BRUNO TAPPIZ
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Resumo IPEN-doc 29563 Comparison of 238U mass fraction measured by ICP–MS and Instrumental Neutron Activation Analysis techniques2022 - TAPPIZ, BRUNO; SILVA, PAULO S.C. da; OSTERMANN, CAROLINE; LIMA, NICOLE P. de; ANDRADE, MARIANA N. de; BUSTILLOS, OSCAR V.Introduction: Uranium is an element present in ambient air, water, soil and rocks [1]. The most abundant natural radioisotope of this actinide (238U) produces in its chain decay the radionuclide 222Rn [2], which is a tracer for atmospheric mixing and transport model validations [3]. The 238U activity concentration in superficial soil samples is a crucial parameter for some 222Rn flux map modeling methodologies [4]. Methods: In this study, 18 superficial soil samples were analyzed. The content of 238U was assessed using two techniques: (i) by the comparative method of the Instrumental Neutron Activation Analysis (INAA) [5] and by ICP–MS (ELAN 6000, PerkinElmer) [6]. Certified Reference Materials (CRM) SRM 1646a Estuarine Sediment and USG STM–2 were used both as comparators in the INAA technique and to ensure quality control. The normality and homoscedasticity of the data were evaluated. Finally, the Mann- Whitney U test [7] was used to assess whether or not there is a significant difference (α = 0.05) between the two techniques. Results: The z-score was calculated to ensure quality control. Z-scores values was obtained by the Modified Horwitz Equation [8], which takes into account the order of magnitude of the content of the analyte and is independent of the CRM uncertainties, unavailable for the CRM used. The z-score values obtained (n = 3) for the radionuclide 238U were 0.5 for the CRM USG STM–2 and -0.4 for SRM 1646a. The z-scores obtained are smaller than 2 therefore they are considered satisfactory [9]. Regarding the statistical parameters of the comparison between the techniques, the normality (Shapiro Wilk) was not verified (p = 0.02 for ICP-MS and p = 0.03 for INAA). The p-value for the test for equal variances (F test) was 0.71 Mann-Whitney U test was used instead of Student’s test due to the non-verification of the normality parameter in the data. The p-value from the Mann-Whitney test (0.51) indicates that there is no significant difference between the 238U content measured by the two techniques. Conclusions: Statistical analysis showed that there is no significant difference between the 238U mass fraction measured by the ICP–MS and the INAA – comparative method. In the future, certified reference materials will also be assessed by ICP–MS in order to corroborate this statistical comparison from a metrological point of view.Artigo IPEN-doc 28203 Determination of 238-U and 232-Th in soil samples collected near the Amazon Tall Tower Observatory, Brazilian Amazon2021 - TAPPIZ, B.; SILVA, P.S.C.; CARVALHO, E.F.; BOTIA, S.; LINHARES, H.M.S.M.D.; OSTERMANN, C.K.; BUSTILLOS, O.V.Artigo IPEN-doc 27861 Expanded uncertainty assessment in fish samples analyzed by INAA and AAS2021 - TAPPIZ, BRUNO; MOREIRA, EDSON G.Measurement uncertainty was estimated following the EURACHEM guide (Quantifying Uncertainty in Analytical Measurement) for the elements As, Br, Cl, Co, Cr, Cs, Fe, K, Mg, Mn, Na, Rb, Sb, Se and Zn determined by In-strumental Neutron Activation Analysis (INAA) and for the elements Cd, Hg and Pb determined by Atomic Absorption Spectrometry (AAS) in the fillet of the most consumed fish species at São Paulo city, Brazil. INAA expanded uncertainties ranged from 1.0 to 21% and the main contributions were due the counting statistics of sample and pipetted standards. For AAS, expanded uncertainties ranged from 6.5 to 13% and the main contri-butions were associated to the calibration curves. Uncertainty results were compared with the standard devia-tions of the mass fraction in the fishes (n = 10). Due to the wide variability in the mass fraction in the analyzed fish tissues, explained by factors such gender, age, fat content and fishing location of the specimens of each spe-cies, standard deviations were greater than expanded uncertainties, which means that the natural variability of the elements determined is greater than the data dispersion associated with the analytical techniques. Hence the used techniques were adequate for the fish fillet samples analyses.Artigo IPEN-doc 26156 Measurement uncertainty evaluation in fish samples analyzed by INAA and AAS2019 - TAPPIZ, BRUNO; MOREIRA, EDSON G.Measurement uncertainty was estimated following the EURACHEM guide (Quantifying Uncertainty in Analytical Measurement) for the elements As, Br, Cl, Co, Cr, Cs, Fe, K, Mg, Mn, Na, Rb, Sb, Se and Zn determined by Instrumental Neutron Activation Analysis (INAA) and for the elements Cd, Hg and Pb determined by Atomic Absorption Spectrometry (AAS) in the fillet of the most consumed fish species at São Paulo city, Brazil. INAA expanded uncertainties ranged from 1.0 to 21% and the main contributions were due the counting statistics of sample and pipetted standards. For AAS, expanded uncertainties ranged from 6.5 to 13% and the main contributions were associated to the calibration curves. Uncertainty results were compared with the standard deviations of the mass fraction in the fishes (n = 10). Due to the wide variability in the mass fraction in the analyzed fish tissues, explained by factors such gender, age, fat content and fishing location of the specimens of each specie, standard deviations were greater than expanded uncertainties, which means that the natural variability of the elements determined is greater than the data dispersion associateDissertação IPEN-doc 25978 Determinação de contaminantes inorgânicos em pescados consumidos em São Paulo como contribuição à garantia da segurança alimentar2019 - TAPPIZ, BRUNOO consumo do pescado é importante para a saúde humana pelo fato desse alimento ser fonte de proteína de alta qualidade, vitaminas, nutrientes essenciais e dois ácidos poli-insaturados ômega-3. Entretanto, o pescado também pode apresentar risco à saúde humana se estiver contaminado por substâncias tóxicas. Visando avaliar o teor de elementos essenciais e tóxicos, foram utilizado as técnicas de Análise por Ativação Neutrônica e Espectrometria de Absorção Atômica na determinação dos elementos As, Br, Cd, Cl, Co, Cr, Cs, Fe, Hg, K, Mg, Mn, Na, Pb, Rb, Sb, Se e Zn nos tecidos comestíveis (filés) de seis pescados dentre os mais consumidos na cidade de São Paulo: corvina - Micropogonias furnieri (Desmarest, 1823); pescada - Cynoscion leiarchus (Cuvier, 1830); robalo - Centropomus undecimalis (Bloch, 1792); sardinha - Sardinella brasiliensis (Steindachner, 1879); anchova - Pomatomus saltatrix (Linnaeus, 1766) e tainha - Mugil liza (Valenciennes, 1836). Para validar os métodos analíticos utilizados em relação à exatidão, foram utilizados o índice z e o valor de HorRat em materiais de referência certificados analisados sob as mesmas condições das amostras. Os elementos Br, K e Na foram determinados por duas modalidades de irradiação e o teste-t de Student foi utilizado para verificar se havia ou não diferença significativa entre as técnicas. Na determinação dos elementos essenciais e potencialmente tóxicos, foi possível a construção de banco de dados para os elementos Br, Cl, Co, Cs, Fe, K, Mg, Mn, Na, Rb, Se e Zn para potenciais futuras discussões. Para avaliar se havia ou não risco à segurança alimentar, foram comparado os teores de As, Cd, Hg e Pb com a legislação vigente no Brasil e com valores internacionais. Em relação à segurança alimentar, para os contaminantes Cd e Pb foram obtidos teores abaixo de todos os limites técnicos usados neste trabalho. Para As, a maior parte deve estar na forma orgânica, portanto, a determinação de Hg se mostrou determinante. De forma geral, não haveria perigo no consumo da sardinha, pescada, tainha, corvina e robalo, enquanto que para a anchova foi inconclusivo.