ASTM E1184-10
(Practice)Standard Practice for Determination of Elements by Graphite Furnace Atomic Absorption Spectrometry
Standard Practice for Determination of Elements by Graphite Furnace Atomic Absorption Spectrometry
SIGNIFICANCE AND USE
This practice is intended for users who are attempting to establish GF-AAS procedures. It should be helpful for establishing a complete atomic absorption analysis program.
SCOPE
1.1 This practice covers a procedure for the determination of microgram per millilitre (μg/mL) or lower concentrations of elements in solution using a graphite furnace attached to an atomic absorption spectrometer. A general description of the equipment is provided. Recommendations are made for preparing the instrument for measurements, establishing optimum temperature conditions and other criteria which should result in determining a useful calibration concentration range, and measuring and calculating the test solution analyte concentration.
1.2 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.
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. Specific safety hazard statements are given in Section 9.
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Designation: E1184 − 10
StandardPractice for
Determination of Elements by Graphite Furnace Atomic
1
Absorption Spectrometry
This standard is issued under the fixed designation E1184; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber in parentheses indicates the year of last reapproval.A
superscript epsilon (´) indicates an editorial change since the last revision or reapproval.
1. Scope 3. Terminology
1.1 This practice covers a procedure for the determination 3.1 RefertoTerminologiesE131andE135forthedefinition
of terms used in this practice.
of microgram per millilitre (µg/mL) or lower concentrations of
elements in solution using a graphite furnace attached to an
3.2 Definitions of Terms Specific to This Standard:
atomic absorption spectrometer. A general description of the
3.2.1 atomization—the formation of ground state atoms that
equipment is provided. Recommendations are made for pre-
absorb radiation from a line emission source. The atomization
paring the instrument for measurements, establishing optimum
process in graphite furnace atomic absorption spectrometry
temperatureconditionsandothercriteriawhichshouldresultin
(GF-AAS) analysis is covered in 6.2.
determining a useful calibration concentration range, and
3.2.2 pyrolysis—the process of heating a specimen to a
measuring and calculating the test solution analyte concentra-
temperature high enough to remove or alter its original matrix,
tion.
butnotsohighastovolatilizetheelementtobemeasured.The
1.2 The values stated in SI units are to be regarded as
purpose of the pyrolysis step in GF-AAS analysis is to remove
standard. The values given in parentheses are for information
or alter the original specimen matrix, thereby reducing or
only.
eliminating possible interferences to the formation of ground
state atoms that are formed when the temperature is increased
1.3 This standard does not purport to address all of the
during the atomization step. Many publications and references
safety concerns, if any, associated with its use. It is the
will refer to pyrolysis as charring or ashing.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
3.2.3 pyrolytic graphite coating—alayerofpyrolyticgraph-
bility of regulatory limitations prior to use. Specific safety
ite that coats a graphite tube used in GF-AAS analysis.
hazard statements are given in Section 9.
Pyrolytic graphite is formed by pyrolizing a hydrocarbon, for
example, methane, at 2000°C.
2. Referenced Documents
3.2.4 ramping—a slow, controlled increase of the tempera-
2
2.1 ASTM Standards:
ture in the graphite tube. Ramping will provide for an efficient
E50Practices for Apparatus, Reagents, and Safety Consid-
but not too rapid removal or decomposition of the specimen
erations for Chemical Analysis of Metals, Ores, and
matrix. Most graphite furnaces allow for ramping during the
Related Materials
drying,pyrolysis,andatomizationsteps.Itisusuallyemployed
E131Terminology Relating to Molecular Spectroscopy
during the drying and pyrolysis steps. However, some instru-
E135Terminology Relating to Analytical Chemistry for
ment manufacturers may recommend ramping during the
Metals, Ores, and Related Materials
atomization step depending on the specimen matrix and the
E406Practice for Using Controlled Atmospheres in Spec-
elementbeingmeasured(forexample,theanalysisofcadmium
trochemical Analysis
or lead in hair or blood). The power supplies for most
D1193Specification for Reagent Water
instruments also allow the rate of the temperature increase to
be varied.
1
This practice is under the jurisdiction ofASTM Committee E01 on Analytical 4. Significance and Use
ChemistryforMetals,Ores,andRelatedMaterialsandisthedirectresponsibilityof
4.1 Thispracticeisintendedforuserswhoareattemptingto
Subcommittee E01.20 on Fundamental Practices.
establish GF-AAS procedures. It should be helpful for estab-
Current edition approved June 1, 2010. Published August 2010. Originally
approved in 1987. Last previous edition approved in 2002 as E1184–02. DOI:
lishing a complete atomic absorption analysis program.
10.1520/E1184-10.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
5. Theory of Atomic Absorption Spectrometry (AAS)
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
5.1 In flame atomic absorption spectrometry (Flame-AAS),
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. a test solution is aspirated into a flame through which passes
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
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E1184 − 10
r
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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:E1184–02 Designation:E1184–10
Standard Practice for
Electrothermal (Graphite Furnace) Atomic Absorption
AnalysisDetermination of Elements by Graphite Furnace
1
Atomic Absorption Spectrometry
This standard is issued under the fixed designation E1184; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber 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 practice covers a procedure for the determination of microgram per millilitre (µg/mL) or lower concentrations of
elements in solution using an electrothermal atomization device a graphite furnace attached to an atomic absorption
spectrophotometer.spectrometer.Ageneraldescriptionoftheequipmentisprovided.Recommendationsaremadeforpreparingthe
instrument for measurements, establishing optimum temperature conditions and other criteria which should result in determining
a useful calibration concentration range, and measuring and calculating the test solution analyte concentration.
1.2 The values stated in SI units are to be regarded as standard. The values given in parentheses are for information only.
1.3 This standard does not purport to address all of the safety problems,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.
NOTE1—This practice is a companion to Practice E663. .
2. Referenced Documents
2
2.1 ASTM Standards:
E50 PracticesforApparatus,Reagents,andSafetyConsiderationsforChemicalAnalysisofMetals,Ores,andRelatedMaterials
E131 Terminology Relating to Molecular Spectroscopy
E135 Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
E406 Practice for Using Controlled Atmospheres in Spectrochemical Analysis E416Practice for Planning and Safe Operation
of a Spectrochemical Laboratory
E663Practice for Flame Atomic Absorption Analysis
E863Practice for Describing Atomic Absorption Spectrometric Equipment
D1193 Specification for Reagent Water
3. Terminology
3.1Refer to Terminology
3.1 Refer to Terminologies E131 and E135 for the definition of terms used in this practice.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 atomization—the formation of ground state atoms that absorb radiation from a line emission source (see Practice E663).
source.The atomization process in electrothermal graphite furnace atomic absorption spectrometry (GF-AAS) analysis is covered
in greater detail in 6.2.
3.2.2 pyrolysis—the process of heating a specimen to a temperature high enough to remove or alter its original matrix, but not
sohighastovolatilizetheelementtobemeasured.ThepurposeofthepyrolysisstepinelectrothermalatomicabsorptionGF-AAS
analysis is to remove or alter the original specimen matrix, thereby reducing or eliminating possible interferences to the formation
of ground state atoms that are formed when the temperature is increased during the atomization step. Many publications and
references will refer to pyrolysis as charring or ashing. ashing.
3.2.3 pyrolytic graphite coating—a layer of pyrolytic graphite that coats a graphite tube used in electrothermal atomic
1
This practice is under the jurisdiction of ASTM Committee E01 on Analytical Chemistry for Metals, Ores, and Related Materials and is the direct responsibility of
Subcommittee E01.20 on Fundamental Practices.
CurrenteditionapprovedOct.10,2002.PublishedJune2003.Originallyapprovedin1987.Lastpreviouseditionapprovedin1998asE1184–98.DOI:10.1520/E1184-02.
Current edition approved June 1, 2010. Published August 2010. Originally approved in 1987. Last previous edition approved in 2002 as E1184–02. DOI:
10.1520/E1184-10.
2
ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,orcontactASTMCustomerServiceatservice@astm.org.For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
1
---------------------- Page: 1 ----------------------
E1184–10
absorption GF-AAS analysis. Pyrolytic graphite is formed by pyrolizing a hydrocarbon, for example, methane, at 2000°C.
3.2.4 ramping—a slow, controlled increase of the temperature in the gr
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