Standard Practice for Using Controlled Atmospheres in Atomic Emission Spectrometry

SIGNIFICANCE AND USE
4.1 An increasing number of atomic emission spectrometers are equipped with enclosed excitation stands and plasmas which call for atmospheres other than ambient air. This practice is intended for users of such equipment.
SCOPE
1.1 This practice covers general recommendations relative to the use of gas shielding during and immediately prior to specimen excitation in atomic emission spectrochemical analysis. It describes the concept of excitation shielding, the means of introducing gases, and the variables involved with handling gases.  
1.2 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.  
1.3 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.

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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: E406 − 19
Standard Practice for
Using Controlled Atmospheres in Atomic Emission
1
Spectrometry
This standard is issued under the fixed designation E406; 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 which call for atmospheres other than ambient air. This
practice is intended for users of such equipment.
1.1 This practice covers general recommendations relative
to the use of gas shielding during and immediately prior to
5. Reference to this Practice in ASTM Standards
specimenexcitationinatomicemissionspectrochemicalanaly-
5.1 The inclusion of the following paragraph, or suitable
sis. It describes the concept of excitation shielding, the means
equivalent, in any ASTM spectrochemical method, preferably
of introducing gases, and the variables involved with handling
in the section on excitation, shall constitute due notification
gases.
that this practice shall be followed:
1.2 This standard does not purport to address all of the
X.1 Gas Handling—Store and introduce the gas as directed
safety concerns, if any, associated with its use. It is the
in Practice E406.
responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter- 6. Concepts of Excitation Shielding
mine the applicability of regulatory limitations prior to use.
6.1 Control of Excitation Reactions:
1.3 This international standard was developed in accor-
6.1.1 Nonequilibriumreactionsinvolvingvariableoxidation
dance with internationally recognized principles on standard-
rates and temperature gradients in the analytical gap produce
ization established in the Decision on Principles for the
spurious analytical results. The use of artificial gas mixtures
Development of International Standards, Guides and Recom-
can provide more positive control of excitation reactions than
mendations issued by the World Trade Organization Technical
is possible in air, although air alone is advantageous in some
Barriers to Trade (TBT) Committee.
instances.
6.1.2 Methods of introducing the gas require special con-
2. Referenced Documents
sideration.Temperature gradients in both the specimen and the
2
2.1 ASTM Standards:
excitationcolumncanbecontrolledbythecoolingeffectofthe
E135Terminology Relating to Analytical Chemistry for gasflow.Also,currentdensitycanbeincreasedbyconstricting
Metals, Ores, and Related Materials
the excitation column with a flow of gas.
6.1.3 Control of oxidation reactions is possible by employ-
3. Terminology
ing nonreactive or reducing atmospheres. For example, argon
can be used to preclude oxidation reactions during excitation.
3.1 For definitions of terms used in this practice, refer to
A gas may be selected for a particular reaction, such as
Terminology E135.
nitrogentoproducecyanogenbandsasameasureofthecarbon
content of a specimen. Oxygen is used in some instances to
4. Significance and Use
ensure complete oxidation or specimen consumption. In point-
4.1 Anincreasingnumberofatomicemissionspectrometers
to-planesparkanalysis,areducingatmospherecanbeprovided
are equipped with enclosed excitation stands and plasmas
by the use of carbon or graphite counter electrodes in combi-
3
nation with an inert gas or by the use of special circuit
4
parameters in ambient air.
1
This practice is under the jurisdiction ofASTM Committee E01 on Analytical
6.2 Effects of Controlled Atmospheres:
ChemistryforMetals,Ores,andRelatedMaterialsandisthedirectresponsibilityof
6.2.1 Numerous analytical advantages can be realized with
Subcommittee E01.20 on Fundamental Practices.
Current edition approved Oct. 1, 2019. Published October 2019. Originally
controlled atmospheres:
approved in 1970. Last previous edition approved in 2012 as E406–81(2012). DOI:
10.1520/E0406-19.
2 3
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Schreiber, T. P., and Majkowaki, R. F.,“Effect of Oxygen on Spark Excitation
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM and Spectral Character,” Spectrochimica Acta, Vol 15, 1959, p. 991.
4
Standards volume information, refer to the standard’s Document Summary page on Bartel, R., and Goldblatt, A., “The Direct Reading Spectrometric Analysis of
the ASTM website. Alloy Cast Iron,” Spectrochimica Acta, Vol 9, 1957, p. 227.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
1

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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: E406 − 81 (Reapproved 2012) E406 − 19
Standard Practice for
Using Controlled Atmospheres in Spectrochemical
1
AnalysisAtomic Emission Spectrometry
This standard is issued under the fixed designation E406; 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 practice covers general recommendations relative to the use of gas shielding during and immediately prior to specimen
excitation in opticalatomic emission spectrochemical analysis. It describes the concept of excitation shielding, the means of
introducing gases, and the variables involved with handling gases.
1.2 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.
1.3 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.
2. Referenced Documents
2
2.1 ASTM Standards:
E135 Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
3
E416 Practice for Planning and Safe Operation of a Spectrochemical Laboratory (Withdrawn 2005)
3. Terminology
3.1 For definitions of terms used in this practice, refer to Terminology E135.
4. Significance and Use
4.1 An increasing number of opticalatomic emission spectrometers are equipped with enclosed excitation stands and plasmas
which call for atmospheres other than ambient air. This practice is intended for users of such equipment.
5. Reference to this Practice in ASTM Standards
5.1 The inclusion of the following paragraph, or suitable equivalent, in any ASTM spectrochemical method, preferably in the
section on excitation, shall constitute due notification that this practice shall be followed:
X.1 Gas Handling—Store and introduce the gas in accordance withas directed in Practice E406.
6. Concepts of Excitation Shielding
6.1 Control of Excitation Reactions:
6.1.1 Nonequilibrium reactions involving variable oxidation rates and temperature gradients in the analytical gap produce
spurious analytical results. The use of artificial gas mixtures can provide more positive control of excitation reactions than is
possible in air, although air alone is advantageous in some instances.
6.1.2 Methods of introducing the gas require special consideration. Temperature gradients in both the specimen and the
excitation column can be controlled by the cooling effect of the gas flow. Also, current density can be increased by constricting
the excitation column with a flow of gas.
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.
Current edition approved Dec. 1, 2012Oct. 1, 2019. Published December 2012October 2019. Originally approved in 1970. Last previous edition approved in 20082012
as E406 – 81 (2008).E406–81(2012). DOI: 10.1520/E0406-81R12.10.1520/E0406-19.
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 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

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E406 − 19
6.1.3 Control of oxidation reactions is possible by employing nonreactive or reducing atmospheres. For example, argon can be
used to preclude oxidation reactions during excitation. A gas may be selected for a particular reaction, such as nitrogen to produce
cyanogen bands as a measure of the carbon content of a specimen. Oxygen is used in some instances to ensure complete oxidation
or specimen consumption. In point-to-plane spark analysis, a reducing atmosphere can be provided by the use of carbon or graphite
3 4
counter electrodes in combination with an inert gas
...

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