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ETDs @PUC-Rio
Estatística
Título: EVALUATION OF ANALYTICAL STRATEGIES FOR ELEMENTAL DETERMINATION IN BIODIESEL BY INDUCTIVELY COUPLED PLASMA OPTICAL EMISSION SPECTROMETRY (ICP OES)
Autor: VITOR CORNAQUI PEREIRA MARROCOS
Colaborador(es): TATIANA DILLENBURG SAINT PIERRE - Orientador
JEFFERSON RODRIGUES DE SOUZA - Coorientador
Catalogação: 09/SET/2024 Língua(s): PORTUGUESE - BRAZIL
Tipo: TEXT Subtipo: THESIS
Notas: [pt] Todos os dados constantes dos documentos são de inteira responsabilidade de seus autores. Os dados utilizados nas descrições dos documentos estão em conformidade com os sistemas da administração da PUC-Rio.
[en] All data contained in the documents are the sole responsibility of the authors. The data used in the descriptions of the documents are in conformity with the systems of the administration of PUC-Rio.
Referência(s): [pt] https://www.maxwell.vrac.puc-rio.br/projetosEspeciais/ETDs/consultas/conteudo.php?strSecao=resultado&nrSeq=67908&idi=1
[en] https://www.maxwell.vrac.puc-rio.br/projetosEspeciais/ETDs/consultas/conteudo.php?strSecao=resultado&nrSeq=67908&idi=2
DOI: https://doi.org/10.17771/PUCRio.acad.67908
Resumo:
Direct introduction of organic solvents into inductively coupled plasma (ICP) spectrometers represents a limitation to reliability of the results due to matrix effects. Different calibration methods, such as Standard Dilution Analysis (SDA) and Multi-energy Calibration (MEC) have been proposed to overcome this kind of interference, reducing analysis time, reagent consumption and waste generation. In SDA with two internal standards (IS), the signal is acquired over time during the mixing process of two analytical solutions: one consisting of 50 percent of sample + 50 percent of analytical standards and IS1 (S1) and the other consisting of 50 percent of sample + 50 percent of blank solution and IS2 (S2). In MEC calibration, which also uses two solutions similarly to SDA, but without IS, signals from the elements are measured simultaneously at different wavelengths. These methods were applied to the determination of Ca, K, Mg, Na, P, Si and S in biodiesel samples diluted in xylene by inductively coupled plasma optical emission spectrometry (ICP OES) and compared to calibrations by standard addition (SA) and internal standardization (IS). Limits of quantification showed no statistically significant difference compared to the traditional methods, whereas the limits found by SDA ranged from 0.05 mg kg-1 (Ca) to 1.4 mg kg-1 (Na) for SDA, and from 0.01 mg kg-1 (Mg) to 0.98 mg kg-1 (P) for MEC. The trueness was verified through recovery tests on biodiesel samples and the standard reference material NIST 1084a (Wear metals in lubricating oil), with recoveries of 101 ± 6 percent for SDA and 108 ± 8 percent for MEC. Long-term signal stability and lower economic and environmental impacts places SDA and MEC as an interesting strategy for elemental determination in biodiesel and oil samples diluted in xylene.
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