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ASTM E1508-12a(2019)

(Guide)

Standard Guide for Quantitative Analysis by Energy-Dispersive Spectroscopy

Standard Guide for Quantitative Analysis by Energy-Dispersive Spectroscopy

SIGNIFICANCE AND USE
5.1 This guide covers procedures for quantifying the elemental composition of phases in a microstructure. It includes both methods that use standards as well as standardless methods, and it discusses the precision and accuracy that one can expect from the technique. The guide applies to EDS with a solid-state X-ray detector used on an SEM or EPMA.  
5.2 EDS is a suitable technique for routine quantitative analysis of elements that are 1) heavier than or equal to sodium in atomic weight, 2) present in tenths of a percent or greater by weight, and 3) occupying a few cubic micrometres, or more, of the specimen. Elements of lower atomic number than sodium can be analyzed with either ultra-thin-window or windowless spectrometers, generally with less precision than is possible for heavier elements. Trace elements, defined as 2 can be analyzed but with lower precision compared with analyses of elements present in greater concentration.
SCOPE
1.1 This guide is intended to assist those using energy-dispersive spectroscopy (EDS) for quantitative analysis of materials with a scanning electron microscope (SEM) or electron probe microanalyzer (EPMA). It is not intended to substitute for a formal course of instruction, but rather to provide a guide to the capabilities and limitations of the technique and to its use. For a more detailed treatment of the subject, see Goldstein, et al. (1) This guide does not cover EDS with a transmission electron microscope (TEM).  
1.2 Units—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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.  
1.4 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
31-Oct-2019
ICS
71.040.50 - Physicochemical methods of analysis
Technical Committee
E04 - Metallography
Drafting Committee
E04.11 - X-Ray and Electron Metallography
Current Stage
Ref Project

Relations

Refers
ASTM E7-14 - Standard Terminology Relating to Metallography
Effective Date
01-Nov-2014
Refers
ASTM E7-15 - Standard Terminology Relating to Metallography
Effective Date
01-Jun-2015
Referred By
ASTM F628-23 - Standard Specification for Acrylonitrile-Butadiene-Styrene (ABS) Schedule 40 Plastic Drain, Waste, and Vent Pipe With a Cellular Core
Effective Date
01-Nov-2019
Referred By
ASTM E2142-08(2015) - Standard Test Methods for Rating and Classifying Inclusions in Steel Using the Scanning Electron Microscope
Effective Date
01-Nov-2019

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ASTM E1508-12a(2019) - Standard Guide for Quantitative Analysis by Energy-Dispersive SpectroscopyASTM E1508-12a(2019) - Standard Guide for Quantitative Analysis by Energy-Dispersive Spectroscopy
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ASTM E1508-12a(2019) - Standard Guide for Quantitative Analysis by Energy-Dispersive Spectroscopy
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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: E1508 − 12a (Reapproved 2019)
Standard Guide for
1
Quantitative Analysis by Energy-Dispersive Spectroscopy
This standard is issued under the fixed designation E1508; 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 E691 Practice for Conducting an Interlaboratory Study to
Determine the Precision of a Test Method
1.1 This guide is intended to assist those using energy-
dispersive spectroscopy (EDS) for quantitative analysis of
3. Terminology
materials with a scanning electron microscope (SEM) or
electron probe microanalyzer (EPMA). It is not intended to 3.1 Definitions—For definitions of terms used in this guide,
substitute for a formal course of instruction, but rather to
see Terminologies E7 and E673.
provide a guide to the capabilities and limitations of the
3.2 Definitions of Terms Specific to This Standard:
technique and to its use. For a more detailed treatment of the
3.2.1 accelerating voltage—the high voltage between the
subject,seeGoldstein,etal. (1)ThisguidedoesnotcoverEDS
cathode and the anode in the electron gun of an electron beam
with a transmission electron microscope (TEM).
instrument, such as an SEM or EPMA.
1.2 Units—The values stated in SI units are to be regarded
3.2.2 beam current—the current of the electron beam mea-
as standard. No other units of measurement are included in this
sured with a Faraday cup positioned near the specimen.
standard.
3.2.3 Bremsstrahlung—background X rays produced by in-
1.3 This standard does not purport to address all of the
elastic scattering (loss of energy) of the primary electron beam
safety concerns, if any, associated with its use. It is the
in the specimen. It covers a range of energies up to the energy
responsibility of the user of this standard to establish appro-
of the electron beam.
priate safety, health, and environmental practices and deter-
3.2.4 critical excitation voltage—the minimum voltage re-
mine the applicability of regulatory limitations prior to use.
quired to ionize an atom by ejecting an electron from a specific
1.4 This international standard was developed in accor-
electron shell.
dance with internationally recognized principles on standard-
3.2.5 dead time—the time during which the system will not
ization established in the Decision on Principles for the
process incoming X rays (real time less live time).
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
3.2.6 k-ratio—the ratio of background-subtracted X-ray in-
Barriers to Trade (TBT) Committee.
tensity in the unknown specimen to that of the standard.
3.2.7 live time—the time that the system is available to
2. Referenced Documents
detect incoming X rays.
2
2.1 ASTM Standards:
3.2.8 overvoltage—the ratio of accelerating voltage to the
E3 Guide for Preparation of Metallographic Specimens
critical excitation voltage for a particular X-ray line.
E7 Terminology Relating to Metallography
3.2.9 SDD (silicon drift detector)—An x-ray detector char-
E673 Terminology Relating to SurfaceAnalysis (Withdrawn
acterized by a pattern in the biasing electrodes which induces
3
2012)
generated electrons to move laterally (drift) to a small-area
anode for collection, resulting in greatly reduced capacitance
which to a first approximation does not depend on the active
1
ThisguideisunderthejurisdictionofASTMCommitteeE04onMetallography
area, in contrast to conventional detectors using flat-plate
and is the direct responsibility of Subcommittee E04.11 on X-Ray and Electron
electrodes. (2)
Metallography.
Current edition approved Nov. 1, 2019. Published November 2019. Originally 3.2.10 shaping time—a measure of the time it takes the
approved in 1993. Last previous edition approved in 2012 as E1508 – 12a. DOI:
amplifier to integrate the incoming charge; it depends on the
10.1520/E1508-12AR19.
time constant of the circuitry.
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
3.2.11 spectrum—the energy range of electromagnetic ra-
Standards volume information, refer to the standard’s Document Summary page on
diation produced by the method and, when graphically
the ASTM website.
3
displayed, is the relationship of X-ray counts detected to X-ray
The last approved version of this historical standard is referenced on
www.astm.org. energy.
Copyright © ASTM International, 100
...

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SCOPE
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3.1 Definitions given in Section 4 are intended for use in all standards on analytical chemistry for metals, ores, and related materials. The definitions should be used uniformly and consistently. The purpose of these definitions is to promote clear understanding and interpretation of the standards in which the terms are used.
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4.1 This practice covers all aspects of sampling and preparing steel and iron for chemical analysis as defined in Test Methods, Practices, and Definitions A751 and Specification A48/A48M. Such subjects as sampling location and the sampling of lots are defined.  
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1.1 This practice covers the sampling of all grades of steel, both cast and wrought, and all types (grades) of cast irons and blast furnace iron for chemical and spectrochemical determination of composition. This practice is similar to ISO 14284.  
1.2 This practice is divided into the following sections.    
Sections  
Requirements for Sampling and Sample Preparation  
6  
General  
6.1  
Sample  
6.2  
Selection of a Sample  
6.3  
Preparation of a Sample  
6.4  
Liquid Iron for Steelmaking and Pig Iron Production  
7  
General  
7.1  
Spoon Sampling  
7.2  
Probe Sampling  
7.3  
Preparation of a Sample for Analysis  
7.4  
Liquid Iron for Cast Iron Production  
8  
General  
8.1  
Spoon Sampling  
8.2  
Probe Sampling  
8.3  
Preparation of a Sample for Analysis  
8.4  
Sampling and Sample Preparation for the Determination of  
8.5  
Oxygen and Hydrogen  
Liquid Steel for Steel Production  
9  
General  
9.1  
Probe Sampling  
9.2  
Spoon Sampling  
9.3  
Preparation of a Sample for Analysis  
9.4  
Sampling and Sample Preparation for the Determination  
9.5  
of Oxygen  
Sampling and Sample Preparation for the Determination  
9.6  
of Hydrogen  
Pig Irons  
10  
General  
10.1  
Increment Sampling  
10.2  
Preparation of a Sample for Analysis  
10.3  
Cast Iron Products  
11  
General  
11.1  
Sampling and Sample Preparation  
11.2  
Sections  
Steel Products  
12  
General  
12.1  
Selection of a Laboratory Sample or a Sample for  
12.2  
Analysis from a Cast Product  
Selection of a Laboratory Sample or a Sample for  
12.3  
Analysis from a Wrought Product  
Preparation of a Sample for Analysis  
12.4  
Sampling of Leaded Steel  
12.5  
Sampling and Sample Preparation for the Determination  
12.6  
of Oxygen  
Sampling and Sample Preparation for the Determination  
12.7  
of Hydrogen  
Keywords  
13  
Annexes  
Sampling Probes for Use with Liquid Iron and Steel  
Annex A1  
Sampling Probes for Use with Liquid Steel for the  
Annex A2  
Determination of Hydrogen  
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5.1 Gamma-ray spectrometry is of use in identifying radionuclides and in making quantitative measurements. Use of a semiconductor detector is necessary for high-resolution measurements.  
5.2 Variation of the physical geometry of the sample and its relationship with the detector will produce both qualitative and quantitative variations in the gamma-ray spectrum. To adequately account for these geometry effects, calibrations are designed to duplicate all conditions including source-to-detector distance, sample shape and size, and sample matrix encountered when samples are measured.  
5.3 Since some spectrometry systems are calibrated at many discrete distances from the detector, a wide range of activity levels can be measured on the same detector. For high-level samples, extremely low-efficiency geometries may be used. Quantitative measurements can be made accurately and precisely when high activity level samples are placed at distances of 10 cm or more from the detector.  
5.4 Electronic problems, such as erroneous deadtime correction, loss of resolution, and random summing, may be avoided by keeping the gross count rate below 2000 counts per second (s–1) and also keeping the deadtime of the analyzer below 5 %. Total counting time is governed by the radioactivity of the sample, the detector to source distance and the acceptable Poisson counting uncertainty.
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1.1 This practice covers the measurement of gamma-ray emitting radionuclides in water by means of gamma-ray spectrometry. It is applicable to nuclides emitting gamma-rays with energies greater than 45 keV. For typical counting systems and sample types, activity levels of about 40 Bq are easily measured and sensitivities as low as 0.4 Bq are found for many nuclides. Count rates in excess of 2000 counts per second should be avoided because of electronic limitations. High count rate samples can be accommodated by dilution, by increasing the sample to detector distance, or by using digital signal processors.  
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1.4 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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ASTM E2867-14(2023)(Practice)
Standard Practice for Estimating Uncertainty of Test Results Derived from Spectrophotometry

SIGNIFICANCE AND USE
5.1 Many competent measurement laboratories comply with accepted quality system requirements such as ISO 9001, QS 9000, or ISO 17025. When using standard test methods, the measurement results should agree with those from other similar laboratories within the combined uncertainty limits of the laboratories’ measurement systems. It is for this reason that quality system requirements demand that a statement of the uncertainty of the test results accompany every test result.  
5.2 Preparation of uncertainty estimates is a requirement for laboratory certification under ISO 17025. This practice describes the procedures by which such uncertainty estimates may be calculated.
SCOPE
1.1 This practice describes a protocol to be utilized by measurement laboratories for estimating and reporting the uncertainty of a measurement result when the result is derived from a measurand that has been obtained by spectrophotometry.  
1.2 This practice is specifically limited to the reporting of uncertainty of color measurement results that are reported as color-differences in ΔE format, even though the measurement itself may be reported in other units such as percent reflectance or transmittance.  
1.3 The procedures defined here are not intended to be applicable to national standardizing laboratories or transfer laboratories.  
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.  
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.

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