Título: | METHOD VALIDATION OF ZDDP QUANTIFICATION IN LUBRICATING OIL BY INFRARED SPECTROMETRY | ||||||||||||||||||||||||||||||||||||||||||||
Autor: |
VANESSA BREDER VALENTE ZANATTA |
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Colaborador(es): |
JOSE MARCUS DE OLIVEIRA GODOY - Orientador ROBERTA MIRANDA TEIXEIRA - Coorientador |
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Catalogação: | 19/JAN/2010 | 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=14998&idi=1 [en] https://www.maxwell.vrac.puc-rio.br/projetosEspeciais/ETDs/consultas/conteudo.php?strSecao=resultado&nrSeq=14998&idi=2 |
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DOI: | https://doi.org/10.17771/PUCRio.acad.14998 | ||||||||||||||||||||||||||||||||||||||||||||
Resumo: | |||||||||||||||||||||||||||||||||||||||||||||
This study aimed to develop and validate an analytical method for
determining the concentration of ZDDP in lubricating oils by infrared
spectrometry. We chose to express the concentration of ZDDP based on
phosphorus content, due to the need for comparison with analytical techniques
that determine the total of this element. The method was able to determine the
level of phosphorus by spectrometry in the infrared range from 0.0770 to 0.1500%
m/m, this represents around 0.96 to 1.87% m/m of the ZDDP additives studied.
Date was obtained with ten scans in absorbance in the range of wave number 1100
- 900 cm-1, resolution 0.5 cm-1, using zinc selenite cell (ZnSe) with 0.10 mm
optical path. The analytical curves were constructed using a linear regression by
the method of least squares. Real samples were analyzed and the results were
compared with those obtained by the technique of ICP-OES. Validation was
carried out evaluating the following parameters: specificity and selectivity,
working range, linear working range and linearity, sensitivity, accuracy and
tendency (bias), accuracy, robustness and uncertainty of measurement. Based on
the results were possible to use the methodology in quality control of products
whose formulation is composed of ZDDP. Statistical analysis showed that no
significant difference between the techniques studied (ICP-OES and IR),
considering the range and the products in question. We applied the Student t-test
to compare the certified value of the concentration of phosphorus of a MRC with
the values obtained using the proposed method. Statistical analysis of results
showed that no significant difference between the value of the concentration of
phosphorus and the certified value found.
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