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Considerations and Influencing Parameters in EDS Microanalysis of Biogenic Hydroxyapatite

Calcium phosphates (CPs) used as biomaterials have been intensively studied in recent years. In most studies, the determination of the chemical composition is mandatory. Due to the versatility and possibilities of performing qualitative and quantitative compositional analyses, energy dispersive spec...

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Autores principales: Miculescu, Florin, Luță, Cristina, Constantinescu, Andreea Elena, Maidaniuc, Andreea, Mocanu, Aura-Cătălina, Miculescu, Marian, Voicu, Ștefan Ioan, Ciocan, Lucian Toma
Formato: Online Artículo Texto
Lenguaje:English
Publicado: MDPI 2020
Materias:
Acceso en línea:https://www.ncbi.nlm.nih.gov/pmc/articles/PMC7711801/
https://www.ncbi.nlm.nih.gov/pubmed/33203117
http://dx.doi.org/10.3390/jfb11040082
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author Miculescu, Florin
Luță, Cristina
Constantinescu, Andreea Elena
Maidaniuc, Andreea
Mocanu, Aura-Cătălina
Miculescu, Marian
Voicu, Ștefan Ioan
Ciocan, Lucian Toma
author_facet Miculescu, Florin
Luță, Cristina
Constantinescu, Andreea Elena
Maidaniuc, Andreea
Mocanu, Aura-Cătălina
Miculescu, Marian
Voicu, Ștefan Ioan
Ciocan, Lucian Toma
author_sort Miculescu, Florin
collection PubMed
description Calcium phosphates (CPs) used as biomaterials have been intensively studied in recent years. In most studies, the determination of the chemical composition is mandatory. Due to the versatility and possibilities of performing qualitative and quantitative compositional analyses, energy dispersive spectrometry (EDS) is a widely used technique in this regard. The range of calcium phosphates is very diverse, the first method of approximating the type of compound being EDS microanalysis, by assessing the atomic Ca/P ratio. The value of this ratio can be influenced by several factors correlated with instrumental parameters and analysed samples. This article highlights the influence of the electron beam acceleration voltage (1 kV–30 kV) and of the particle size of calcium phosphate powders on the EDS analysis results. The characterised powders were obtained from bovine bones heat-treated at 1200 °C for 2 h, which have been ground and granulometrically sorted by mechanical vibration. The granulometric sorting generated three types of samples, with particle sizes < 20 μm, < 40 μm and < 100 μm, respectively. These were morphologically and dimensionally analysed by scanning electron microscopy (SEM) and compositionally by EDS, after the spectrometer was calibrated with a standard reference material (SRM) from NIST (National Institute of Standards and Technology). The results showed that the adjusting of acceleration voltage and of the powder particle size significantly influences the spectrum profile and the results of EDS analyses, which can lead to an erroneous primary identification of the analysed calcium phosphate type.
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spelling pubmed-77118012020-12-04 Considerations and Influencing Parameters in EDS Microanalysis of Biogenic Hydroxyapatite Miculescu, Florin Luță, Cristina Constantinescu, Andreea Elena Maidaniuc, Andreea Mocanu, Aura-Cătălina Miculescu, Marian Voicu, Ștefan Ioan Ciocan, Lucian Toma J Funct Biomater Article Calcium phosphates (CPs) used as biomaterials have been intensively studied in recent years. In most studies, the determination of the chemical composition is mandatory. Due to the versatility and possibilities of performing qualitative and quantitative compositional analyses, energy dispersive spectrometry (EDS) is a widely used technique in this regard. The range of calcium phosphates is very diverse, the first method of approximating the type of compound being EDS microanalysis, by assessing the atomic Ca/P ratio. The value of this ratio can be influenced by several factors correlated with instrumental parameters and analysed samples. This article highlights the influence of the electron beam acceleration voltage (1 kV–30 kV) and of the particle size of calcium phosphate powders on the EDS analysis results. The characterised powders were obtained from bovine bones heat-treated at 1200 °C for 2 h, which have been ground and granulometrically sorted by mechanical vibration. The granulometric sorting generated three types of samples, with particle sizes < 20 μm, < 40 μm and < 100 μm, respectively. These were morphologically and dimensionally analysed by scanning electron microscopy (SEM) and compositionally by EDS, after the spectrometer was calibrated with a standard reference material (SRM) from NIST (National Institute of Standards and Technology). The results showed that the adjusting of acceleration voltage and of the powder particle size significantly influences the spectrum profile and the results of EDS analyses, which can lead to an erroneous primary identification of the analysed calcium phosphate type. MDPI 2020-11-15 /pmc/articles/PMC7711801/ /pubmed/33203117 http://dx.doi.org/10.3390/jfb11040082 Text en © 2020 by the authors. Licensee MDPI, Basel, Switzerland. This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY) license (http://creativecommons.org/licenses/by/4.0/).
spellingShingle Article
Miculescu, Florin
Luță, Cristina
Constantinescu, Andreea Elena
Maidaniuc, Andreea
Mocanu, Aura-Cătălina
Miculescu, Marian
Voicu, Ștefan Ioan
Ciocan, Lucian Toma
Considerations and Influencing Parameters in EDS Microanalysis of Biogenic Hydroxyapatite
title Considerations and Influencing Parameters in EDS Microanalysis of Biogenic Hydroxyapatite
title_full Considerations and Influencing Parameters in EDS Microanalysis of Biogenic Hydroxyapatite
title_fullStr Considerations and Influencing Parameters in EDS Microanalysis of Biogenic Hydroxyapatite
title_full_unstemmed Considerations and Influencing Parameters in EDS Microanalysis of Biogenic Hydroxyapatite
title_short Considerations and Influencing Parameters in EDS Microanalysis of Biogenic Hydroxyapatite
title_sort considerations and influencing parameters in eds microanalysis of biogenic hydroxyapatite
topic Article
url https://www.ncbi.nlm.nih.gov/pmc/articles/PMC7711801/
https://www.ncbi.nlm.nih.gov/pubmed/33203117
http://dx.doi.org/10.3390/jfb11040082
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