Título: | CELLULOSE SUBSTRATE ROOM-TEMPERATURE PHOSPHORIMETRY FOR THE DETERMINATION OF 2 METHYL INDOL E 7 METHYL INDOL: METHOD DEVELOPMENT, VALIDATION AND CRITICAL EVALUATION OF THE APPLICABILITY OF THE TECHNIQUE | |||||||
Autor: |
SELMA CUNHA MELLO |
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Colaborador(es): |
RICARDO QUEIROZ AUCELIO - Orientador |
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Catalogação: | 05/NOV/2008 | Língua(s): | PORTUGUESE - BRAZIL |
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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. |
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Referência(s): |
[pt] https://www.maxwell.vrac.puc-rio.br/projetosEspeciais/ETDs/consultas/conteudo.php?strSecao=resultado&nrSeq=12450&idi=1 [en] https://www.maxwell.vrac.puc-rio.br/projetosEspeciais/ETDs/consultas/conteudo.php?strSecao=resultado&nrSeq=12450&idi=2 |
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DOI: | https://doi.org/10.17771/PUCRio.acad.12450 | |||||||
Resumo: | ||||||||
In this work, room-temperature phosphorimetry using
cellulose substrates was evaluated as analytical technique
for the determination of two indol derivatives (2 methyl
indol and 7 methyl indol). The phosphorescence from both
analytes were studied in a univaried way in function of
several experimental parameters such as the phosphorescence
decay rate; type and quantity of phosphorescence inducer
(heavy atom salt); amount of surfactant used as
cellulose surface modifier and the influence of the
hidrogenionic concentration of the analyte carrier
solution. Once defined the relevant factors, central
composite designs were performed in order to obtain
response surfaces that pointed out possible interactions
among factors and lead to the best experimental conditions.
For 2 methyl indol, the best conditions were achieved by
using ethanol/water analyte carrier solution at its
original pH, and substrates containing TlNO3/SDS or
KI. Simillar conditions were found for 7 methyl indol. For
each of the selected conditions, studies were performed
aiming to find the analytical figures of merit
which included: selectivity, linearity of the working
range, limit of detection, limit of quantification,
accuracy, precision, robustness and the uncertainty of the
phosphorescence measurement from the solid substrate. In
all cases, the linear response presented a linear behavior
in function of the mass of the analytes placed on the
substrate [R(2) > 0,99]. Limits of detection (blank signals
average + 3sb) and limits of quantification (blank signals
average + 10sb) were in the mol L(-1) range (absolut values
of tenths of ng). The repeatability of the method presented
values between 15 and 23%, being the main components of the
phosphorescence measurement, which were calculated based on
the procedure indicated in the ISO GUM. The uncertainty
value was between 22 and 35% (combined uncertainty)
epending on the experimental condition and on the
analyte used in the calculation process. The selectivity
towards other indols (indol and 7 methyl indol) and other
classes of nitrogenated polycyclic aromatic compounds was
evaluated by comparing phosphorescence characteristics from
these substances. While no discrimination was possible for
the indols, selectivity in the determination of 2 methyl
indol and 7 methyl indol in the presence of acridine, 7,8
benzoquinoline and quinoline) was found.
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