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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Universidad Nacional de Colombia
2022-11-01
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Series: | Ingeniería e Investigación |
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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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publishDate | 2022-11-01 |
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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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