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

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), v...

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Main Authors: Carlos M. Garzón, Juan P.N. Cruz, Johan K. Noreña, Eduar F. Pineda, Juan S. Cachaya
Format: Article
Language:English
Published: Universidad Nacional de Colombia 2022-11-01
Series:Ingeniería e Investigación
Subjects:
Online Access:https://revistas.unal.edu.co/index.php/ingeinv/article/view/94361
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author Carlos M. Garzón
Juan P.N. Cruz
Johan K. Noreña
Eduar F. Pineda
Juan S. Cachaya
author_facet Carlos M. Garzón
Juan P.N. Cruz
Johan K. Noreña
Eduar F. Pineda
Juan S. Cachaya
author_sort Carlos M. Garzón
collection DOAJ
description 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.
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spelling doaj.art-619bff5ef8b643bdb0b0a4e240c80ac12023-02-16T01:05:09ZengUniversidad Nacional de ColombiaIngeniería e Investigación0120-56092248-87232022-11-01431e94361e9436110.15446/ing.investig.9436176529Effects of Variations in Operating Conditions on the Preci-sion and Accuracy of Standardless Elemental Analysis of Stainless Steel by SEM-EDSCarlos M. Garzón0https://orcid.org/0000-0001-9429-5433Juan P.N. Cruz1https://orcid.org/0000-0001-9734-9345Johan K. Noreña2https://orcid.org/0000-0002-7961-9054Eduar F. Pineda3https://orcid.org/0000-0001-5098-3541Juan S. Cachaya4https://orcid.org/0000-0002-2734-727XUniversidad Nacional de ColombiaUniversidad Nacional de ColombiaUniversidad Nacional de ColombiaUniversidad Nacional de ColombiaUniversidad Nacional de ColombiaIt 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.https://revistas.unal.edu.co/index.php/ingeinv/article/view/94361scanning electron microscopyenergy dispersive spectroscopysdd detectorelemental analysisaccuracy
spellingShingle Carlos M. Garzón
Juan P.N. Cruz
Johan K. Noreña
Eduar F. Pineda
Juan S. Cachaya
Effects of Variations in Operating Conditions on the Preci-sion and Accuracy of Standardless Elemental Analysis of Stainless Steel by SEM-EDS
Ingeniería e Investigación
scanning electron microscopy
energy dispersive spectroscopy
sdd detector
elemental analysis
accuracy
title Effects of Variations in Operating Conditions on the Preci-sion and Accuracy of Standardless Elemental Analysis of Stainless Steel by SEM-EDS
title_full Effects of Variations in Operating Conditions on the Preci-sion and Accuracy of Standardless Elemental Analysis of Stainless Steel by SEM-EDS
title_fullStr Effects of Variations in Operating Conditions on the Preci-sion and Accuracy of Standardless Elemental Analysis of Stainless Steel by SEM-EDS
title_full_unstemmed Effects of Variations in Operating Conditions on the Preci-sion and Accuracy of Standardless Elemental Analysis of Stainless Steel by SEM-EDS
title_short Effects of Variations in Operating Conditions on the Preci-sion and Accuracy of Standardless Elemental Analysis of Stainless Steel by SEM-EDS
title_sort effects of variations in operating conditions on the preci sion and accuracy of standardless elemental analysis of stainless steel by sem eds
topic scanning electron microscopy
energy dispersive spectroscopy
sdd detector
elemental analysis
accuracy
url https://revistas.unal.edu.co/index.php/ingeinv/article/view/94361
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