ASTM E1834-18

Standard Test Method for Analysis of Nickel Alloys by Graphite Furnace Atomic Absorption Spectrometry

SIGNIFICANCE AND USE
5.1 This test method is primarily intended to test material for compliance with specifications such as those under the jurisdiction of ASTM Technical Committee B02 on Nonferrous Metals and Alloys. It may also be used to test compliance with other specifications that are compatible with the test method.  
5.2 It is assumed that users of this test method shall be trained analysts capable of performing common laboratory procedures skillfully and safely, and that the work shall 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 test method shall prepare their own work instructions. These work instructions shall include detailed operating instructions for the specific laboratory, the specific reference materials employed, and the performance acceptance criteria. It is also expected that, when applicable, each laboratory shall participate in proficiency test programs, such as described in Practice E2027, and that the results from the participating laboratory shall be satisfactory.
SCOPE
1.1 This test method describes the graphite furnace atomic absorption spectrometric analysis of nickel, such as specified by ASTM 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 test method:    
Element  
Quantification Range (μg/g)  
Bismuth  
0.2 - 3  
Lead  
0.6 - 12  
Selenium  
0.7 - 10  
Tellurium  
0.4 - 6  
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 a test method validation study that includes an instrument performance evaluation as described in Practice E1770 is performed. Additionally, the validation study shall 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 as to the intended purpose of the analytical results.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific hazards statements see 8.2.4.2 and 9.  
1.5 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.

General Information

• Status: Published
• Publication Date: 30-Nov-2018
• ICS: 77.120.40 - Nickel, chromium and their alloys
• Technical Committee: E01 - Analytical Chemistry for Metals, Ores, and Related Materials
• Drafting Committee: E01.08 - Ni and Co and High Temperature Alloys

Relations

• Refers: ASTM E135-20 - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
• Effective Date: 01-Jan-2020
• Refers: ASTM E135-19 - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
• Effective Date: 15-May-2019
• Refers: ASTM E1770-19 - Standard Practice for Optimization of Instrumentation for Graphite Furnace Atomic Absorption Spectrometry
• Effective Date: 15-Apr-2019
• Refers: ASTM E2027-17 - Standard Practice for Conducting Proficiency Tests in the Chemical Analysis of Metals, Ores, and Related Materials
• Effective Date: 15-Nov-2017
• Refers: ASTM E50-17 - Standard Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials
• Effective Date: 01-Sep-2017
• Refers: ASTM E88-11(2017) - Standard Practice for Sampling Nonferrous Metals and Alloys in Cast Form for Determination of Chemical Composition
• Effective Date: 01-Sep-2017
• Refers: ASTM E50-11(2016) - Standard Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials
• Effective Date: 01-Aug-2016
• Refers: ASTM E135-16 - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
• Effective Date: 15-May-2016
• Refers: ASTM E135-15a - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
• Effective Date: 01-Jul-2015
• Refers: ASTM E135-15 - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
• Effective Date: 15-May-2015
• Refers: ASTM E1770-14 - Standard Practice for Optimization of Electrothermal Atomic Absorption Spectrometric Equipment
• Effective Date: 01-Dec-2014
• Refers: ASTM E135-14b - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
• Effective Date: 15-Aug-2014
• Refers: ASTM E177-14 - Standard Practice for Use of the Terms Precision and Bias in ASTM Test Methods
• Effective Date: 01-May-2014
• Refers: ASTM E135-14a - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
• Effective Date: 01-Apr-2014
• Refers: ASTM E135-14 - Standard Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
• Effective Date: 15-Feb-2014

Overview

ASTM E1834-18 is the standard test method for the analysis of nickel alloys by graphite furnace atomic absorption spectrometry (GFAAS). Published by ASTM International, this standard is primarily intended for laboratories conducting chemical composition analysis of nickel-containing alloys, especially as specified by ASTM Committee B02 on Nonferrous Metals and Alloys. The method covers a wide range of elements present in nickel-based alloys and provides guidance for both qualitative and quantitative analysis to ensure material compliance with relevant specifications.

Key Topics

• Scope of Analysis: ASTM E1834-18 describes procedures for determining the concentration of elements in nickel alloys, such as aluminum, boron, carbon, chromium, copper, cobalt, iron, magnesium, molybdenum, niobium, nickel, phosphorous, silicon, sulfur, titanium, tungsten, and vanadium. The method can also quantify trace elements including bismuth, lead, selenium, and tellurium within defined concentration ranges.
• Performance-Based Approach: This standard emphasizes the quality of analytical results over rigid procedural steps. Laboratories are expected to develop their own detailed work instructions tailored to their equipment, reference materials, and operational requirements.
• Calibration and Validation: Guidance is provided on preparing matrix-matched calibration solutions, using certified reference materials (CRMs), and applying method validation studies, particularly if extending the method to new elements or concentration ranges.
• Interferences and Controls: The method addresses potential spectral interferences, especially in complex matrices like nickel alloys, and recommends the use of Zeeman background correction techniques to minimize errors.
• Precision and Bias: ASTM E1834-18 includes data on repeatability and reproducibility, supporting its effectiveness in interlaboratory environments.

Applications

• Quality Control in Manufacturing: The standard is widely used in quality assurance and control departments to verify material composition of nickel alloys for aerospace, energy, and industrial components.
• Materials Compliance: Laboratories utilize this method to demonstrate compliance with customer or regulatory specifications, especially those under the jurisdiction of ASTM Committee B02.
• Research and Development: Metallurgical and materials science researchers apply this method for accurate chemical characterization of high-performance alloys in experimental and development settings.
• Certification and Proficiency Testing: Participation in proficiency testing programs, such as those described in ASTM E2027, is encouraged to ensure continued laboratory competence in trace element analysis.

Related Standards

ASTM E1834-18 refers to and complements several other important standards in the analysis of metals and alloys:

• ASTM E50 - General practices for apparatus, reagents, and safety in metal analysis laboratories.
• ASTM E55 and ASTM E88 - Procedures for sampling wrought and cast nonferrous metals and alloys.
• ASTM E1770 - Optimization of electrothermal atomic absorption spectrometric equipment, particularly relevant for method validation.
• ASTM E2027 - Guidelines for participation in proficiency testing programs.
• ISO Guide 31 & ISO Guide 34 - International requirements for certified reference materials.
• ISO 17034 - Competence of reference material producers.
• ISO Guide 98-3 - Guidance on the expression of uncertainty in measurement.

Practical Value

By following ASTM E1834-18, laboratories can provide reliable, reproducible, and traceable chemical analysis of nickel-based alloys. The standard supports manufacturers, suppliers, and clients by ensuring analytical results are consistent with international best practices and regulatory requirements. Adhering to this method fosters data integrity, improves supply chain trust, and enhances product quality, safety, and global market acceptance.

Utilizing analytical standards like ASTM E1834-18 is essential for any organization involved in the production, certification, or use of nickel alloys in demanding applications.

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: E1834 − 18
Standard Test Method for
Analysis of Nickel Alloys by Graphite Furnace Atomic
Absorption Spectrometry
This standard is issued under the fixed designation E1834; 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 1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
1.1 This test method describes the graphite furnace atomic
responsibility of the user of this standard to establish appro-
absorption spectrometric analysis of nickel, such as specified
priate safety, health, and environmental practices and deter-
byASTM Committee B02, and having chemical compositions
mine the applicability of regulatory limitations prior to use.
within the following limits:
For specific hazards statements see 8.2.4.2 and 9.
Application Range
Element
1.5 This international standard was developed in accor-
(Mass Fraction %)
Aluminum 0. 01 - 6.00 dance with internationally recognized principles on standard-
Boron 0. 01 - 0.10
ization established in the Decision on Principles for the
Carbon 0. 01 - 0.15
Development of International Standards, Guides and Recom-
Chromium 0. 01 - 33.00
Copper 0.01 - 35.00 mendations issued by the World Trade Organization Technical
Cobalt 0. 01 - 20.00
Barriers to Trade (TBT) Committee.
Iron 0.05 - 50.00
Magnesium 0. 01 - 0.020
2. Referenced Documents
Molybdenum 0. 01 - 30.0
Niobium 0. 01 - 6.0
2.1 ASTM Standards:
Nickel 25.00 - 100.0
D1193 Specification for Reagent Water
Phosphorous 0.001 - 0.025
Silicon 0.01 - 1.50
E29 Practice for Using Significant Digits in Test Data to
Sulfur 0.0001 - 0.01
Determine Conformance with Specifications
Titanium 0.0001 - 6.0
Tungsten 0.01 - 5.0 E50 Practices for Apparatus, Reagents, and Safety Consid-
Vanadium 0.0005 - 1.0
erations for Chemical Analysis of Metals, Ores, and
1.2 The following elements may be determined using this
Related Materials
test method: E55 Practice for Sampling Wrought Nonferrous Metals and
Alloys for Determination of Chemical Composition
Element Quantification Range (µg/g)
Bismuth 0.2 - 3
E88 Practice for Sampling Nonferrous Metals andAlloys in
Lead 0.6 - 12
Cast Form for Determination of Chemical Composition
Selenium 0.7 - 10
E135 Terminology Relating to Analytical Chemistry for
Tellurium 0.4 - 6
Metals, Ores, and Related Materials
1.3 Thistestmethodhasonlybeeninterlaboratory-testedfor
E177 Practice for Use of the Terms Precision and Bias in
the elements and ranges specified. It may be possible to extend
ASTM Test Methods
this test method to other elements or different concentration
E691 Practice for Conducting an Interlaboratory Study to
ranges provided that a test method validation study that
Determine the Precision of a Test Method
includes an instrument performance evaluation as described in
E1329 Practice for Verification and Use of Control Charts in
Practice E1770 is performed.Additionally, the validation study
Spectrochemical Analysis (Withdrawn 2019)
shall evaluate the acceptability of sample preparation method-
E1770 Practice for Optimization of Electrothermal Atomic
ology using reference materials or spike recoveries, or both.
Absorption Spectrometric Equipment
The user is cautioned to carefully evaluate the validation data
E2027 Practice for Conducting Proficiency Tests in the
as to the intended purpose of the analytical results.
1 2
This test method is under the jurisdiction of ASTM Committee E01 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
responsibility of Subcommittee E01.08 on Ni and Co and HighTemperatureAlloys. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Dec. 1, 2018. Published February 2019. Originally the ASTM website.
approved in 1996. Last previous edition approved in 2011 as E1834–11. DOI: The last approved version of this historical standard is referenced on
10.1520/E1834-18. www.astm.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E1834 − 18
ChemicalAnalysis of Metals, Ores, and Related Materials 6.3 One significant problem may be encountered for deter-
mination of bismuth in alloys with iron in excess of 10 %. It is
2.2 ISO Standards:
possible that use of Zeeman background correction will cause
ISO Guide 98-3 Uncertainty of measurement -- Part 3:
over-correction for background, resulting in erroneously low
Guide to the expression of uncertainty in measurement
results. This potential problem results from reading the shifted
(GUM:1995) – 1st Ed.
pi (π) absorption components of the iron 222.9 nm line during
ISO 17034 General requirements for the competence of
thebackgroundreadcycle.Allmodernspectrometersandthose
reference material producers
with chart recorders allow inspection of absorption profiles
obtained during analysis. During initial instrument optimiza-
3. Terminology
tion and method validation, the user of this test method shall
3.1 Definitions—For definitions of terms used in this test
assess the effect of this possible issue on the results to be
method, refer to Terminology E135.
reported. Adjustment of char time and temperatures may help
minimize this problem. Bismuth determinations made using
4. Summary of Test Method
thepeakheightmeasurementmodemayalsohelpminimizethe
4.1 Samples are dissolved in a mixture of mineral acids and
error associated with this issue.
the resulting solutions are measured using graphite furnace
6.4 The atomic lines in Table 1 have been used to analyze
atomic absorption spectrometry.
the listed elements in nickel alloys and are suggested for the
5. Significance and Use user. The user may choose to use different atomic lines
provided that sensitivity is adequate. It is recommended that
5.1 This test method is primarily intended to test material
once atomic lines are determined, the user of this test method
for compliance with specifications such as those under the
specify this information or reference instrument programs that
jurisdictionofASTMTechnicalCommitteeB02onNonferrous
include this information in their laboratory analysis proce-
Metals andAlloys. It may also be used to test compliance with
dures.
other specifications that are compatible with the test method.
5.2 It is assumed that users of this test method shall be
7. Apparatus
trained analysts capable of performing common laboratory
7.1 Graphite Furnace Atomic Absorption Spectrometer,
procedures skillfully and safely, and that the work shall be
preferably equipped with a Zeeman background correction
performed in a properly equipped laboratory.
accessory. Suitability of the spectrometer shall be established
5.3 This is a performance-based method that relies more on
using the performance criteria described in 12.7.
the demonstrated quality of the test result than on strict
adherence to specific procedural steps. It is expected that 7.2 Graphite Tubes used in this test method shall utilize a
laboratoriesusingthistestmethodshallpreparetheirownwork L’vov type platform.
instructions. These work instructions shall include detailed
7.3 Sample Preparation Equipment—Machine tools used in
operating instructions for the specific laboratory, the specific
this test method shall be capable of removing surface oxides
reference materials employed, and the performance acceptance
and other contamination from the as-received sample and then
criteria. It is also expected that, when applicable, each labora-
taking uncontaminated and chemically representative chips
tory shall participate in proficiency test programs, such as
suitable for analysis.
described in Practice E2027, and that the results from the
participating laboratory shall be satisfactory. 7.4 All labware used in this test method shall be suitably
cleaned for trace level analysis.
6. Interferences
8. Reagents and Materials
6.1 The narrow bandwidth emitted by the source lamp
makes spectral overlaps rare. However, molecular absorption
8.1 Reagents:
bands are more likely to overlap the atomic absorption line.
8.1.1 Purity of Reagents—Reagent grade chemicals shall be
This problem is commonly encountered in complex nickel
used in all tests. Unless otherwise indicated, it is intended that
alloys and a background correction technique shall be em-
all reagents conform to the specifications of the Committee on
ployed. The use of the Zeeman background correction tech-
Analytical Reagents of the American Chemical Society where
nique should be used in performance of this test method.
6.2 When Zeeman background correction is used for nickel
alloy analysis, background absorbance up to approximately 1.5
absorbance units is adequately corrected for. The user is
TABLE 1 Suggested Atomic Absorption Analytical Lines/
cautioned to examine calibration and sample solution back-
Interference
ground levels during method validation to verify that back-
Potential
Element Wavelength (nm)
Interference
ground absorbance is less than 1.5 absorbance units.
Bismuth 223.1 Fe
Lead 283.3
Selenium 196.0
Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St., Tellurium 214.3
4th Floor, New York, NY 10036, http://www.ansi.org.
E1834 − 18
platedigestion.Alternativedigestionmethodssuchasmicrowaveorbomb
such specifications are available. However, the purity of acid
digestion may be used.
reagents utilized in this procedure shall be suitable for trace
metal analysis and shall not contain impurities in any signifi-
8.2.4.1 Weigh 1.0 g of pure nickel into an HF resistant
cant amount. Other grades may be used provided it is first
digestion vessel. Use one vessel for each calibration solution.
ascertained that the reagent is of sufficiently high purity to
8.2.4.2 Dissolve the pure nickel in 20 mL of HNO +HF+
permit its use without lessening the accuracy of the determi-
H20(1+1+1)per gram of sample. Caution—If powdered
nation.
nickel is used, add the acid cautiously as powdered metals tend
8.1.2 Reagent Water—The purity of reagent water shall
to be very reactive.
conform to the requirements of Specification D1193 for re-
8.2.4.3 Heat the digestion vessels gently until the nickel
agent water, Type I. The water purification method used shall
dissolves. Remove the beakers from the heat. Continue to heat
be capable of removing all elements in concentrations that
the vessels gently to reduce this solution to approximately 5
might bias the test results.
8.1.3 1000 µg/mL Palladium + 500 µg/mL Magnesium mL to remove excess HF. Wet salts may form.
Matrix Modifier—To prepare this modifier, mix 1 mL of 2000
8.2.4.4 Cool the beakers slightly and then redissolve the
µg/mL palladium (in dilute HNO ) and 1 mL of 1000 µg/mL
salts by heating in approximately 20 mL of water.
magnesium (in dilute HNO ). Five µL of this solution adds 5
8.2.4.5 Cool the nickel solutions and transfer into 50 mL
µgofpalladiumand2.5µgofmagnesiumnitratetothefurnace.
plastic flasks. Polypropylene or polymethylpentene flasks are
8.1.4 HNO +HF+H O(1+1+1)—To 150 mLof water
3 2
acceptable for this purpose.
carefully add 150 mLof HNO and 150 mLHF. Mix and store
8.2.5 Add the required amounts of single element CRM
in an HF resistant bottle.
solutions to the flasks, leaving one analyte-free for use as a
8.1.5 High Purity Nickel—The nickel selected shall be free
blank.
of the scoped analytes.
8.2.6 The laboratory may choose to prepare calibration
8.2 Calibration Solutions:
solutions by dissolving nickel alloy certified reference materi-
8.2.1 In this test method, calibration is performed by either
als containing analytes covering the expected sample compo-
(1) laboratory-prepared, matrix-matched solutions created
sition range. For this, the calibration blank may be either a
from assayed pure nickel and single element reference material
reagent blank of the reagents used for sample dissolution as
solutions, (2) solutions of dissolved, solid, certified reference
described in Section 13 or a pure nickel matrix blank prepared
material (CRMs) for nickel alloys, or (3) the method of
as described in 8.2.4.
standard additions using single element reference material
solutions to spike prepared samples. The CRMs should have
8.2.7 The method of standard additions is an acceptable
been produced using an ISO 17034 compliant process.
method of calibration. Two different approaches may be used
8.2.2 Sections 8.2.3–8.2.5 describe the preparation of
in the preparation of the spiked calibration solutions, as
matrix-matched calibration solutions for analysis of sample
discussed below. If the method of standard additions is used, it
solutions that contain 1 g alloy/50 mL final dilution. It is
is necessary to demonstrate instrument performance as de-
acceptable to vary final concentrations as long as the user’s
scribed in 12.7 through 12.10, prior to preparing samples and
method demonstrates acceptable measurement variability and
spiking them with additions of calibration solutions. When
detection limit (see 12.7). Section 8.2.6 describes preparation
measured, the prepared sample/calibration solutions shall yield
of dissolved solid CRM solutions. Section 8.2.7 describes
a linear calibration of instrument response versus amount of
preparation of calibration solutions for methods of additions.
added element.
8.2.3 Determine the number and concentrations of calibra-
8.2.7.1 Method 1:
tion solutions needed to cover the concentration range for each
(1) GFAAis typically employed for the scoped elements to
element. It is suggested that the calibration solutions have their
verify the absence of the element of interest from the material.
highest concentration slightly above the highest expected
Single point method of additions is employed by some labo-
sample concentration (Sk as described in Practice E1770), a
ratories to verify the absence of the analyte of interest. This
concentration in the mid range of the expected sample
approach to calibration shall be well validated as described in
concentrations, a concentration at or near the reporting limit
(S1 as described Practice E1770), and a blank (S0 as described Section 15.
(2) PrepareonesamplesolutioninaccordancewithSection
in Practice E1770). Regardless, a minimum of three solutions
including a blank shall be used for calibration. It is important 13. This solution shall serve as the unspiked calibration
that the higher concentration solutions do not yield absor- solution.
bances outside the linear range (see 12.10 to 12.11).
(3) Prepare another sample solution in accordance with
8.2.4 Prepare matrix solutions as follows:
Section 13. Spike the solution with an aliquot of CRM solution
to yield a final solution concentration known to fall within the
NOTE 1—The following preparation instructions are written for hot
linear range for the analyte of interest. It is acceptable to use
the solution prepared in 8.2.7.1(2) and make the CRM solution
Reagent Chemicals, American Chemical Society Specifications, American
spike directly to the platform in the graphite tube to yield the
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
spiked calibration solution.
listed by the American Chemical Society, see the United States Pharmacopeia and
National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville, MD. 8.2.7.2 Method 2:
E1834 − 18
(1) If samples have concentrations falling above the 12.3 Define the number of replicate measurements to be
method scope minimum, then Method 1 cannot be used. A made and averaged for a single reported result. Typically, a
more rigorous approach to generating the method of additions minimum of two replicates is specified.
calibration solutions shall be taken.
12.4 Use of a mixed 5 µg palladium plus 2.5 µg magnesium
(2) Prepare four sample solutions as described in Section
matrix modifier is recommended. Set up the instrument auto-
13.SpikethesesamplesolutionswithCRMaliquotstoproduce
sampler to add the matrix modifier to the furnace during the
solutions that cover the linear range for the analyte of interest.
heating parameter optimization study, during calibration and
Acceptable linear range is discussed in Section 12.
during sample analysis. The user may choose not to use a
(3) It is acceptable to prepare a single sample solution as
modifier or to use different modifiers or modifier masses,
described in Section 13 and spike the sample solution directly
provided method validation in accordance with Section 15
on the furnace platform to produce the four spike calibration
demonstrates the acceptability of the selected protocol.
solutions.
12.5 The manufacturer shall specify the maximum total
8.3 Other Materials:
volume of sample and modifier solution that may be pipetted
8.3.1 Argon—The atomic absorption spectrometer shall use
ontotheL’vovplatform.Thisvolumeshallbeconsideredwhen
argon to protect the tube from oxidation during heating and to
optimizing heating parameters.
remove vapor from the tube. The purity of the argon supply
shall be as specified by the instrument manufacturer.
12.6 Optimize the heating parameters to minimize sample
8.3.2 Control Materials:
backgrounds while maximizing absorbance. Practice E1770
8.3.2.1 A laboratory may choose to procure, produce, or
provides a suggested procedure for optimization of heating
have manufactured a chip material containing analyte contents
parameters.
in the range of typical samples to be used as a control material.
12.7 Determineinstrumentperformancedataasdescribedin
These chips should be well blended and checked for homoge-
Practice E1770. Evaluate the data as follows:
neity.
12.7.1 Compare the calculated instrument detection limit to
8.3.2.2 A laboratory may find it difficult to procure or have
the method lower scope limit. If the instrument does not
manufactured the materials described in 8.3.2.1 for all of the
demonstrate a detection limit equivalent to or better than the
necessary analytes or alloys. For this situation, it is acceptable
lower scope limit, it is possible that the user may not be able to
to prepare equivalent reference material solutions using an
meet this method’s lower scope.
alternative source of nickel for the matrix solution, spiked with
different single element CRM solutions. 12.7.2 Compare the standard deviation determined for the
most concentrated solution (S ) with the method minimum SD
k
9. Hazards
(S ) for a ma
...

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: E1834 − 11 E1834 − 18
Standard Test Method for
Analysis of Nickel Alloys by Graphite Furnace Atomic
Absorption Spectrometry
This standard is issued under the fixed designation E1834; 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 graphite furnace atomic absorption spectrometric analysis of nickel, such as specified by
ASTM Committee B02, and having chemical compositions within the following limits:
Application Range
Element
(Wt. %)
Application Range
Element
(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 test method:
Element Quantification Range (μg/g)
Bismuth 0.2 - 3
Lead 0.6 - 12
Selenium 0.7 - 10
Tellurium 0.4 - 6
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 a test method validation study that includes an
instrument performance evaluation as described in Practice E1770 is performed. Additionally, the validation study shall 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 as to the intended purpose of the analytical results.
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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use. For specific hazards statements see Note 28.2.4.2 and Section 9.
1.5 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.
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 Dec. 1, 2011Dec. 1, 2018. Published February 2012February 2019. Originally approved in 1996. Last previous edition approved in 20092011
as E1834 – 09.E1834–11. DOI: 10.1520/E1834-11.10.1520/E1834-18.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
E1834 − 18
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 (Withdrawn 2019)
E1770 Practice for Optimization of Electrothermal Atomic Absorption Spectrometric Equipment
E2027 Practice for Conducting Proficiency Tests in the Chemical Analysis of Metals, Ores, and Related Materials
2.2 ISO Standards:
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) –
1st Ed.
ISO 17034 General requirements for the competence of reference material producers
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 graphite furnace atomic
absorption spectrometry.
5. Significance and Use
5.1 This test method is primarily intended to test material for compliance with specifications such as those under the jurisdiction
of ASTM Technical Committee B02 on Nonferrous Metals and Alloys. It may also be used to test compliance with other
specifications that are compatible with the test method.
5.2 It is assumed that users of this test method shall be trained analysts capable of performing common laboratory procedures
skillfully and safely, and that the work shall 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 test method shall prepare their own work instructions. These
work instructions shall include detailed operating instructions for the specific laboratory, the specific reference materials employed,
and the performance acceptance criteria. It is also expected that, when applicable, each laboratory shall participate in proficiency
test programs, such as described in Practice E2027, and that the results from the participating laboratory shall be satisfactory.
6. Interferences
6.1 The narrow bandwidth emitted by the source lamp makes spectral overlaps rare. However, molecular absorption bands are
more likely to overlap the atomic absorption line. This problem is commonly encountered in complex nickel alloys and a
background correction technique shall be employed. The use of the Zeeman background correction technique should be used in
performance of this test method.
6.2 When Zeeman background correction is used for nickel alloy analysis, background absorbance up to approximately 1.5
absorbance units is adequately corrected for. The user is cautioned to examine calibration and sample solution background levels
during method validation to verify that background absorbance is less than 1.5 absorbance units.
6.3 One significant problem may be encountered for determination of bismuth in alloys with iron in excess of 10 %. It is
possible that use of Zeeman background correction will cause over-correction for background, resulting in erroneously low results.
This potential problem results from reading the shifted pi (π) absorption components of the iron 222.9 nm line during the
background read cycle. All modern spectrometers and those with chart recorders allow inspection of absorption profiles obtained
during analysis. During initial instrument optimization and method validation, the user of this test method shall assess the effect
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. 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.
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of this possible issue on the results to be reported. Adjustment of char time and temperatures may help minimize this problem.
Bismuth determinations made using the peak height measurement mode may also help minimize the error associated with this
issue.
6.4 The atomic lines 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 different atomic lines provided that sensitivity is adequate. It is recommended that once atomic lines
are determined, the user of this test method specify this information or reference instrument programs that include this information
in their laboratory analysis procedures.
7. Apparatus
7.1 Graphite Furnace Atomic Absorption Spectrometer, preferably equipped with a Zeeman background correction accessory.
Suitability of the spectrometer shall be established using the performance criteria described in 12.7.
7.2 Graphite Tubes used in this test method shall utilize a L’vov type platform.
7.3 Sample Preparation Equipment—Machine tools used in this test method shall be capable of removing surface oxides and
other contamination from the as-received sample and then taking uncontaminated and chemically representative chips suitable for
analysis.
7.4 All labware used in this test method shall 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 shall not contain impurities in any significant amount. 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 Water—The purity of reagent water shall conform to the requirements of Specification D1193 for reagent water,
Type I. The water purification method used shall be capable of removing all elements in concentrations that might bias the test
results.
8.1.3 1000 μg/mL Palladium + 500 μg/mL Magnesium Matrix Modifier—To prepare this modifier, mix 1 mL of 2000 μg/mL
palladium (in dilute nitricHNO acid) ) and 1 mL of 1000 μg/mL magnesium (in dilute nitricHNO acid). ). Five μL of this solution
3 3
adds 5 μg of palladium and 2.5 μg of magnesium nitrate to the furnace.
8.1.4 HNO + HF + H O (1 + 1 + 1)—To 150 mL of water carefully add 150 mL of HNO and 150 mL HF. Mix and store
3 2 3
in an HF resistant bottle.
8.1.5 High Purity Nickel—The nickel selected shall be free of the scoped analytes.
8.2 Calibration Solutions:
8.2.1 In this test method, calibration is based performed by either on(1) laboratory-prepared, pure nickel matrix-matched
matrix-matched solutions created from assayed pure nickel and single element reference material solutions, dissolved(2) solid
solutions of dissolved, solid, certified reference material (CRM) solutions, (CRMs) for nickel alloys, or on(3) samples to which
methodsthe method of standard additions spikes have been made. The matrix-matched solutions are prepared with nickel of known
purity. These matrix solutions are then spiked with aliquots of single element (CRM) solutions, which contain the elements of
interest. The CRMs shall be compliant with ISO Guide 31 and ISO Guide 34.using single element reference material solutions to
spike prepared samples. The CRMs should have been produced using an ISO 17034 compliant process.
8.2.2 Sections 8.2.3–8.2.5 describe the preparation of matrix-matched calibration solutions for analysis of sample solutions that
contain 1 g alloy/50 mL final dilution. It is acceptable to vary final concentrations as long as the user’s method demonstrates
acceptable measurement variability and detection limit (see 12.7). Section 8.2.6 describes preparation of dissolved solid CRM
solutions. Section 8.2.7 describes preparation of calibration solutions for methods of additions.
TABLE 1 Suggested Atomic Absorption Analytical Lines/
Interference/Modifiers Lines/Interference
Potential
Element Wavelength (nm)
Interference
Bismuth 223.1 Fe
Lead 283.3
Selenium 196.0
Tellurium 214.3
Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. 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.
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8.2.3 Determine the number and compositionconcentrations 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 (Sk as described in Practice E1770), a concentration in the mid range of the expected sample concentrations,
a concentration at or near the reporting limit (S1 as described Practice E1770), and a blank (S0 as described in Practice E1770).
In any case, Regardless, a minimum of three solutions including a blank shall be used for calibration. It is important that the higher
concentration solutions do not yield absorbances outside of the linear range (see 12.10 to 12.11).
8.2.4 Prepare matrix solutions as follows:
NOTE 1—The following preparation instructions are written for hot plate digestion. Alternative digestion methods such as microwave or bomb digestion
may be used.
8.2.4.1 Weigh 1.0 g of pure nickel into an HF resistant digestion vessel. Use one vessel for each calibration solution.
8.2.4.2 Dissolve the pure nickel in 20 mL of HNO + HF + H20 (1 + 1 + 1) per gram of sample. Caution—If powdered nickel
is used, add the acid cautiously as powdered metals tend to be very reactive.
NOTE 2—Caution—If powdered nickel is used, add the acid cautiously as powdered metals tend to be very reactive.
8.2.4.3 Heat the digestion vessels gently until the nickel dissolves. Remove the beakers from the heat. Continue to heat the
vessels gently to reduce this solution to approximately 5 mL in order to remove excess HF. Wet salts may form.
8.2.4.4 Cool the beakers slightly and then redissolve the salts by heating in approximately 20 mL of water.
8.2.4.5 Cool the nickel solutions and transfer into 50 mL plastic flasks. Polypropylene or polymethylpentene flasks are
acceptable for this purpose.
8.2.5 Add the required amountamounts of single element CRM solutions intoto the flasks, making sure to leave leaving one
analyte-free for use as a blank.
8.2.6 The laboratory may choose to prepare calibration solutions by dissolving nickel alloy certified reference materials
containing analytes covering the expected sample concentration range. In this case, composition range. For this, the calibration
blank may be either a reagent blank of the reagents used for sample dissolution as described in Section 13 or a pure nickel matrix
blank prepared as described in 8.2.4.
8.2.7 The method of standard additions is also an acceptable method of calibration solution preparation. calibration. Two
different approaches may be used in the preparation of the spiked calibration solutions. solutions, as discussed below. If the method
of standard additions is used, it will be is necessary to demonstrate instrument performance as described in Sections 12.7 through
12.10, prior to routinely preparing method of additions calibration solutions. The methods of additions calibration solutions
prepared preparing samples and spiking them with additions of calibration solutions. When measured, the prepared sample/
calibration solutions shall yield a linear calibration of instrument response when analyzed.versus amount of added element.
8.2.7.1 Method 1:
(1) GFAA is typically employed for the scoped elements to verify the absence of the element of interest from the material. Single
point method of additions is employed by some laboratories in order to verify the absence of the analyte of interest. This approach
to calibration shall be well validated as described in Section 15.
(1) GFAA is typically employed for the scoped elements to verify the absence of the element of interest from the material.
Single point method of additions is employed by some laboratories to verify the absence of the analyte of interest. This approach
to calibration shall be well validated as described in Section 15.
(2) Prepare one sample solution in accordance with Section 13. This solution shall serve as the unspiked calibration solution.
(3) Prepare another sample solution in accordance with Section 13. Spike the solution with an aliquot of CRM solution to yield
a final solution concentration known to fall within the linear range for the analyte of interest. It is acceptable to use the solution
prepared in 8.2.7.1(2) and make the CRM solution spike directly to the platform in the graphite tube to yield the spiked calibration
solution.
(2) Prepare one sample solution in accordance with Section 13. This solution shall serve as the unspiked calibration solution.
(3) Prepare another sample solution in accordance with Section 13. Spike the solution with an aliquot of CRM solution to yield
a final solution concentration known to fall within the linear range for the analyte of interest. It is acceptable to use the solution
prepared in 8.2.7.1(2) and make the CRM solution spike directly to the platform in the graphite tube to yield the spiked calibration
solution.
8.2.7.2 Method 2:
(1) If samples routinely have concentrations falling above the method scope minimum, then Method 1 cannot be used. A more
rigorous approach to generating the method of additions calibration solutions shall be taken.
(1) If samples have concentrations falling above the method scope minimum, then Method 1 cannot be used. A more rigorous
approach to generating the method of additions calibration solutions shall be taken.
(2) Prepare four sample solutions as described in Section 13. Spike these sample solutions with CRM aliquots to produce
solutions that cover the linear range for the analyte of interest. Acceptable linear range is discussed in Section 12.
(3) It is acceptable to prepare a single sample solution as described in Section 13 and spike the sample solution directly on the
furnace platform to produce the four spike calibration solutions.
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(2) Prepare four sample solutions as described in Section 13. Spike these sample solutions with CRM aliquots to produce
solutions that cover the linear range for the analyte of interest. Acceptable linear range is discussed in Section 12.
(3) It is acceptable to prepare a single sample solution as described in Section 13 and spike the sample solution directly on the
furnace platform to produce the four spike calibration solutions.
8.3 Other Materials:
8.3.1 Argon—The atomic absorption spectrometer shall use argon to protect the tube from oxidation during heating and to
remove vapor from the tube. The purity of the argon supply shall be as specified by 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.
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 For this situation, it is acceptable to prepare equivalent reference material
solutions using an alternative source of nickel for the matrix solution and solution, spiked with different single element CRM
solutions.
9. Hazards
9.1 This test 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 sampl
...