ASTM E2823-11

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: E2823 − 11
Standard Test Method for
Analysis of Nickel Alloys by Inductively Coupled Plasma
Mass Spectrometry (Performance-Based Method)
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 cautioned to carefully evaluate the validation data as to the
intended purpose of the analytical results.
1.1 This test method describes the inductively coupled
1.4 This standard does not purport to address all of the
plasma mass spectrometric analysis of nickel, as specified by
safety concerns, if any, associated with its use. It is the
Committee B02, and having chemical compositions within the
responsibility of the user of this standard to establish appro-
following limits:
priate safety and health practices and determine the applica-
Element Application Range (Wt. %)
bility of regulatory limitations prior to use. Specific safety
Aluminum 0. 01–6.00
Boron 0. 01–0.10
hazard statements are given in Section 9.
Carbon 0. 01–0.15
Chromium 0. 01–33.00
2. Referenced Documents
Copper 0.01–35.00
Cobalt 0. 01–20.00
2.1 ASTM Standards:
Iron 0.05–50.00
D1193 Specification for Reagent Water
Magnesium 0. 01–0.020
Molybdenum 0. 01–30.0 E50 Practices for Apparatus, Reagents, and Safety Consid-
Niobium 0. 01–6.0
erations for Chemical Analysis of Metals, Ores, and
Nickel 25.00–100.0
Related Materials
Phosphorous 0.001–0.025
Silicon 0.01–1.50
E55 Practice for Sampling Wrought Nonferrous Metals and
Sulfur 0.0001–0.01
Alloys for Determination of Chemical Composition
Titanium 0.0001–6.0
E88 Practice for Sampling Nonferrous Metals andAlloys in
Tungsten 0.01–5.0
Vanadium 0.0005–1.0
Cast Form for Determination of Chemical Composition
E135 Terminology Relating to Analytical Chemistry for
1.2 The following elements may be determined using this
Metals, Ores, and Related Materials
method.
E177 Practice for Use of the Terms Precision and Bias in
Element Quantification Range (µg/g)
ASTM Test Methods
Antimony 0.5–50
Bismuth 0.1–11 E691 Practice for Conducting an Interlaboratory Study to
Gallium 2.9–54
Determine the Precision of a Test Method
Lead 0.4–21
E1329 Practice for Verification and Use of Control Charts in
Silver 1–35
Tin 2.2–97
Spectrochemical Analysis
Thallium 0.5–3.0
E1479 Practice for Describing and Specifying Inductively-
1.3 This method has only been interlaboratory tested for the Coupled Plasma Atomic Emission Spectrometers
E1601 Practice for Conducting an Interlaboratory Study to
elementsandrangesspecified.Itmaybepossibletoextendthis
method to other elements or different composition ranges Evaluate the Performance of an Analytical Method
provided that method validation that includes evaluation of E2027 Practice for Conducting Proficiency Tests in the
method sensitivity, precision, and bias as described in this ChemicalAnalysis of Metals, Ores, and Related Materials
documentisperformed.Additionally,thevalidationstudymust E2165 Practice for Establishing an Uncertainty Budget for
evaluate the acceptability of sample preparation methodology the Chemical Analysis of Metals, Ores, and Related
using reference materials and/or spike recoveries. The user is Materials (Withdrawn 2007)
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
This test method is under the jurisdiction of ASTM Committee E01 on contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct Standards volume information, refer to the standard’s Document Summary page on
responsibility of Subcommittee E01.08 on Ni and Co and HighTemperatureAlloys. the ASTM website.
Current edition approved May 1, 2011. Published July 2011. DOI: 10.1520/ The last approved version of this historical standard is referenced on
E2823-11. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E2823 − 11
2.2 ISO Standards: internal standard solution during sample analysis is also
ISO 17025 General Requirements for the Competence of possible provided acceptable instrument sensitivity is main-
Calibration and Testing Laboratories tained.
ISO Guide 31 Contents of Certificates of Reference Materi-
6.3 Isobaric and polyatomic mass overlap interferences are
als
best addressed by selecting an alternate atomic mass. Some
ISO Guide 34 Quality System Guidelines for the Production
instrument manufacturers offer software options for math-
of Reference Materials
ematically correcting for common interferences, but the user is
ISO Guide 98-3 Uncertainty of Measurement—Part 3:
cautioned to carefully evaluate this approach to mass overlap
Guide to the Expression of Uncertainty in Measurement
correction. However, some laboratories participating in the
(GUM:1995), First Edition
interlaboratory study found it necessary to generate a math-
ematical correction for the effect of the ZrO interference on the
3. Terminology
Ag 107 isotope. In this case the Zr 91 isotope was used for
3.1 Definitions—For definitions of terms used in this test
zirconium determination.
method, refer to Terminology E135.
6.4 Modern instruments may have a collision or reaction
cell which can use ion-molecule collisions or reactions to
4. Summary of Test Method
remove spectral interferences. The user of this method must
4.1 Samples are dissolved in a mixture of mineral acids and
examine this information to ascertain the need for collision/
the resulting solutions are measured using inductively coupled
reaction cells for the removal of spectral interferences.
plasma mass spectrometry.
6.5 The isotopes listed in Table 1 have been used to analyze
5. Significance and Use the listed elements in nickel alloys and are suggested for the
user. The user may choose to use multiple isotopes to help
5.1 This test method for the chemical analysis of nickel
verifythatatomicmassselectionisoptimizedfortheparticular
alloysisprimarilyintendedtotestmaterialforcompliancewith
alloy being determined. It is recommended that once isotopes
specifications such as those under jurisdiction of ASTM
and appropriate spectral corrections are determined, the user of
committee B02. It may also be used to test compliance with
this method specify this information or reference instrument
other specifications that are compatible with the test method.
programs which include this information in their laboratory
5.2 Itisassumedthatallwhousethismethodwillbetrained
analysis procedures.
analysts capable of performing common laboratory procedures
skillfully and safely, and that the work will be performed in a
7. Apparatus
properly equipped laboratory.
7.1 Suitability of an Inductively Coupled Plasma Mass
5.3 This is a performance-based method that relies more on
Spectrometer for testing of this method will be established
the demonstrated quality of the test result than on strict
using the performance criteria described in section 12.1. The
adherence to specific procedural steps. It is expected that
sample introduction system shall be capable of handling
laboratories using this method will prepare their own work
solutions containing trace amounts of HF. Each instrument
instructions. These work instructions will include detailed
shall be installed and operated according to the manufacturer’s
operating instructions for the specific laboratory, the specific
recommendations.
reference materials employed, and performance acceptance
7.2 Sample Preparation Equipment—Machinetoolsshallbe
criteria. It is also expected that, when applicable, each labora-
used that are capable of removing surface oxides and other
tory will participate in proficiency test programs, such as
contamination from the as-received sample and then taking
described in Practice E2027, and that the results from the
uncontaminated and chemically representative chips suitable
participating laboratory will be satisfactory.
for analysis.
6. Interferences
7.3 All labware used should be suitably cleaned for trace
level analysis.
6.1 When possible, analyte isotopes are selected, which are
free from mass overlap interferences. Because isotope choices
8. Reagents and Materials
are limited, this is not always an option. It is the responsibility
8.1 Reagents:
of the user to determine run conditions and parameters that
avoidorcompensateforinterferencesthatmaybiastestresults.
6.2 The use of an internal standard may compensate for the
TABLE 1 Suggested Isotopes/Interference
physical interferences resulting from variations in sample and
Potential
Element Isotope
calibrationsolutionaerosoltransportrates.Theusermaychose
Interference
to add the internal standard by spiking each solution with a
Antimony 121
Bismuth 209
specified amount of an appropriate certified reference material
Gallium 71
(CRM) solution.Alternatively, on-line addition of a peripheral
Lead 208
Silver 107 ZrO, FeCr
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 − 11
8.1.1 Purity of Reagents—Reagent grade chemicals shall be dissolve many types of nickel alloys . For high Mo-Cr alloys it
used in all tests. Unless otherwise indicated, it is intended that has been found that concentrated HCl with the addition of
all reagents conform to the specifications of the Committee on concentrated HNO dropwise may be necessary to avoid
Analytical Reagents of the American Chemical Society where passivation.
such specifications are available. However, the purity of acid
8.2.4.4 Heat the digestion vessels gently until the nickel
reagents utilized in this procedure shall be suitable for trace
dissolves. Remove the beakers from the heat, add 10 drops of
metal analysis and should not contain impurities in any
49 % HF, and swirl gently. If HNO +HF+HO(1+1+1)
3 2
significant amount. Other grades may be used, provided it is
is used for digestion it is not necessary to add additional HF.
first ascertained that the reagent is of sufficiently high purity to
The laboratory may choose to reduce this solution to wet salts
permit its use without lessening the accuracy of the determi-
in order to remove excess HF and then re-dissolve by heating
nation.
the salts in approximately 20 mL of water.
8.1.2 Reagent Water—The purity of reagent water shall
8.2.4.5 If an internal standard is to be used, add the
conform to the requirements of Specification D1193 for re-
predetermined amount into each solution.
agent water, Type I. The water purification method used must
8.2.4.6 Cool the nickel solutions and transfer into 1-L
be capable of removal of all elements in concentrations that
plastic flasks. Polypropylene or polymethylpentene flasks are
might bias the test results.
acceptable for this purpose.
8.1.3 Internal Standard—The use of an internal standard is
8.2.5 Add the needed amount of single element CRM
recommended. The use of an internal standard may compen-
solutions into the flasks, making sure to leave one analyte-free
sate for the physical interferences resulting from variations in
for use as a blank. Maintain the acidity necessary to assure
sample and calibration solution aerosol transport rates.
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. The CRMs shall be compliant with ISO
8.3.1 Argon and Collision/Reaction Gases—The ICP argon
Guides 31 and 34.
supply and any collision/reaction gas supply shall be specified
8.2.2 Step 8.2.3 and following describe the preparation of
by the instrument manufacturer.
calibration solutions for analysis of sample solutions that
8.3.2 Control Materials:
contain 1 g alloy/L final dilution. It is acceptable to vary final
8.3.2.1 A laboratory may choose to procure, produce, or
concentrations as long as the user’s method demonstrates
have manufactured a chip material containing analyte contents
adequate sensitivity and precision (see section 12.1).
in the range of typical samples to be used as a control material.
8.2.3 Determine the number and composition of calibration
These chips should be well blended and checked for homoge-
solutions needed to cover the concentration range for each
neity.
element. It is suggested that the calibration solutions have their
highest concentration slightly above the highest expected
8.3.2.2 A laboratory may find it difficult to procure or have
sample concentration, a concentration in the mid range of the manufactured the materials described in 8.3.2.1 for all of the
expected sample concentrations, a concentration at or near the
necessary analytes or alloys. If this is the case, then it is
reporting limit, and a blank. In any case, a minimum of three acceptable to prepare equivalent reference material solutions
solutions including a blank must be used for calibration. usinganalternativesourceofnickelforthematrixsolutionand
8.2.4 Prepare matrix solutions as follows: spiked with different single element CRM solutions.
8.2.4.1 Weigh 0.5 g of pure nickel into an HF resistant
digestionvessel.Useonevesselforeachcalibrationsolutionto 9. Hazards
be made.
9.1 This method involves the use of concentrated HF. Read
8.2.4.2 Dissolve the pure nickel in 20 mL of acid mixture
and follow label precautions, MSDS information, and refer to
per gram of sample. Select acid mixtures that will dissolve the
Practice E50. For precautions to be observed in the use of
alloys to be analyzed using this method.
certain other reagents in this test method, refer to Practice E50.
NOTE 1—Caution: If powdered nickel is used, add the acid cautiously
as powdered metals tend to be very reactive.
10. Sampling, Test Specimens, and Test Units
8.2.4.3 A mixture of HCl + HNO (9 + 1), HCl + HO+
3 2
10.1 Laboratories shall follow written practices for sam-
HNO (3+2+1),orHNO +HF+H O (1 + 1 + 1) will
3 3 2
pling and preparation of test samples. These practices shall
me
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