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Optimization of experimental conditions for measurements of perfluorinated organic acids by GC
Ston, Martin ; Čabala, Radomír (advisor) ; Coufal, Pavel (referee)
Commercial software Pro ezGC was used for calculation of optimal temperature program for analysis of isobutylesters of perfluorinated organic acids (C6 - C12) by gas chromatography with flame ionization detector. Optimization was done with respect to the complete resolution of all peaks of analytes. The calculated temperature program was also applied to the analysis of substances of interest on GC-MS. The calculated and measured values have been compared. The measured resolutions were higher than the calculated ones in all cases. Keywords: perfluorinated organic acids, isobutylesters, peak resolution Subject words: gas chromatography, numerical optimization
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Testing and optimization of pressure modulator conditions for GCxGC analyses
Ston, Martin ; Čabala, Radomír (advisor) ; Jelínek, Ivan (referee)
Pulse (fluid) pressure modulator was constructed for comprehensive gas chromatography. Optimal conditions of its connection to the gas chromatograph with a flame ionization detector were found for the analysis of selected mixture of volatile solvents. Pressure interdependences in the system and relations between dimensions of modulator capillaries and columns have been evaluated with respect to the length of the modulation period and pulse duration. Two non-polar columns (15 m × 0.25 mm DB-5MS, 10 m × 0.15 mm CP-Sil 5 CB) of the same stationary phase were tested to compare the separation efficiency in the first dimension and the DB-5MS column was selected. The Supelcowax 10 columns of the lengths 1, 2 and 3 m were compared in the second dimension. It was found that using of 3 m length column lead to the extension of analysis time, however the increase in separation efficiency in the second dimension was very evident. The experimental measurements have shown that the selected parameters for the evaluation of the separation efficiency (the peak capacity and total resolution product) were inappropriate. Gasoline, kerosene and diesel fuel were analyzed as examples of real samples. Amount of added ethanol as a biofuel additive was determined in the gasoline sample. Pulse pressure modulator was modified...
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Development and optimization of a robust pressure modulator for multidimensional gas chromatography
Ston, Martin
Comprehensive gas chromatography (GC×GC) is a modern and advanced analytical method designed to separate very complex samples, when the separation efficiency of classical gas chromatography is not sufficient. GC×GC allows complete simultaneous analysis of a sample on two different columns, interconnected by special interface called the modulator. Three types of control units were set up and a robust pulse flow modulator (PFM) was developed in this work. PFM working parameters have been always optimized to allow combinations of columns with different sizes. Optimized PFM allows application of columns with 10-60 m length and 0.15-0.25 mm internal diameters for the first dimensions and with 1-10 m length and 0.25-0.32 mm internal diameters for the second dimension. For demonstration reasons, analyses of complex real samples, such as essential oils, oil derivatives and biological samples, were performed. PFM was compared with the commercial cryofocusation modulator Zoex for the selected column set and one sample (a mixture of volatile solvents) on a gas chromatograph equipped with both modulators. The average repeatability of retention times, expressed as a relative standard deviation, was approximately 2.0 % for PFM (cryofocusation about 0.5 %) and of the peak areas was approximately 3.5 %...
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Development and optimization of a robust pressure modulator for multidimensional gas chromatography
Ston, Martin
Comprehensive gas chromatography (GC×GC) is a modern and advanced analytical method designed to separate very complex samples, when the separation efficiency of classical gas chromatography is not sufficient. GC×GC allows complete simultaneous analysis of a sample on two different columns, interconnected by special interface called the modulator. Three types of control units were set up and a robust pulse flow modulator (PFM) was developed in this work. PFM working parameters have been always optimized to allow combinations of columns with different sizes. Optimized PFM allows application of columns with 10-60 m length and 0.15-0.25 mm internal diameters for the first dimensions and with 1-10 m length and 0.25-0.32 mm internal diameters for the second dimension. For demonstration reasons, analyses of complex real samples, such as essential oils, oil derivatives and biological samples, were performed. PFM was compared with the commercial cryofocusation modulator Zoex for the selected column set and one sample (a mixture of volatile solvents) on a gas chromatograph equipped with both modulators. The average repeatability of retention times, expressed as a relative standard deviation, was approximately 2.0 % for PFM (cryofocusation about 0.5 %) and of the peak areas was approximately 3.5 %...
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Development and optimization of a robust pressure modulator for multidimensional gas chromatography
Ston, Martin ; Čabala, Radomír (advisor) ; Ventura, Karel (referee) ; Jelínek, Ivan (referee)
Comprehensive gas chromatography (GC×GC) is a modern and advanced analytical method designed to separate very complex samples, when the separation efficiency of classical gas chromatography is not sufficient. GC×GC allows complete simultaneous analysis of a sample on two different columns, interconnected by special interface called the modulator. Three types of control units were set up and a robust pulse flow modulator (PFM) was developed in this work. PFM working parameters have been always optimized to allow combinations of columns with different sizes. Optimized PFM allows application of columns with 10-60 m length and 0.15-0.25 mm internal diameters for the first dimensions and with 1-10 m length and 0.25-0.32 mm internal diameters for the second dimension. For demonstration reasons, analyses of complex real samples, such as essential oils, oil derivatives and biological samples, were performed. PFM was compared with the commercial cryofocusation modulator Zoex for the selected column set and one sample (a mixture of volatile solvents) on a gas chromatograph equipped with both modulators. The average repeatability of retention times, expressed as a relative standard deviation, was approximately 2.0 % for PFM (cryofocusation about 0.5 %) and of the peak areas was approximately 3.5 %...
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Testing and optimization of pressure modulator conditions for GCxGC analyses
Ston, Martin ; Čabala, Radomír (advisor) ; Jelínek, Ivan (referee)
Pulse (fluid) pressure modulator was constructed for comprehensive gas chromatography. Optimal conditions of its connection to the gas chromatograph with a flame ionization detector were found for the analysis of selected mixture of volatile solvents. Pressure interdependences in the system and relations between dimensions of modulator capillaries and columns have been evaluated with respect to the length of the modulation period and pulse duration. Two non-polar columns (15 m × 0.25 mm DB-5MS, 10 m × 0.15 mm CP-Sil 5 CB) of the same stationary phase were tested to compare the separation efficiency in the first dimension and the DB-5MS column was selected. The Supelcowax 10 columns of the lengths 1, 2 and 3 m were compared in the second dimension. It was found that using of 3 m length column lead to the extension of analysis time, however the increase in separation efficiency in the second dimension was very evident. The experimental measurements have shown that the selected parameters for the evaluation of the separation efficiency (the peak capacity and total resolution product) were inappropriate. Gasoline, kerosene and diesel fuel were analyzed as examples of real samples. Amount of added ethanol as a biofuel additive was determined in the gasoline sample. Pulse pressure modulator was modified...
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Optimization of experimental conditions for measurements of perfluorinated organic acids by GC
Ston, Martin ; Coufal, Pavel (referee) ; Čabala, Radomír (advisor)
Commercial software Pro ezGC was used for calculation of optimal temperature program for analysis of isobutylesters of perfluorinated organic acids (C6 - C12) by gas chromatography with flame ionization detector. Optimization was done with respect to the complete resolution of all peaks of analytes. The calculated temperature program was also applied to the analysis of substances of interest on GC-MS. The calculated and measured values have been compared. The measured resolutions were higher than the calculated ones in all cases. Keywords: perfluorinated organic acids, isobutylesters, peak resolution Subject words: gas chromatography, numerical optimization
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