Standard Guide for Direct Current Plasma-Atomic Emission Spectrometry Analysis

SIGNIFICANCE AND USE
Analyses using DCP-AES require proper preparation of test solutions, accurate calibration, and control of analytical procedures. ASTM test methods that refer to this guide shall provide specifics on test solutions, calibration, and procedures.
DCP-AES analysis is primarily concerned with testing materials for compliance with specifications, but may range from qualitative estimations to umpire analysis. These may involve measuring major and minor constituents or trace impurities, or both. This guide suggests some approaches to these different analytical needs.
This guide assists analysts in developing new methods.
It is assumed that the users of this guide will be trained analysts capable of performing common laboratory procedures skillfully and safely. It is expected that the work will be performed in a properly equipped laboratory.
This guide does not purport to define all of the quality assurance parameters necessary for DCP-AES analysis. Analysts should ensure that proper quality assurance procedures are followed, especially those defined by the test method. Refer to Guide E 882.
SCOPE
1.1 This guide covers procedures for using a direct current plasma-atomic emission spectrometer (DCP-AES) to determine the concentration of elements in solution. Recommendations are provided for preparing and calibrating the instrument, assessing instrument performance, diagnosing and correcting for interferences, measuring test solutions, and calculating results. A method to correct for instrument drift is included.
1.2 This guide does not specify all the operating conditions for a DCP-AES because of the differences between models of these instruments. Analysts should follow instructions provided by the manufacturer of the particular instrument.
1.3 This guide does not attempt to specify in detail all of the hardware components and computer software of the instrument. It is assumed that the instrument, whether commercially available, modified, or custom built, will be capable of performing the analyses for which it is intended, and that the analyst has verified this before performing the analysis.
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 precautionary statements are given in Section 7.

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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:E1097–07
Standard Guide for
Direct Current Plasma-Atomic Emission Spectrometry
1
Analysis
This standard is issued under the fixed designation E1097; 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 E135 Terminology Relating to Analytical Chemistry for
Metals, Ores, and Related Materials
1.1 This guide covers procedures for using a direct current
E882 Guide for Accountability and Quality Control in the
plasma-atomic emission spectrometer (DCP-AES) to deter-
Chemical Analysis Laboratory
mine the concentration of elements in solution. Recommenda-
E1601 Practice for Conducting an Interlaboratory Study to
tionsareprovidedforpreparingandcalibratingtheinstrument,
Evaluate the Performance of an Analytical Method
assessing instrument performance, diagnosing and correcting
for interferences, measuring test solutions, and calculating
3. Terminology
results. A method to correct for instrument drift is included.
3.1 Definitions: For definitions of terms used in this guide,
1.2 This guide does not specify all the operating conditions
refer to Terminology E135.
for a DCP-AES because of the differences between models of
3.2 Definitions of Terms Specific to This Standard:
these instruments. Analysts should follow instructions pro-
3.2.1 background equivalent concentration (BEC), n—in
vided by the manufacturer of the particular instrument.
DCP-AES,theanalyteconcentrationwhosesignalisequivalent
1.3 Thisguidedoesnotattempttospecifyindetailallofthe
to the signal generated by the plasm and matrix at the analyte
hardware components and computer software of the instru-
line when the actual analyte concentration is zero.
ment. It is assumed that the instrument, whether commercially
3.2.2 detection limit (DL), n—in addition to the DLdefined
available, modified, or custom built, will be capable of per-
in Terminology E135, the following detection limits are
forming the analyses for which it is intended, and that the
described and used in this guide:
analyst has verified this before performing the analysis.
3.2.2.1 instrumental detection limit (IDL), n—in DCP-AES,
1.4 This standard does not purport to address all of the
the analyte concentration corresponding to three times the
safety concerns, if any, associated with its use. It is the
standarddeviationofthebackgroundnoisebeneaththeanalyte
responsibility of the user of this standard to establish appro-
line on a set of nine consecutive 10-s measurements of the
priate safety and health practices and determine the applica-
background intensity of the blank.
bility of regulatory limitations prior to use. Specific precau-
3.2.2.2 method detection limit (MDL), n—in DCP-AES, the
tionary statements are given in Section 7.
detection limit measured on the matrix blank.
2. Referenced Documents 3.2.3 equivalent analyte concentration, n—the apparent
2
concentration of an interfering element on an anlalyte.
2.1 ASTM Standards:
3.2.4 linear dynamic range, n—the concentration range
E29 Practice for Using Significant Digits in Test Data to
fromthelimitofquantificationtothehighestconcentrationthat
Determine Conformance with Specifications
remains within 610% of linearity based on lower concentra-
E50 Practices for Apparatus, Reagents, and Safety Consid-
tions.
erations for Chemical Analysis of Metals, Ores, and
3.2.5 limit of quantification (LOQ), n—the lowest concen-
Related Materials
tration at which the instrument can measure reliably with a
defined error and confidence level.
1
This guide is under the jurisdiction of ASTM Committee E01 on Analytical
3.2.6 sensitivity, n—theslopeoftheanalyticalcurve,which
Chemistry for Metals, Ores and Related Materials and is the direct responsibility of
is the ratio of the change in emission intensity to the change in
Subcommittee E01.20 on Fundamental Practices.
concentration.
Current edition approved Nov. 1, 2007. Published November 2007. Originally
approved in 1986. Last previous edition approved in 2003 as E1097–03. DOI:
4. Summary of Guide
10.1520/E1097-07.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
4.1 Direct current plasma-atomic emission spectrometers,
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
eithersimultaneousorsequential,measuretheconcentrationof
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. elements in solution. Samples, calibration and other solutions
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
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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:E1097–03 Designation:E1097–07
Standard Guide for
Direct Current Plasma-Atomic Emission Spectrometry
1
Analysis
This standard is issued under the fixed designation E1097; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope
1.1 This guide covers procedures for using a direct current argon plasma atomic plasma-atomic emission spectrometer
(DCP-AES) to determine the concentration of elements in solution. Recommendations are provided for preparing and calibrating
the instrument, assessing instrument performance, diagnosing and correcting for interferences, measuring test solutions, and
calculating results. A method to correct for instrument drift is included.
1.2 ThisguidedoesnotspecifyalltheoperatingconditionsforaDCP-AESbecauseofthedifferencesbetweenmodelsofthese
instruments. Analysts should follow instructions provided by the manufacturer of the particular instrument.
1.3 This guide does not attempt to specify in detail all of the hardware components and computer software of the instrument.
It is assumed that the instrument, whether commercially available, modified, or custom built, will be capable of performing the
analyses for which it is intended, and that the analyst has verified this before performing the analysis.
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 and health practices and determine the applicability of regulatory
limitations prior to use. Specific precautionary statements are given in Section 87.
2. Referenced Documents
2
2.1 ASTM Standards:
E29 Practice for Using Significant Digits in Test Data to Determine Conformance with Specifications
E50 Practices for Apparatus, Reagents, and Safety PrecautionsConsiderations for Chemical Analysis of Metals, Ores, and
Related Materials
E135 Terminology Relating to Analytical Chemistry for Metals, Ores, and Related Materials
E743Guide for Spectrochemical Laboratory Quality Assurance
E876Practice for Use of Statistics in the Evaluation of Spectrometric Data
E882 Guide for Accountability and Quality Control in the Chemical Analysis Laboratory
E1601Practice for Conducting an Interlaboratory Study to Evaluate the Performance of an Analytical Method
E1832PracticeforDescribingandSpecifyingaDirectCurrentPlasmaAtomicEmissionSpectrometer PracticeforConducting
an Interlaboratory Study to Evaluate the Performance of an Analytical Method
3. Terminology
3.1 Definitions: 3.1.1ForFor definitions of terms used in this guide, refer to Terminology E135.
3.2 Definitions of Terms Specific to this Guide: This Standard:
3.2.1 background equivalent concentration (BEC), n—in DCP-AES,theanalyteconcentrationwhosesignalisequivalenttothe
signal generated by the plasmaplasm and matrix at the analyte line when the actual analyte concentration is zero.
3.2.2 detection limit (DL), n—the smallest quantity detectable by the DCP. detection limit (DL), n—in addition to the DL
defined in Terminology E135, the following detection limits are described and used in this guide:
3.2.2.1 approximate detection limit (ADL), n—an estimated detection limit calculated from the background equivalent
concentration. instrumental detection limit (IDL), n— in DCP-AES, the analyte concentration corresponding to three times the
standard deviation of the background noise beneath the analyte line on a set of nine consecutive 10-s measurements of the
background intensity of the blank.
1
This guide is under the jurisdiction of ASTM Committee E01 on Analytical Chemistry for Metals, Ores,Ores and Related Materials and is the direct responsibility of
Subcommittee E01.20 on General Analytical Fundamental Practices.
CurrenteditionapprovedOct.Nov.1,2003.2007.PublishedDec.2003.November2007.OriginallypublishedasE-3ProposalP152.approvedin1986.Lastpreviousedition
approved in 19972003 as E1097–97.E1097–03.
2
ForreferencedASTMstandards,visittheASTMwebsite,www.astm.org,orcontactASTMCustomerServiceatservice@astm.org.For Annual Book ofASTM 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.
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