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Abstract(s)
O presente estágio tem como principal objetivo adquirir conhecimentos e experiência prática em processos de implementação e validação de metodologias analíticas, com aplicação à análise de Mercúrio por Espetrometria de massa acoplada a um Plasma Indutivo (ICP-MS), em matrizes de Água para Consumo Humano e Água Natural Doce, assente nos requisitos da Norma de Acreditação NP EN ISO/IEC 17025:2018. Este documento foi desenvolvido durante um período de dez meses de estágio curricular, entre Outubro de 2020 e Setembro de 2021, que decorreu no Laboratório da Águas do Norte S.A, no âmbito do Mestrado em Engenharia Química, ramo Qualidade, do Instituto Superior de Engenharia do Porto. Na metodologia de implementação e validação da análise ao mercúrio, assim como os resultados obtidos desta análise incluiu o estudo de interferências espetrais onde foram preparadas várias amostras com concentrações crescentes de cada interferente, e analisou-se em modo STD e em modo KED. Com as contagens obtidas representou-se graficamente o interferente/isótopo interferido. Após verificação experimental, concluise que o isótopo escolhido foi o 202 Hg. Em relação às interferências não espetrais, usouse a estratégia do padrão interno onde se realizou um estudo experimental para averiguar qual o padrão interno que é afetado de modo semelhante ao mercúrio. O padrão interno escolhido foi o ródio (Rh). Além do estudo da linearidade também foi feita a determinação da precisão, da exatidão e da incerteza expandida, de acordo com os procedimentos em vigor no laboratório Acreditado da Águas do Norte. O trabalho desenvolvido teve em vista a Acreditação desta análise. Por fim, o processo de implementação e validação foi concluído com sucesso uma vez que todos os requisitos da matriz de validação foram cumpridos, ou seja, encontramse dentro dos parâmetros legislados pela Decreto-Lei nº 306/2007 de 27 de agosto alterado pelo Decreto-Lei nº 152/2017 de 7 de dezembro.
The present internship has the main goal of acquiring knowledge and practical experience in processes of implementation and validation of analytical methodology, with the application of Mercury analysis via Inductively coupled plasma mass spectrometry (ICP-MS), in matrices of Water for Human Consumption and Natural Fresh Water, within the demands of the NP EN ISO/IEC 17025:2018 Accreditation Norm. This document was developed over a ten-month curricular internship, between October 2020 and September 2021, which was undertaken in the Águas do Norte S.A company, towards the Master of Chemical Engineering, Quality field, in Porto's Higher Institute of Engineering. In the mercury's analysis implementation and validation methodology, as well as the results obtained from this analysis, the study of spectral interferences was included, where several samples with growing concentrations of each interferant were prepared and analyzed in STD and KED modes. With the counts obtained, the interfered interferent/isotope was graphically represented. Following experimental verification, it was concluded that the chosen isotope was the 202 Hg. Regarding the non-spectral interferences, the internal standard strategy was used, where an experimental study to determine which internal standard is affected in a similar way to mercury was conducted. The internal standard chosen was rhodium. Besides the linearity study, the determination of the precision, accuracy and expanded uncertainty were also determined, according to the procedures in force in the Aguas do Norte Accredited laboratory. The work developed aimed for the Accreditation of this analysis. Finally, the methodology of implementation and validation was successfully concluded seeing that all validation matrices requisites were completed, that is, are within the legislated parameters under the Decree-Law nº 306/2007 of August 27th, altered by the Decree-Law nº 152/2017 of December 7th .
The present internship has the main goal of acquiring knowledge and practical experience in processes of implementation and validation of analytical methodology, with the application of Mercury analysis via Inductively coupled plasma mass spectrometry (ICP-MS), in matrices of Water for Human Consumption and Natural Fresh Water, within the demands of the NP EN ISO/IEC 17025:2018 Accreditation Norm. This document was developed over a ten-month curricular internship, between October 2020 and September 2021, which was undertaken in the Águas do Norte S.A company, towards the Master of Chemical Engineering, Quality field, in Porto's Higher Institute of Engineering. In the mercury's analysis implementation and validation methodology, as well as the results obtained from this analysis, the study of spectral interferences was included, where several samples with growing concentrations of each interferant were prepared and analyzed in STD and KED modes. With the counts obtained, the interfered interferent/isotope was graphically represented. Following experimental verification, it was concluded that the chosen isotope was the 202 Hg. Regarding the non-spectral interferences, the internal standard strategy was used, where an experimental study to determine which internal standard is affected in a similar way to mercury was conducted. The internal standard chosen was rhodium. Besides the linearity study, the determination of the precision, accuracy and expanded uncertainty were also determined, according to the procedures in force in the Aguas do Norte Accredited laboratory. The work developed aimed for the Accreditation of this analysis. Finally, the methodology of implementation and validation was successfully concluded seeing that all validation matrices requisites were completed, that is, are within the legislated parameters under the Decree-Law nº 306/2007 of August 27th, altered by the Decree-Law nº 152/2017 of December 7th .
Description
Keywords
Mercúrio ICP-MS Água consumo humano e natural doce Implementação e validação de métodos de análise química Mercury ICP-MS Water for Human Consumption and Natural Fresh Water Implementation and validation of analytical methodology