The current world energy crisis had led to the need for alternative energy source, one of these
sources is the use of oil for the production of biodiesel using the transesterification process. This
in turn requires the full process understanding in order to efficiently and easily monitor and control
the transesterification reaction. In this work Transesterification reaction, using rapeseed oil and
ethanol as an esterifying agent with Sodium Hydroxide as a catalyst, was monitored using Fourier
Transform Infrared Spectroscopy (FTIR). This method was implemented as the analysis method
in an on-line manner.2-Dimensional Correlation Spectroscopy was used on samples taken directly
from the reaction mixture, in order to find regions of interest that directly correlate to the
concentration or percentage of parameters of interest including : Triglycerides, Monoglycerides,
Diglycerides, Fatty Acid Ethyl Esters, and Conversion. It was found that 2-Dimensional
Correlation Spectroscopy can be easily implemented and leads to promising results, and Fourier
Transform Infrared Spectroscopy was found to be reliable, with results within 5% error of the
reference method used (Gas Chromatography). Fourier Transform Infrared (FT-IR) Spectroscopy
with 2D-COS analysis was found to be quick, with the possibility of automation and would provide
a jump forward for large-scale process control in the Ethanolysis On-Line monitoring when
compared to classical Off-Line method.
Anotace v angličtině
The current world energy crisis had led to the need for alternative energy source, one of these
sources is the use of oil for the production of biodiesel using the transesterification process. This
in turn requires the full process understanding in order to efficiently and easily monitor and control
the transesterification reaction. In this work Transesterification reaction, using rapeseed oil and
ethanol as an esterifying agent with Sodium Hydroxide as a catalyst, was monitored using Fourier
Transform Infrared Spectroscopy (FTIR). This method was implemented as the analysis method
in an on-line manner.2-Dimensional Correlation Spectroscopy was used on samples taken directly
from the reaction mixture, in order to find regions of interest that directly correlate to the
concentration or percentage of parameters of interest including : Triglycerides, Monoglycerides,
Diglycerides, Fatty Acid Ethyl Esters, and Conversion. It was found that 2-Dimensional
Correlation Spectroscopy can be easily implemented and leads to promising results, and Fourier
Transform Infrared Spectroscopy was found to be reliable, with results within 5% error of the
reference method used (Gas Chromatography). Fourier Transform Infrared (FT-IR) Spectroscopy
with 2D-COS analysis was found to be quick, with the possibility of automation and would provide
a jump forward for large-scale process control in the Ethanolysis On-Line monitoring when
compared to classical Off-Line method.
The current world energy crisis had led to the need for alternative energy source, one of these
sources is the use of oil for the production of biodiesel using the transesterification process. This
in turn requires the full process understanding in order to efficiently and easily monitor and control
the transesterification reaction. In this work Transesterification reaction, using rapeseed oil and
ethanol as an esterifying agent with Sodium Hydroxide as a catalyst, was monitored using Fourier
Transform Infrared Spectroscopy (FTIR). This method was implemented as the analysis method
in an on-line manner.2-Dimensional Correlation Spectroscopy was used on samples taken directly
from the reaction mixture, in order to find regions of interest that directly correlate to the
concentration or percentage of parameters of interest including : Triglycerides, Monoglycerides,
Diglycerides, Fatty Acid Ethyl Esters, and Conversion. It was found that 2-Dimensional
Correlation Spectroscopy can be easily implemented and leads to promising results, and Fourier
Transform Infrared Spectroscopy was found to be reliable, with results within 5% error of the
reference method used (Gas Chromatography). Fourier Transform Infrared (FT-IR) Spectroscopy
with 2D-COS analysis was found to be quick, with the possibility of automation and would provide
a jump forward for large-scale process control in the Ethanolysis On-Line monitoring when
compared to classical Off-Line method.
Anotace v angličtině
The current world energy crisis had led to the need for alternative energy source, one of these
sources is the use of oil for the production of biodiesel using the transesterification process. This
in turn requires the full process understanding in order to efficiently and easily monitor and control
the transesterification reaction. In this work Transesterification reaction, using rapeseed oil and
ethanol as an esterifying agent with Sodium Hydroxide as a catalyst, was monitored using Fourier
Transform Infrared Spectroscopy (FTIR). This method was implemented as the analysis method
in an on-line manner.2-Dimensional Correlation Spectroscopy was used on samples taken directly
from the reaction mixture, in order to find regions of interest that directly correlate to the
concentration or percentage of parameters of interest including : Triglycerides, Monoglycerides,
Diglycerides, Fatty Acid Ethyl Esters, and Conversion. It was found that 2-Dimensional
Correlation Spectroscopy can be easily implemented and leads to promising results, and Fourier
Transform Infrared Spectroscopy was found to be reliable, with results within 5% error of the
reference method used (Gas Chromatography). Fourier Transform Infrared (FT-IR) Spectroscopy
with 2D-COS analysis was found to be quick, with the possibility of automation and would provide
a jump forward for large-scale process control in the Ethanolysis On-Line monitoring when
compared to classical Off-Line method.
Review current literature aimed at analytical monitoring of alcoholysis reaction (transesterification) of triglycerides. Focus especially at methods suitable for on-line analysis.
Monitor triglyceride ethanolysis reaction with chosen method(s), preferably in an on-line manner.
Evaluate performance of tested method(s) and perform basic validation against standard reference method – gas chromatographic determination of reaction mixture composition.
Critically evaluate gained results, discuss them and summarize in a form of Master thesis.
Zásady pro vypracování
Review current literature aimed at analytical monitoring of alcoholysis reaction (transesterification) of triglycerides. Focus especially at methods suitable for on-line analysis.
Monitor triglyceride ethanolysis reaction with chosen method(s), preferably in an on-line manner.
Evaluate performance of tested method(s) and perform basic validation against standard reference method – gas chromatographic determination of reaction mixture composition.
Critically evaluate gained results, discuss them and summarize in a form of Master thesis.
Seznam doporučené literatury
[1] Zagonel GF, Peralta-Zamora P, Ramos LP. Multivariate monitoring of soybean oil ethanolysis by FTIR. Talanta 2004;63:1021–5. https://doi.org/10.1016/j.talanta.2004.01.008.
[2] Mahamuni NN, Adewuyi YG. Fourier transform infrared spectroscopy (FTIR) method to monitor soy biodiesel and soybean oil in transesterification reactions, petrodiesel- biodiesel blends, and blend adulteration with soy oil. Energy and Fuels 2009;23:3773–82. https://doi.org/10.1021/ef900130m.
[3] Mwenge P, Seodigeng T. In situ Real-Time Multivariate Analysis of Methanolysis Monitoring of Sunflower Oil Using FTIR. Int J Chem Mol Eng 2020;14:136–48.
[4] Husár J, Pecha J, Šánek L. Development and validation of a simple and reliable alternative method for process monitoring and final product quality control during fatty acid ethyl esters production. Talanta 2021;235:122752. https://doi.org/10.1016/J.TALANTA.2021.122752.
[5] Knothe G, Krahl J, Van Gerpen JH. The Biodiesel Handbook. 2nd ed. Urbana, Ill.: AOCS Press, c2010, online (xiii, 501 p.). ISBN 9781615835843.
Seznam doporučené literatury
[1] Zagonel GF, Peralta-Zamora P, Ramos LP. Multivariate monitoring of soybean oil ethanolysis by FTIR. Talanta 2004;63:1021–5. https://doi.org/10.1016/j.talanta.2004.01.008.
[2] Mahamuni NN, Adewuyi YG. Fourier transform infrared spectroscopy (FTIR) method to monitor soy biodiesel and soybean oil in transesterification reactions, petrodiesel- biodiesel blends, and blend adulteration with soy oil. Energy and Fuels 2009;23:3773–82. https://doi.org/10.1021/ef900130m.
[3] Mwenge P, Seodigeng T. In situ Real-Time Multivariate Analysis of Methanolysis Monitoring of Sunflower Oil Using FTIR. Int J Chem Mol Eng 2020;14:136–48.
[4] Husár J, Pecha J, Šánek L. Development and validation of a simple and reliable alternative method for process monitoring and final product quality control during fatty acid ethyl esters production. Talanta 2021;235:122752. https://doi.org/10.1016/J.TALANTA.2021.122752.
[5] Knothe G, Krahl J, Van Gerpen JH. The Biodiesel Handbook. 2nd ed. Urbana, Ill.: AOCS Press, c2010, online (xiii, 501 p.). ISBN 9781615835843.
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External examiner´s questions:
1. The model reaction system was based on the rapeseed oil only. How much aplicable the obtained results are for the other fat systems?
2. The waste fats may contain different impurities. The spectral methods may be more sensitive to those impurities compared to chromatography. Could you comment on sensitivity of developed approach to impurities.
3. The random validation data are not specified. Were they selected as the random portion of the obtained bulk data or were they obtained of specific experiment (same or different conditions)?
4. The discussion around Fig. 27 compare the performance of raw and corrected data vs refreactive index method. Would the conclusion change, if the comparison was made vs the GC data?
After the presentation of the work by the student and after the evaluation of the student's answers to the opponent's questions, a discussion was held in which the student answered the additional questions of the committee members.
Additional questions: prof. Koutný: How sensitive is this method?
The student answered all questions excellently and without mistakes; after considering the suggestions of the supervisor and the opponent, the commission then decided on the overall evaluation of the oral defence.