method. Element Quantification Range (μg/g) Antimony 0.5–50 Bismuth 0.1–11 Gallium 2.9–54 Lead 0.4–21 Silver 1–35 Tin 2.2–97 Thallium 0.5–3.0 1.3 This method has only been interlaboratory tested for the elements and ranges specified. It may be possible to extend this method to other elements or different composition ranges provided that method validation that includes evaluation of method sensitivity, precision, and bias as described in this document is performed. Additionally, the validation study must evaluate the acceptability of sample preparation methodology using reference materials and/or spike recoveries. The user is cautioned to carefully evaluate the validation data as to the intended purpose of the analytical results. Guide E2857 provides additional guidance on method validation. 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. Specific safety hazard statements are given in Section 9.
SIGNIFICANCE AND USE 5.1 This test method for the chemical analysis of nickel and 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. 5.2 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. 5.3 This is a performance-based 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 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 E2027, and that the results from the participating laboratory will be satisfactory. SCOPE 1.1 This test method describes the inductively coupled plasma mass spectrometric analysis of nickel and nickel allys, as specified by Committee B02, and having chemical compositions within the following limits: Element Application Range (Mass Fraction %) Aluminum 0. 01–6.00 Boron 0. 01–0.10 Carbon 0. 01–0.15 Chromium 0. 01–33.00 Copper 0.01–35.00 Cobalt 0. 01–20.00 Iron 0.05–50.00 Magnesium 0. 01–0.020 Molybdenum 0. 01–30.0 Niobium 0. 01–6.0 Nickel 25.00–100.0 Phosphorous 0.001–0.025 Silicon 0.01–1.50 Sulfur 0.0001–0.01 Titanium 0.0001–6.0 Tungsten 0.01–5.0 Vanadium 0.0005–1.0 1.2 The following elements may be determined using this method. Element Quantification Range (μg/g) Antimony 0.5–50 Bismuth 0.1–11 Gallium 2.9–54 Lead 0.4–21 Silver 1–35 Tin 2.2–97 Thallium 0.5–3.0 1.3 This method has only been interlaboratory tested for the elements and ranges specified. It may be possible to extend this method to other elements or different composition ranges provided that method validation that includes evaluation of method sensitivity, precision, and bias as described in this document is performed. Additionally, the validation study must evaluate the acceptability of sample preparation methodology using reference materials and/or spike recoveries. The user is cautioned to carefully evaluate the validation data as to the intended purpose of the analytical results. Guide E2857 provides additional guidance on method validation. 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. Specific safety hazard statements are given in Section 9.
ASTM E2823-17 is classified under the following ICS (International Classification for Standards) categories: 77.040.30 - Chemical analysis of metals; 77.120.40 - Nickel, chromium and their alloys. The ICS classification helps identify the subject area and facilitates finding related standards.
ASTM E2823-17 has the following relationships with other standards: It is inter standard links to ASTM E2823-11, ASTM E135-20, ASTM E1601-19, ASTM E2972-15(2019), ASTM E135-19, ASTM E2027-17, ASTM E88-11(2017), ASTM E50-17, ASTM E1479-16, ASTM E50-11(2016), ASTM E135-16, ASTM E135-15a, ASTM E135-15, ASTM E2972-15, ASTM E135-14b. Understanding these relationships helps ensure you are using the most current and applicable version of the standard.
ASTM E2823-17 is available in PDF format for immediate download after purchase. The document can be added to your cart and obtained through the secure checkout process. Digital delivery ensures instant access to the complete standard document.
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: E2823 − 17
Standard Test Method for
Analysis of Nickel Alloys by Inductively Coupled Plasma
Mass Spectrometry (Performance-Based)
This standard is issued under the fixed designation E2823; 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 using reference materials and/or spike recoveries. The user is
cautioned to carefully evaluate the validation data as to the
1.1 This test method describes the inductively coupled
intended purpose of the analytical results. Guide E2857 pro-
plasma mass spectrometric analysis of nickel and nickel allys,
vides additional guidance on method validation.
as specified by Committee B02, and having chemical compo-
1.4 This standard does not purport to address all of the
sitions within the following limits:
safety concerns, if any, associated with its use. It is the
Element Application Range (Mass
Fraction %) responsibility of the user of this standard to establish appro-
Aluminum 0. 01–6.00
priate safety and health practices and determine the applica-
Boron 0. 01–0.10
bility of regulatory limitations prior to use. Specific safety
Carbon 0. 01–0.15
Chromium 0. 01–33.00 hazard statements are given in Section 9.
Copper 0.01–35.00
Cobalt 0. 01–20.00
2. Referenced Documents
Iron 0.05–50.00
Magnesium 0. 01–0.020 2
2.1 ASTM Standards:
Molybdenum 0. 01–30.0
D1193 Specification for Reagent Water
Niobium 0. 01–6.0
Nickel 25.00–100.0
E29 Practice for Using Significant Digits in Test Data to
Phosphorous 0.001–0.025
Determine Conformance with Specifications
Silicon 0.01–1.50
E50 Practices for Apparatus, Reagents, and Safety Consid-
Sulfur 0.0001–0.01
Titanium 0.0001–6.0
erations for Chemical Analysis of Metals, Ores, and
Tungsten 0.01–5.0
Related Materials
Vanadium 0.0005–1.0
E55 Practice for Sampling Wrought Nonferrous Metals and
1.2 The following elements may be determined using this
Alloys for Determination of Chemical Composition
method.
E88 Practice for Sampling Nonferrous Metals andAlloys in
Element Quantification Range (µg/g)
Cast Form for Determination of Chemical Composition
Antimony 0.5–50
E135 Terminology Relating to Analytical Chemistry for
Bismuth 0.1–11
Gallium 2.9–54 Metals, Ores, and Related Materials
Lead 0.4–21
E177 Practice for Use of the Terms Precision and Bias in
Silver 1–35
ASTM Test Methods
Tin 2.2–97
Thallium 0.5–3.0 E691 Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method
1.3 This method has only been interlaboratory tested for the
E1329 Practice for Verification and Use of Control Charts in
elementsandrangesspecified.Itmaybepossibletoextendthis
Spectrochemical Analysis
method to other elements or different composition ranges
E1479 Practice for Describing and Specifying Inductively
provided that method validation that includes evaluation of
Coupled Plasma Atomic Emission Spectrometers
method sensitivity, precision, and bias as described in this
E1601 Practice for Conducting an Interlaboratory Study to
documentisperformed.Additionally,thevalidationstudymust
Evaluate the Performance of an Analytical Method
evaluate the acceptability of sample preparation methodology
E2027 Practice for Conducting Proficiency Tests in the
ChemicalAnalysis of Metals, Ores, and Related Materials
This test method is under the jurisdiction of ASTM Committee E01 on
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct
responsibility of Subcommittee E01.08 on Ni and Co and HighTemperatureAlloys. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Jan. 1, 2017. Published February 2017. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 2011. Last previous edition approved in 2011 as E2823–11. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/E2823-17. the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E2823 − 17
E2165 Practice for Establishing an Uncertainty Budget for 6.2 The use of an internal standard may compensate for the
the Chemical Analysis of Metals, Ores, and Related physical interferences resulting from variations in sample and
Materials (Withdrawn 2007) calibrationsolutionaerosoltransportrates.Theusermaychose
E2857 Guide for Validating Analytical Methods to add the internal standard by spiking each solution with a
E2972 Guide for Production, Testing, and ValueAssignment specified amount of an appropriate certified reference material
of In-House Reference Materials for Metals, Ores, and (CRM) solution.Alternatively, on-line addition of a peripheral
Other Related Materials internal standard solution during sample analysis is also
possible provided acceptable instrument sensitivity is main-
2.2 ISO Standards:
tained.
ISO/IEC 17025 General Requirements for the Competence
of Calibration and Testing Laboratories
6.3 Isobaric and polyatomic mass overlap interferences are
ISO Guide 98-3 Uncertainty of Measurement—Part 3:
best addressed by selecting an alternate atomic mass. Some
Guide to the Expression of Uncertainty in Measurement
instrument manufacturers offer software options for math-
(GUM:1995), First Edition
ematically correcting for common interferences, but the user is
cautioned to carefully evaluate this approach to mass overlap
3. Terminology
correction. However, some laboratories participating in the
interlaboratory study found it necessary to generate a math-
3.1 Definitions—For definitions of terms used in this test
method, refer to Terminology E135. ematical correction for the effect of the ZrO interference on the
Ag 107 isotope. In this case the Zr 91 isotope was used for
4. Summary of Test Method
zirconium determination.
4.1 Samples are dissolved in a mixture of mineral acids and
6.4 Modern instruments may have a collision or reaction
the resulting solutions are measured using inductively coupled
cell that can use ion-molecule collisions or reactions to remove
plasma mass spectrometry.
spectral interferences. The user of this method must examine
this information to ascertain the need for collision/reaction
5. Significance and Use
cells for the removal of spectral interferences. However, it
5.1 This test method for the chemical analysis of nickel and should be noted that no collision/reaction gases were used by
the laboratories participating in the interlaboratory study of the
nickel alloys is primarily intended to test material for compli-
ance with specifications such as those under jurisdiction of elements listed in the Scope, thus implying that the use of
collision/reaction gases is not required for determination of
ASTM committee B02. It may also be used to test compliance
with other specifications that are compatible with the test those elements.
method.
6.5 The isotopes listed in Table 1 have been used to analyze
5.2 Itisassumedthatallwhousethismethodwillbetrained the listed elements in nickel alloys and are suggested for the
user. The user may choose to use multiple isotopes to help
analysts capable of performing common laboratory procedures
skillfully and safely, and that the work will be performed in a verifythatatomicmassselectionisoptimizedfortheparticular
alloy being determined. It is recommended that once isotopes
properly equipped laboratory.
and appropriate spectral corrections are determined, the user of
5.3 This is a performance-based method that relies more on
this method specify this information or reference instrument
the demonstrated quality of the test result than on strict
programs, which include this information in their laboratory
adherence to specific procedural steps. It is expected that
analysis procedures.
laboratories using this method will prepare their own work
instructions. These work instructions will include detailed
7. Apparatus
operating instructions for the specific laboratory, the specific
7.1 Suitability of an Inductively Coupled Plasma Mass
reference materials employed, and performance acceptance
Spectrometer for testing of this method will be established
criteria. It is also expected that, when applicable, each labora-
using the performance criteria described in section 12.1. The
tory will participate in proficiency test programs, such as
sample introduction system shall be capable of handling
described in Practice E2027, and that the results from the
solutions containing trace amounts of HF. Each instrument
participating laboratory will be satisfactory.
shall be installed and operated according to the manufacturer’s
recommendations.
6. Interferences
6.1 When possible, analyte isotopes are selected that are
free from mass overlap interferences. Because isotope choices
TABLE 1 Suggested Isotopes/Interference
are limited, this is not always an option. It is the responsibility
Potential
Element Isotope
Interference
of the user to determine run conditions and parameters that
Antimony 121
avoidorcompensateforinterferencesthatmaybiastestresults.
Bismuth 209
Gallium 71
Lead 208
The last approved version of this historical standard is referenced on
Silver 107 ZrO, FeCr
www.astm.org.
Tin 120 MoO
Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St., Thallium 205
4th Floor, New York, NY 10036, http://www.ansi.org.
E2823 − 17
7.2 Sample Preparation Equipment—Machine tools shall be expected sample concentrations, a concentration at or near the
used that are capable of removing surface oxides and other reporting limit, and a blank. In any case, a minimum of three
contamination from the as-received sample and then taking solutions including a blank must be used for calibration.
uncontaminated and chemically representative chips suitable
8.2.4 Prepare matrix solutions as follows:
for analysis.
8.2.4.1 Weigh 0.5 g of pure nickel into an HF resistant
digestionvessel.Useonevesselforeachcalibrationsolutionto
7.3 All labware used should be suitably cleaned for trace
bemade.Notethatusing0.5gofnickelapproximatesthemass
level analysis.
fraction of nickel (50 %) found in1gofa typical nickel alloy.
8. Reagents and Materials
8.2.4.2 Dissolve the pure nickel in 20 mL of acid mixture
per gram of sample. Select acid mixtures that will dissolve the
8.1 Reagents:
alloys to be analyzed using this method.
8.1.1 Purity of Reagents—Reagent grade chemicals shall be
Caution: If powdered nickel is used, add the acid cautiously
used in all tests. Unless otherwise indicated, it is intended that
as powdered metals tend to be very reactive.
all reagents conform to the specifications of the Committee on
8.2.4.3 A mixture of HCl + HNO (9 + 1), HCl + HO+
Analytical Reagents of the American Chemical Society where
3 2
such specifications are available. However, the purity of acid HNO (3 + 2 + 1), or HNO +HF+H O (1 + 1 + 1) will
3 3 2
dissolve many types of nickel alloys . For high Mo-Cr alloys it
reagents utilized in this procedure shall be suitable for trace
metalanalysisandshouldnotcontainanysignificantamountof has been found that concentrated HCl with the addition of
concentrated HNO dropwise may be necessary to avoid
the analyte. Other grades may be used, provided it is first
ascertained that the reagent is of sufficiently high purity to passivation.
permit its use without lessening the accuracy of the determi-
8.2.4.4 Heat the digestion vessels gently until the nickel
nation.
dissolves. Remove the beakers from the heat, add 10 drops of
8.1.2 Purity of Water—The purity of water used in this test 49 % HF, and swirl gently. If HNO +HF+HO(1+1+1)
3 2
method shall conform to the requirements of Specification
is used for digestion, it is not necessary to add additional HF.
D1193forreagentwater,TypeI.Thewaterpurificationmethod The laboratory may choose to reduce this solution to wet salts
used must be capable of removal of all elements in concentra-
in order to remove excess HF and then re-dissolve by heating
tions that might bias the test results.
the salts in approximately 20 mL of water.
8.1.3 Internal Standard—The use of an internal standard is
8.2.4.5 Ifaninternalstandardisused,addthepredetermined
recommended. The use of an internal standard may compen-
amount into each solution.
sate for the physical interferences resulting from variations in
8.2.4.6 Cool the nickel solutions and transfer into 1-L
sample and calibration solution aerosol transport rates. Select
plastic flasks. Polypropylene or polymethylpentene flasks are
an internal standard element of similar atomic mass to the
acceptable for this purpose.
analyte and one that is not commonly found in the samples to
8.2.5 Add the needed amount of single element CRM
be determined. The exact concentration added is not critical,
solutions to the flasks, ensuring to leave one analyte-free for
however, the amount added should yield a significant signal
use as a blank. Maintain the acidity necessary to assure
when measured.
solution stability. The acidity given on the solution CRM
8.2 Calibration Solutions:
certificate of analysis will provide guidance on the necessary
8.2.1 In this test method, calibration is based on laboratory- acid concentrations needed to do this. Typically, if these
prepared, pure nickel matrix- matched solutions. The matrix
solutions are to match samples prepared using one gram of
solutions are prepared with nickel of known purity. These alloy diluted to1-L, the quantity of acids used in 8.2.4 will be
matrixsolutionsarethenspikedwithaliquotsofsingleelement
sufficient to hold all analytes in solution.
certified reference material (CRM) solutions which contain the
8.3 Other Materials:
elements of interest.
8.3.1 Argon—The ICP-MS argon supply should be in accor-
8.2.2 Step 8.2.3 and following describe the preparation of
dance with the recommendations of the instrument manufac-
calibration solutions for analysis of sample solutions that
turer.
contain 1 g alloy/L final dilution. It is acceptable to vary final
8.3.2 Control Materials:
concentrations as long as the user’s method demonstrates
8.3.2.1 A laboratory may choose to procure, produce, or
adequate sensitivity and precision (see 12.1).
have manufactured a chip material containing analyte contents
8.2.3 Determine the number and composition of calibration
in the range of typical samples to be used as a control material.
solutions needed to cover the concentration range for each
These chips should be well blended and checked for homoge-
element. It is suggested that the calibration solutions have their
neity. Additional guidance on the production of these control
highest concentration slightly above the highest expected
materials may be found in Guide E2972.
sample concentration, a concentration in the mid-range of the
8.3.2.2 A laboratory may find it difficult to procure or have
manufactured the materials described in 8.3.2.1 for all of the
Reagent Chemicals, American Chemical Society Specifications, American
necessary analytes or alloys. If this is the case, then it is
Chemical Society, Washington, DC. https://.acs.pubs.org/reagents/index.html. For
acceptable to prepare equivalent reference material solutions
suggestions on the testing of reagents not listed by theAmerican Chemical Society,
usinganalternativesourceofnickelforthematrixsolutionand
see the United States Pharmacopeia and National Formulary, U.S. Pharmacopeial
Convention, Inc. (USPC), Rockville, MD, https://www.usp.org. spiked with different single element CRM solutions.
E2823 − 17
8.3.3 Collision/Reaction Gases—Collision and/or reaction 100s
% RSD 5 (1)
gases may be used to minimize the effects of isobaric and H
C
polyatomic mass interferences. Manufacturers typically will
where:
provide guidance upon the type and purity of collision and
s = estimated standard deviation, and
reaction gases to be used for a specific analyte.
¯
C = average of the 10 results obtained for the high calibra-
9. Hazards tion solution.
9.1 This method involves the use of HF. Read and follow
12.1.2.1 The calculated % RSD should be < 5.0 %. If it is
label precautions, SDS information, and refer to Practice E50.
not, the user of this method may not be able to meet the
For precautions to be observed in the use of certain other
performance criteria of the method. Some factors that may
reagents in this test method, refer to Practice E50.
affect precision for inductively coupled plasma emission spec-
trometers may also affect inductively coupled plasma mass
10. Sampling, Test Specimens, and Test Units
spectrometers. Practice E1479 provides limited guidance as to
10.1 Laboratories shall follow written practices for sam-
the parameters, which may have an effect on the precision
pling and preparation of test samples. These practices shall characteristics of both spectrometer types. Instrument trouble-
meet all customer requirements. Practices E55 and E88 also shooting manuals provided by the manufacturer of the equip-
provide guidance for sampling. ment may also provide guidance for optimizing performance
for the specific instrument being used.
10.2 Test specimens should be obtained by milling or
drilling chips that are clean and of sufficient quantity to fulfill
12.2 Calibration Procedure:
the sample mass required by the procedure.
12.2.1 Set up the instrument for calibration in a manner
consistent with the manufacturer’s recommendations.
11. Preparation of Apparatus
12.2.2 Specify calibration units consistent with the concen-
11.1 Analytical instrumentation and sample preparation
trations of the calibration solutions prepared in 8.2. The user
equipment shall be installed and operated in a manner consis-
maychoosetospecifyunitsintheICP-MSinstrumentsoftware
tent with manufacturer’s recommendations.
as a mass fraction such as % or mg/kg in order to simplify
calculation and reporting of final results.
12. Calibration
12.2.3 Define the number of replicate measurements to be
12.1 It will be necessary to establish that the instrument made and averaged for a single reported result. Typically, a
being used is capable of demonstrating acceptable sensitivity
minimum of 2 replicates is specified.
and precision for the elements being determined. Once it has
12.2.4 Calibrate the instrument using the calibration solu-
been demonstrated that the instrument has acceptable sensitiv-
tions. Calibration curves for ICP-MS are generally linear over
ity and precision for these elements, it will not be necessary to
several orders of magnitude. Typical calibration methods
routinely evaluate sensitivity and precision. Evaluate equip-
include calculation of a linear function using a calculated
ment sensitivity and precision as described in sections 12.1.1
intercept, calculation of a linear function while forcing the
and
...
This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
Designation: E2823 − 11 E2823 − 17
Standard Test Method for
Analysis of Nickel Alloys by Inductively Coupled Plasma
Mass Spectrometry (Performance-Based
Method)(Performance-Based)
This standard is issued under the fixed designation E2823; 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
1.1 This test method describes the inductively coupled plasma mass spectrometric analysis of nickel, nickel and nickel allys,
as specified by Committee B02, and having chemical compositions within the following limits:
Element Application Range (Wt. (Mass
Fraction %)
Aluminum 0. 01–6.00
Boron 0. 01–0.10
Carbon 0. 01–0.15
Chromium 0. 01–33.00
Copper 0.01–35.00
Cobalt 0. 01–20.00
Iron 0.05–50.00
Magnesium 0. 01–0.020
Molybdenum 0. 01–30.0
Niobium 0. 01–6.0
Nickel 25.00–100.0
Phosphorous 0.001–0.025
Silicon 0.01–1.50
Sulfur 0.0001–0.01
Titanium 0.0001–6.0
Tungsten 0.01–5.0
Vanadium 0.0005–1.0
1.2 The following elements may be determined using this method.
Element Quantification Range (μg/g)
Antimony 0.5–50
Bismuth 0.1–11
Gallium 2.9–54
Lead 0.4–21
Silver 1–35
Tin 2.2–97
Thallium 0.5–3.0
1.3 This method has only been interlaboratory tested for the elements and ranges specified. It may be possible to extend this
method to other elements or different composition ranges provided that method validation that includes evaluation of method
sensitivity, precision, and bias as described in this document is performed. Additionally, the validation study must evaluate the
acceptability of sample preparation methodology using reference materials and/or spike recoveries. The user is cautioned to
carefully evaluate the validation data as to the intended purpose of the analytical results. Guide E2857 provides additional guidance
on method validation.
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. Specific safety hazard statements are given in Section 9.
This test method is under the jurisdiction of ASTM Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials and is the direct responsibility of
Subcommittee E01.08 on Ni and Co and High Temperature Alloys.
Current edition approved May 1, 2011Jan. 1, 2017. Published July 2011February 2017. Originally approved in 2011. Last previous edition approved in 2011 as E2823–11.
DOI: 10.1520/E2823-11.10.1520/E2823-17.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E2823 − 17
2. Referenced Documents
2.1 ASTM Standards:
D1193 Specification for Reagent Water
E29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
E50 Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials
E55 Practice for Sampling Wrought Nonferrous Metals and Alloys for Determination of Chemical Composition
E88 Practice for Sampling Nonferrous Metals and Alloys in Cast Form for Determination of Chemical Composition
E135 Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
E177 Practice for Use of the Terms Precision and Bias in ASTM Test Methods
E691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method
E1329 Practice for Verification and Use of Control Charts in Spectrochemical Analysis
E1479 Practice for Describing and Specifying Inductively Coupled Plasma Atomic Emission Spectrometers
E1601 Practice for Conducting an Interlaboratory Study to Evaluate the Performance of an Analytical Method
E2027 Practice for Conducting Proficiency Tests in the Chemical Analysis of Metals, Ores, and Related Materials
E2165 Practice for Establishing an Uncertainty Budget for the Chemical Analysis of Metals, Ores, and Related Materials
(Withdrawn 2007)
E2857 Guide for Validating Analytical Methods
E2972 Guide for Production, Testing, and Value Assignment of In-House Reference Materials for Metals, Ores, and Other
Related Materials
2.2 ISO Standards:
ISOISO/IEC 17025 General Requirements for the Competence of Calibration and Testing Laboratories
ISO Guide 31 Contents of Certificates of Reference Materials
ISO Guide 34 Quality System Guidelines for the Production of Reference Materials
ISO Guide 98-3 Uncertainty of Measurement—Part 3: Guide to the Expression of Uncertainty in Measurement (GUM:1995),
First Edition
3. Terminology
3.1 Definitions—For definitions of terms used in this test method, refer to Terminology E135.
4. Summary of Test Method
4.1 Samples are dissolved in a mixture of mineral acids and the resulting solutions are measured using inductively coupled
plasma mass spectrometry.
5. Significance and Use
5.1 This test method for the chemical analysis of nickel and 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.
5.2 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.
5.3 This is a performance-based 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 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 E2027, and that the results from the participating laboratory will be satisfactory.
6. Interferences
6.1 When possible, analyte isotopes are selected, whichselected that are free from mass overlap interferences. Because isotope
choices are limited, this is not always an option. It is the responsibility of the user to determine run conditions and parameters that
avoid or compensate for interferences that may bias test results.
6.2 The use of an internal standard may compensate for the physical interferences resulting from variations in sample and
calibration solution aerosol transport rates. The user may chose to add the internal standard by spiking each solution with a
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 ASTM website.
The last approved version of this historical standard is referenced on www.astm.org.
Available from American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http://www.ansi.org.
E2823 − 17
specified amount of an appropriate certified reference material (CRM) solution. Alternatively, on-line addition of a peripheral
internal standard solution during sample analysis is also possible provided acceptable instrument sensitivity is maintained.
6.3 Isobaric and polyatomic mass overlap interferences are best addressed by selecting an alternate atomic mass. Some
instrument manufacturers offer software options for mathematically correcting for common interferences, but the user is cautioned
to carefully evaluate this approach to mass overlap correction. However, some laboratories participating in the interlaboratory
study found it necessary to generate a mathematical correction for the effect of the ZrO interference on the Ag 107 isotope. In this
case the Zr 91 isotope was used for zirconium determination.
6.4 Modern instruments may have a collision or reaction cell whichthat can use ion-molecule collisions or reactions to remove
spectral interferences. The user of this method must examine this information to ascertain the need for collision/reaction cells for
the removal of spectral interferences. However, it should be noted that no collision/reaction gases were used by the laboratories
participating in the interlaboratory study of the elements listed in the Scope, thus implying that the use of collision/reaction gases
is not required for determination of those elements.
6.5 The isotopes listed in Table 1 have been used to analyze the listed elements in nickel alloys and are suggested for the user.
The user may choose to use multiple isotopes to help verify that atomic mass selection is optimized for the particular alloy being
determined. It is recommended that once isotopes and appropriate spectral corrections are determined, the user of this method
specify this information or reference instrument programs, which include this information in their laboratory analysis procedures.
7. Apparatus
7.1 Suitability of an Inductively Coupled Plasma Mass Spectrometer for testing of this method will be established using the
performance criteria described in section 12.1. The sample introduction system shall be capable of handling solutions containing
trace amounts of HF. Each instrument shall be installed and operated according to the manufacturer’s recommendations.
7.2 Sample Preparation Equipment—Machine tools shall be used that are capable of removing surface oxides and other
contamination from the as-received sample and then taking uncontaminated and chemically representative chips suitable for
analysis.
7.3 All labware used should be suitably cleaned for trace level analysis.
8. Reagents and Materials
8.1 Reagents:
8.1.1 Purity of Reagents—Reagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that all
reagents conform to the specifications of the Committee on Analytical Reagents of the American Chemical Society where such
specifications are available. However, the purity of acid reagents utilized in this procedure shall be suitable for trace metal analysis
and should not contain impurities in any significant amount. amount of the analyte. Other grades may be used, provided it is first
ascertained that the reagent is of sufficiently high purity to permit its use without lessening the accuracy of the determination.
8.1.2 Reagent Purity of Water—The purity of reagent water water used in this test method shall conform to the requirements
of Specification D1193 for reagent water, Type I. The water purification method used must be capable of removal of all elements
in concentrations that might bias the test results.
8.1.3 Internal Standard—The use of an internal standard is recommended. The use of an internal standard may compensate for
the physical interferences resulting from variations in sample and calibration solution aerosol transport rates. Select an internal
standard element of similar atomic mass to the analyte and one that is not commonly found in the samples to be determined. The
exact concentration added is not critical, however, the amount added should yield a significant signal when measured.
8.2 Calibration Solutions:
Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. https://.acs.pubs.org/reagents/index.html. For suggestions
on the testing of reagents not listed by the American Chemical Society, see the United States Pharmacopeia and National Formulary, U.S. Pharmacopeial Convention, Inc.
(USPC), Rockville, MD, https://www.usp.org.
TABLE 1 Suggested Isotopes/Interference
Potential
Element Isotope
Interference
Antimony 121
Bismuth 209
Gallium 71
Lead 208
Silver 107 ZrO, FeCr
Tin 120 MoO
Thallium 205
E2823 − 17
8.2.1 In this test method, calibration is based on laboratory-prepared, pure nickel matrix- matched solutions. The matrix
solutions are prepared with nickel of known purity. These matrix solutions are then spiked with aliquots of single element certified
reference material (CRM) solutions which contain the elements of interest. The CRMs shall be compliant with ISO Guides 31 and
34.
8.2.2 Step 8.2.3 and following describe the preparation of calibration solutions for analysis of sample solutions that contain 1
g alloy/L final dilution. It is acceptable to vary final concentrations as long as the user’s method demonstrates adequate sensitivity
and precision (see section 12.1).
8.2.3 Determine the number and composition of calibration solutions needed to cover the concentration range for each element.
It is suggested that the calibration solutions have their highest concentration slightly above the highest expected sample
concentration, a concentration in the mid range mid-range of the expected sample concentrations, a concentration at or near the
reporting limit, and a blank. In any case, a minimum of three solutions including a blank must be used for calibration.
8.2.4 Prepare matrix solutions as follows:
8.2.4.1 Weigh 0.5 g of pure nickel into an HF resistant digestion vessel. Use one vessel for each calibration solution to be made.
Note that using 0.5 g of nickel approximates the mass fraction of nickel (50 %) found in 1 g of a typical nickel alloy.
8.2.4.2 Dissolve the pure nickel in 20 mL of acid mixture per gram of sample. Select acid mixtures that will dissolve the alloys
to be analyzed using this method.
NOTE 1—Caution: If powdered nickel is used, add the acid cautiously as powdered metals tend to be very reactive.
Caution: If powdered nickel is used, add the acid cautiously as powdered metals tend to be very reactive.
8.2.4.3 A mixture of HCl + HNO (9 + 1), HCl + H O + HNO (3 + 2 + 1), or HNO + HF + H O (1 + 1 + 1) will dissolve
3 2 3 3 2
many types of nickel alloys . For high Mo-Cr alloys it has been found that concentrated HCl with the addition of concentrated
HNO dropwise may be necessary to avoid passivation.
8.2.4.4 Heat the digestion vessels gently until the nickel dissolves. Remove the beakers from the heat, add 10 drops of 49 %
HF, and swirl gently. If HNO + HF + H O (1 + 1 + 1) is used for digestion, it is not necessary to add additional HF. The laboratory
3 2
may choose to reduce this solution to wet salts in order to remove excess HF and then re-dissolve by heating the salts in
approximately 20 mL of water.
8.2.4.5 If an internal standard is to be used, add the predetermined amount into each solution.
8.2.4.6 Cool the nickel solutions and transfer into 1-L plastic flasks. Polypropylene or polymethylpentene flasks are acceptable
for this purpose.
8.2.5 Add the needed amount of single element CRM solutions intoto the flasks, making sure ensuring to leave one analyte-free
for use as a blank. Maintain the acidity necessary to assure solution stability. The acidity given on the solution CRM certificate
of analysis will provide guidance on the necessary acid concentrations needed to do this. Typically, if these solutions are to match
samples prepared using one gram of alloy diluted to1-L, the quantity of acids used in 8.2.4 will be sufficient to hold all analytes
in solution.
8.3 Other Materials:
8.3.1 Argon and Collision/Reaction Gases—Argon—The ICPICP-MS argon supply and any collision/reaction gas supply shall
be specified by the should be in accordance with the recommendations of the instrument manufacturer.
8.3.2 Control Materials:
8.3.2.1 A laboratory may choose to procure, produce, or have manufactured a chip material containing analyte contents in the
range of typical samples to be used as a control material. These chips should be well blended and checked for homogeneity.
Additional guidance on the production of these control materials may be found in Guide E2972.
8.3.2.2 A laboratory may find it difficult to procure or have manufactured the materials described in 8.3.2.1 for all of the
necessary analytes or alloys. If this is the case, then it is acceptable to prepare equivalent reference material solutions using an
alternative source of nickel for the matrix solution and spiked with different single element CRM solutions.
8.3.3 Collision/Reaction Gases—Collision and/or reaction gases may be used to minimize the effects of isobaric and polyatomic
mass interferences. Manufacturers typically will provide guidance upon the type and purity of collision and reaction gases to be
used for a specific analyte.
9. Hazards
9.1 This method involves the use of concentrated HF. Read and follow label precautions, MSDSSDS information, and refer to
Practice E50. For precautions to be observed in the use of certain other reagents in this test method, refer to Practice E50.
10. Sampling, Test Specimens, and Test Units
10.1 Laboratories shall follow written practices for sampling and preparation of test samples. These practices shall meet all
customer requirements. Practices E55 and E88 also provide guidance for sampling.
10.2 Test specimens should be obtained by milling or drilling chips that are clean and of sufficient quantity to fulfill the sample
weightmass required by the procedure.
E2823 − 17
11. Preparation of Apparatus
11.1 Analytical instrumentation and sample preparation equipment shall be installed and operated in a manner consistent with
manufacturer’s recommendations.
12. Calibration
12.1 It will be necessary to establish that the instrument being used is capable of demonstrating acceptable sensitivity and
precision for the elements being determined. Once it has been demonstrated that the instrument has acceptable sensitivity and
precision for these elements, it will not be necessary to routinely evaluate sensitivity and precision. Evaluate equipment sensitivity
and precision as described in sections 12.1.1 and 12.1.2.
12.1.1 Sensitivity—Sensitivity shall be evaluated by first establishing a calibration curve for each element being determined
using calibration solutions prepared as described in section 8.2. At a minimum the calibration curve will contain two points. After
thorough rinsing, the blank solution is analyzed 10 times. Calculate 3 times the standard deviation of this determination as an
approximation of the limit of detection limit. Calculate 10 times the standard deviation to approximate the limit of quantification.
If the instrument/parameter selection of the user does not produce an estimated detection limit of detection equal to or better than
the lower scope limit of the method for the element(s) being determined, then it is probable the method user will be unable to meet
the method’s lower scope limit. If the instrument/parameter selection of the user does not produce a limit of quantification equal
to or better than the lower scope limit of the method for the element(s) being determined, then it is possible the method user will
be unable to consistently meet the method’s lower scope limit.
12.1.2 Precision—The short-term precision shall be determined as follows. Using the same calibration generated above,in
12.1.1, analyze the high calibration solution 10 times using the instrument/parameters selected by the method user. Calculate the
% Relative Standard Deviation (% RSD) as follows:
100s
% RSD 5 (1)
H
C
where:
s = estimated standard deviation, and
C¯ = average of the 10 results for measured concentration.
C¯ = average of the 10 results obtained for the high calibration solution.
12.1.2.1 The calculated % RSD should be < 5.0 %. If it is not, the user of this method may not be able to meet the performance
criteria of the method. Some
...
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