Standard Test Method for Determination of Lead in Nickel Alloys by Graphite Furnace Atomic Absorption Spectrometry

SIGNIFICANCE AND USE
This test method is used for the determination of trace levels of lead in nickel alloys by GF-AAS to check compliance with compositional specifications. It is assumed that the procedure will be performed by trained analysts capable of performing common laboratory practices skillfully and safely. It is expected that the work will be performed in a properly equipped laboratory and proper waste disposal procedures will be followed. Appropriate quality control practices must be followed such as those described in Guide E 882.
SCOPE
1.1 This test method covers the determination of lead in nickel alloys in the concentration range 0.00005 % to 0.001 % by graphite furnace atomic absorption spectrometry (GF-AAS).
Note 1—If this test method is used to test materials having contents less than 0.0001 % lead, users in different laboratories may experience more than the usual 5 % risk that their results will differ by more than 50 % relative error.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 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. For specific hazards associated with the use of this test method, see Practices E 50.

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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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:E1834–09
Standard Test Method for
Determination of Lead in Nickel Alloys by Graphite Furnace
1
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 E1601 Practice for Conducting an Interlaboratory Study to
Evaluate the Performance of an Analytical Method
1.1 This test method covers the determination of lead in
E1770 Practice for Optimization of Electrothermal Atomic
nickel alloys in the concentration range 0.00005 % to 0.001 %
Absorption Spectrometric Equipment
by graphite furnace atomic absorption spectrometry (GF-
3
2.2 ISO Standards:
AAS).
ISO 5725:1986 PrecisionofTestMethods—Determination
NOTE 1—If this test method is used to test materials having contents
of Repeatability and Reproducibility for a Standard Test
less than 0.0001 % lead, users in different laboratories may experience
Method by Inter-Laboratory Tests
more than the usual 5 % risk that their results will differ by more than
ISO 11437:1994 Nickel Alloys — Determination of Trace-
50 % relative error.
Element Content — Electrothermal Atomic Absorption
1.2 The values stated in SI units are to be regarded as
Spectrometric Method–Part 2: Determination of Lead
standard. No other units of measurement are included in this
Content
standard.
1.3 This standard does not purport to address all of the
3. Terminology
safety concerns, if any, associated with its use. It is the
3.1 Definitions—For definitions of terms used in this test
responsibility of the user of this standard to establish appro-
method, refer to Terminology E135.
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use.Forspecifichazards 4. Summary of Test Method
associated with the use of this test method, see Practices E50.
4.1 The sample is dissolved in a mixture of HNO , HF, and
3
water and diluted to a known volume. A nickel-ammonium
2. Referenced Documents
phosphate matrix modifier is added to an appropriate aliquot
2
2.1 ASTM Standards:
and a portion is injected into the graphite furnace atomizer of
E50 Practices for Apparatus, Reagents, and Safety Consid-
an atomic absorption spectrometer, which is provided with a
erations for Chemical Analysis of Metals, Ores, and
background corrector. The sample is dried, pyrolized, and
Related Materials
atomized.Theabsorbanceoftheresonancespectrallineoflead
E135 Terminology Relating to Analytical Chemistry for
is measured at 283.3 nm and compared with that from
Metals, Ores, and Related Materials
matrix-matched calibration solutions.
E882 Guide for Accountability and Quality Control in the
Chemical Analysis Laboratory
5. Significance and Use
E1184 Practice for Electrothermal (Graphite Furnace)
5.1 This test method is used for the determination of trace
Atomic Absorption Analysis
levels of lead in nickel alloys by GF-AAS to check compliance
with compositional specifications. It is assumed that the
1
procedure will be performed by trained analysts capable of
This test method is under the jurisdiction of ASTM Committee E01 on
Analytical Chemistry for Metals, Ores, and Related Materials and is the direct performing common laboratory practices skillfully and safely.
responsibility of Subcommittee E01.08 on Ni and Co and HighTemperatureAlloys.
It is expected that the work will be performed in a properly
Current edition approved July 15, 2009. Published August 2009. Originally
equipped laboratory and proper waste disposal procedures will
approved in 1996. Last previous edition approved in 2002 as E1834 – 96 (2002).
DOI: 10.1520/E1834-09.
2
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
3
Standards volume information, refer to the standard’s Document Summary page on Available fromAmerican National Standards Institute (ANSI), 25 W. 43rd St.,
the ASTM website. 4th Floor, New York, NY 10036, http://www.ansi.org.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1

---------------------- Page: 1 ----------------------
E1834–09
be followed. Appropriate quality control practices must be 8. Reagents
followed such as those described in Guide E882.
8.1 Purity and Concentration of Reagents—The purity and
concentration of common chemical reagents and water shall
6. Apparatus
conform to Practices E50. The reagents should be free of, or
6.1 Atomic Absorption Spectrometer, with graphite furnace
contain minimal amounts (< 0.01 µg/g) of, lead.
...

This document is not anASTM standard and is intended only to provide the user of anASTM 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:E1834–96 (Reapproved 2002) Designation:E1834–09
Standard Test Method for
Determination of Lead in Nickel Alloys by Electrothermal
Graphite Furnace Atomic Absorption Spectrometric
1
MethodSpectrometry
This standard is issued under the fixed designation E 1834; 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 covers the determination of lead in nickel and nickel alloys in the concentration range of 0.00005 % to
0.001 % by electrothermal graphite furnace atomic absorption spectrometry (GF-AAS).
NOTE1—If this test method is used to test materials having contents less than 0.0001% lead, users in different laboratories will experience more than
the usual 5% risk that their results will differ by more than 50% relative error.
1.2 1—If this test method is used to test materials having contents less than 0.0001 % lead, users in different laboratories may
experience more than the usual 5 % risk that their results will differ by more than 50 % relative error.
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.3 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. For specific hazards associated with the use of this practicetest method, see Practices E 50.
2. Referenced Documents
2
2.1 ASTM Standards:
E50 Practices for Apparatus, Reagents, and Safety Precautions for Chemical Analysis of Metals, Ores, and Related Materials
Practices for Apparatus, Reagents, and Safety Considerations for Chemical Analysis of Metals, Ores, and Related Materials
E 135 Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
E 882 Guide for Accountability and Quality Control in the Chemical Analysis Laboratory
E 1184 Practice for Electrothermal (Graphite Furnace) Atomic Absorption Analysis
E1452Practice for Preparation of Calibration Solutions for Spectrophotometric and Spectroscopic Atomic Analysis
E 1601 Practice for Conducting an Interlaboratory Study to Evaluate the Performance of an Analytical Method
E 1770 Practice for Optimization of Electrothermal Atomic Absorption Spectrometric Equipment
2.2 ISO Standards:ISO Standard11437–NickelAlloys–Determination of Trace-Element Content–Electrothermal Atomic Ab-
3
sorption Spectrometric Method–Part 2: Determination of Lead Content
3
ISO Guide5725–Accuracy,Trueness, and Precision of Measurements, Methods and Results ISO Guide 5725:1986 Precision of
Test Methods — Determination of Repeatability and Reproducibility for a Standard Test Method by Inter-Laboratory Tests
ISO Standard 11437:1994 Nickel Alloys — Determination of Trace-Element Content — Electrothermal Atomic Absorption
Spectrometric Method–Part 2: Determination of Lead Content
3. Summary of Test Method
3.1The sample is dissolved in a mixture of nitric acid, hydrofluoric acid, and water. The sample and a nickel-ammonium
phosphate matrix modifier are injected into the electrothermal atomizer of an atomic absorption spectrometer, which is provided
with a background corrector. Measurement of the absorbance is made at a wavelength of 283.3 nm. The lead concentration is
determined from a calibration curve established with nickel solutions containing a known amount of lead. Terminology
3.1 Definitions—For definitions of terms used in this test method, refer to Terminology E 135.
1
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 Oct. 10, 1996. Published December 1996.
Current edition approved July 15, 2009. Published July 2009. Originally approved in 1996. Last previous edition approved in 2002 as E 1834 – 96 (2002).
2
For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM 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.
3
Available from American National Standards I
...

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