Effects of Variations in Operating Conditions on the Precision and Accuracy of Standardless Elemental Analysis of Stainless Steel by SEM-EDS

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Main Author: Carlos M. Garzón
Format: Artículo científico
Language:en
Published: Universidad Nacional de Colombia 2023
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author Carlos M. Garzón
author_facet Carlos M. Garzón
contents Effects of Variations in Operating Conditions on the Precision and Accuracy of Standardless Elemental Analysis of Stainless Steel by SEM-EDS Carlos M. Garzón Juan P. Cruz Johan K. Noreña Eduar F. Pineda Juan S. Cachaya Ingeniería accuracy SDD detector elemental analysis Scanning electron microscopy energy dispersive spectroscopy It is a customary practice to carry out standardless elemental microanalysis by energy dispersive spectroscopy (EDS) under the very same operational conditions as those used for scanning electron microscope (SEM) imaging. In this article, EDS experiments were carried out with stainless steel (SS), varying the EDS testing operating conditions. The results showed that, if X-ray spectra are acquired under operating conditions that are very dissimilar to those optimized for microanalysis, both the detectability limit of minor species (Si, Mo, and Mn) and the uncertainty in the concentration of major alloying elements (Cr and Ni) are noticeably impaired. It was observed that, by improving the signal-to-noise (S-to-N) ratio (i.e., by increasing the accelerating voltage, beam intensity, and total acquisition time, or when the working distance is optimized), the precision of the elemental concentration increases, but the accuracy is only marginally affected. For the major alloying elements, 25% of the measurements showed a percent discrepancy higher than three times the standard deviation, which is inconsistent with a normal statistical distribution. 2023 artículo científico 0120-5609 https://www.redalyc.org/articulo.oa?id=64379907014 https://www.redalyc.org/journal/643/64379907014/ https://www.redalyc.org/journal/643/64379907014/html/ https://www.redalyc.org/journal/643/64379907014/64379907014.epub https://www.redalyc.org/journal/643/64379907014/movil 10.15446/ing.investig.94361 en http://www.redalyc.org/revista.oa?id=643 Ingeniería e Investigación application/pdf Universidad Nacional de Colombia Ingeniería e Investigación (Colombia) Num.1 Vol.43
format Artículo científico
id redalyc_64379907014
institution Redalyc
language en
publishDate 2023
publisher Universidad Nacional de Colombia
spellingShingle Effects of Variations in Operating Conditions on the Precision and Accuracy of Standardless Elemental Analysis of Stainless Steel by SEM-EDS
Carlos M. Garzón
Ingeniería
accuracy
SDD detector
elemental analysis
Scanning electron microscopy
energy dispersive spectroscopy
Effects of Variations in Operating Conditions on the Precision and Accuracy of Standardless Elemental Analysis of Stainless Steel by SEM-EDS Carlos M. Garzón Juan P. Cruz Johan K. Noreña Eduar F. Pineda Juan S. Cachaya Ingeniería accuracy SDD detector elemental analysis Scanning electron microscopy energy dispersive spectroscopy It is a customary practice to carry out standardless elemental microanalysis by energy dispersive spectroscopy (EDS) under the very same operational conditions as those used for scanning electron microscope (SEM) imaging. In this article, EDS experiments were carried out with stainless steel (SS), varying the EDS testing operating conditions. The results showed that, if X-ray spectra are acquired under operating conditions that are very dissimilar to those optimized for microanalysis, both the detectability limit of minor species (Si, Mo, and Mn) and the uncertainty in the concentration of major alloying elements (Cr and Ni) are noticeably impaired. It was observed that, by improving the signal-to-noise (S-to-N) ratio (i.e., by increasing the accelerating voltage, beam intensity, and total acquisition time, or when the working distance is optimized), the precision of the elemental concentration increases, but the accuracy is only marginally affected. For the major alloying elements, 25% of the measurements showed a percent discrepancy higher than three times the standard deviation, which is inconsistent with a normal statistical distribution. 2023 artículo científico 0120-5609 https://www.redalyc.org/articulo.oa?id=64379907014 https://www.redalyc.org/journal/643/64379907014/ https://www.redalyc.org/journal/643/64379907014/html/ https://www.redalyc.org/journal/643/64379907014/64379907014.epub https://www.redalyc.org/journal/643/64379907014/movil 10.15446/ing.investig.94361 en http://www.redalyc.org/revista.oa?id=643 Ingeniería e Investigación application/pdf Universidad Nacional de Colombia Ingeniería e Investigación (Colombia) Num.1 Vol.43
title Effects of Variations in Operating Conditions on the Precision and Accuracy of Standardless Elemental Analysis of Stainless Steel by SEM-EDS
topic Ingeniería
accuracy
SDD detector
elemental analysis
Scanning electron microscopy
energy dispersive spectroscopy
url https://www.redalyc.org/articulo.oa?id=64379907014
https://www.redalyc.org/journal/643/64379907014/
https://www.redalyc.org/journal/643/64379907014/html/
https://www.redalyc.org/journal/643/64379907014/64379907014.epub
https://www.redalyc.org/journal/643/64379907014/movil