- Gdansk University of Technology
Faculty of Chemistry
Department of Chemical and Process Engineering
G. Narutowicza 11/12 Str.
80-233 Gdansk - +48 347 28 10
- GBedit
Przegląd rodzajów chiralnych faz stacjonarnych oraz możliwości ich zastosowań w chromatografii cieczowej Streszczenie: Chromatograficzne rozdzielanie związków optycznie czynnych ma ogromne znaczenie nie tylko w przemyśle farmaceutycznym,... more
Przegląd rodzajów chiralnych faz stacjonarnych oraz możliwości ich zastosowań w chromatografii cieczowej Streszczenie: Chromatograficzne rozdzielanie związków optycznie czynnych ma ogromne znaczenie nie tylko w przemyśle farmaceutycznym, ale i agrochemicznym, a także w b adaniach naukowych różnego rodzaju. W niniejszym opracowaniu scharakteryzowano komercyjnie dostępne chiralne fazy stacjonarne na b azie, cyklodekstryn, polisacharydów, makrocyklicznych antyb iotyków, eterów koronowych, a także fazy proteinowe, ligandowymienne, jonowymienne oraz fazy typu Pirkle'a. Omówiono podstawowe właściwości fizyczne i chemiczne w/w faz stacjonarnych, przedstawiono przykładowe ich struktury, mechanizmy chiralnego rozpoznania oraz podstawowe zastosowania. Opisano również warunki chromatograficznego rozdzielania chiralnego dla wyb ranych farmaceutyków i pestycydów. Słowa kluczowe: chiralne rozdzielenie, chiralne fazy stacjonarne (CSP), chromatografia cieczowa(LC) Types of chiral stationary pha...
12:20-12:50 5. NOWE METODYKI OZNACZANIA DODATKÓW DO PALIW SILNIKOWYCH Z ZASTOSOWANIEM ROZDZIELANIA WIELOWYMIAROWEGO LC-GC P 24 IDENTYFIKACJA PRODUKTÓW ELEKTROCHEMICZNEGO ROZKŁADU CIECZY JONOWYCH ZA POMOCĄ TECHNIKI GC-MS Aleksandra... more
12:20-12:50 5. NOWE METODYKI OZNACZANIA DODATKÓW DO PALIW SILNIKOWYCH Z ZASTOSOWANIEM ROZDZIELANIA WIELOWYMIAROWEGO LC-GC P 24 IDENTYFIKACJA PRODUKTÓW ELEKTROCHEMICZNEGO ROZKŁADU CIECZY JONOWYCH ZA POMOCĄ TECHNIKI GC-MS Aleksandra FABIAŃSKA, Marek GOŁĘBIOWSKI, Piotr STEPNOWSKI, Ewa Maria SIEDLECKA P 25 METODY BADANIA CAŁKOWITEGO POTENCJAŁU ANTYOKSYDACYJNEGO PRODUKTÓW PSZCZELARSKICH Elwira LEWCZUK, Katarzyna CIOŁEK, Paweł M. WANTUSIAK, Paweł PISZCZ, Iwona KIERSZTYN, Bronisław K. GŁÓD, Paweł K. ZARZYCKI P 26 ZASTOSOWANIE TECHNIK HPLC-UV I LC-MS DO IDENTYFIKACJI PRODUKTÓW ELEKTROCHEMICZNEGO ROZKŁADU WYBRANYCH CIECZY JONOWYCH Aleksandra FABIAŃSKA, Marek GOŁĘBIOWSKI, Jadwiga WIŚNIEWSKA, Piotr STEPNOWSKI, Ewa Maria SIEDLECKA P 27 -i -CYKLODEKSTRYNY ROZPUSZCZONE W CIECZY JONOWEJ JAKO FAZY STACJONARNE W CHROMATOGRAFII GAZOWEJ Monika SOBÓTKA, Monika ASZTEMBORSKA, Janusz LIPKOWSKI P 28 OZNACZANIE AKTYWNOŚCI PRZECIWUTLENIAJĄCEJ OLEJÓW ROŚLINNYCH Piotr KOŚCIESZA, Rafał JURCZAK, Paweł PISZCZ, ...
W pracy przedstawiono oraz scharakteryzowano metody detekcji powszechnie wykorzystywane w chromatografii wykluczania (ang. Size Exclusion Chromatography, SEC), dawniej określanej termi¬nem chromatografia zelowa (ang. GelPermeation... more
W pracy przedstawiono oraz scharakteryzowano metody detekcji powszechnie wykorzystywane w chromatografii wykluczania (ang. Size Exclusion Chromatography, SEC), dawniej określanej termi¬nem chromatografia zelowa (ang. GelPermeation Chromatography, GPC). Chromatografia wykluczania umozliwia ustalanie masy cząsteczkowej, a takze określanie rozkladu masy cząsteczkowej rzeczywistych mieszanin. W tej odmianie chromatografii cieczowej związki zostają rozdzielone ze wzgledu na roznice wielkości promienia hydrodynamicznego cząsteczek analitow, co mozna skorelowac z ich masą czą¬steczkową. Cechą charakterystyczną tej techniki jest fakt, ze calkowite rozdzielenie ma miejsce w czasie nizszym, niz czas retencji substancji niezatrzymywanej (czas martwy). W idealnych warunkach SEC faza stacjonarna nie oddzialuje w zaden sposob ze skladnikami badanej probki. Detektory stosowane w SEC powinny charakteryzowac sie uniwersalnością i praktycznie stalym wspol-czynnikiem odpowiedzi detekcji wzgledem wszys...
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The paper presents the first application of deep eutectic solvents (DES) as stationary phases for gas chromatography. DES obtained by mixing tetrabutylammonium chloride (TBAC) as a hydrogen bond acceptor (HBA) with heptadecanoic acid... more
The paper presents the first application of deep eutectic solvents (DES) as stationary phases for gas chromatography. DES obtained by mixing tetrabutylammonium chloride (TBAC) as a hydrogen bond acceptor (HBA) with heptadecanoic acid being a hydrogen bond donor (HBD) in a mole ratio of HBA:HBD equal to 1:2 was characterized by its ability to separate volatile organic compounds (VOCs). The Rohrschneider - McReynolds constants determined reveal that the synthesized DES is a stationary phase of medium polarity. A detailed retention characteristic was determined for a number of groups of chemical compounds, including aromatic hydrocarbons, alcohols, ketones, sulfides and thiophene derivatives. The synthesized DES was found to have a high selectivity towards alcohols. At the same time, the investigated stationary phase was found to have specific interactions with some analytes. For example, a stronger retention was observed for 1-hexanol and 1-heptanol compared to other alcohols. Retention times of these two alcohols are longer by 191% and 300%, respectively, relative to the expected value based on their boiling point. Such an increased retention is caused by a synergistic effect of various kinds of interactions - the possibility of formation of hydrogen bonds between the DES and the hydroxyl group of alcohols and hydrophobic interactions of alkyl chains of the DES with the alkyl chain of alcohols. The ability to modify properties of DESs by replacement of HBA or HBD with a different chemical compound or by dissolving in DES macromolecular substances makes the proposed stationary phase highly flexible. In addition to using the developed DES in chromatographic techniques, the retention data collected indicate the possibility of its application to other separation techniques, i.e. extractive distillation.
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The paper presents an innovative, chemically modified (methylcyanated) asphaltene-based adsorbent that can be an interesting low-cost alternative for traditional adsorbents. Adsorption properties of adsorbents were examined by inverse gas... more
The paper presents an innovative, chemically modified (methylcyanated) asphaltene-based adsorbent that can be an interesting low-cost alternative for traditional adsorbents. Adsorption properties of adsorbents were examined by inverse gas chromatography technique, adsorption isotherms, and breakthrough curves. A significant increase in retention volume for pyridine, 2-pentanone, nitropropane, toluene, and 1-butanol was observed. Rohrschneider–McReynolds constants revealed an increase in strength of interactions as a result of the modification, especially in strong proton–acceptor interaction (by a factor of 4.6). The surface-free energy of asphaltene adsorbents increased from 136.71 to 169.95 mJ m−2 after modification. It is similar to the surface-free energy of silica or alumina. Moreover, modified adsorbent shows very high adsorption potential for pyridine. Adsorption isotherms revealed that monolayer adsorption capacity for pyridine increased 1.5 times after modification. Breakth...
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Cavitation has become on the most often applied methods in a number of industrial technologies. In the case of oxidation of organic pollutants occurring in the aqueous medium, cavitation forms the basis of numerous advanced oxidation... more
Cavitation has become on the most often applied methods in a number of industrial technologies. In the case of oxidation of organic pollutants occurring in the aqueous medium, cavitation forms the basis of numerous advanced oxidation processes (AOPs). This paper presents the results of investigations on the efficiency of oxidation of the following groups of organic compounds: organosulfur, nitro derivatives of benzene, BTEX, and phenol and its derivatives in a basic model effluent using hydrodynamic and acoustic cavitation combined with external oxidants, i.e., hydrogen peroxide, ozone and peroxone. The studies revealed that the combination of cavitation with additional oxidants allows 100% oxidation of the investigated model compounds. However, individual treatments differed with respect to the rate of degradation. Hydrodynamic cavitation aided by peroxone was found to be the most effective treatment (100% oxidation of all the investigated compounds in 60 min). When using hydrodyna...
The paper presents a new procedure for the determination of organic acids in a complex aqueous matrix using ultrasound-assisted dispersive liquid-liquid microextraction followed by injection port derivatization and GC-MS analysis. A deep... more
The paper presents a new procedure for the determination of organic acids in a complex aqueous matrix using ultrasound-assisted dispersive liquid-liquid microextraction followed by injection port derivatization and GC-MS analysis. A deep eutectic solvent (choline chloride: 4-methylphenol in a 1:2 mol ratio) was used both as an extracting solvent and as a derivatizing agent to yield ion pairs which were next converted to methyl esters of organic acids in a hot GC injection port. The procedure was optimized in terms of selection of a deep eutectic solvent, disperser solvent, and the ratio of their volumes, pH, salting out effect, extraction time, injection port temperature and time of opening the split valve. The developed procedure is characterized by low LOD (1.7-8.3 μg/L) and LOQ (5.1-25 μg/L) values, good repeatability (RSD ranging from 4.0 to 6.7%), good recoveries for most of the studied analyte (81,5-106%) and a wide linear range. The procedure was used for the determination of...
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We present a new procedure for the determination of oxygenated volatile organic compounds in samples of postoxidative effluents from the production of petroleum bitumens using dispersive liquid-liquid microextraction and gas... more
We present a new procedure for the determination of oxygenated volatile organic compounds in samples of postoxidative effluents from the production of petroleum bitumens using dispersive liquid-liquid microextraction and gas chromatography with mass spectrometry. The eight extraction parameters were optimized for 43 oxygenated volatile organic compounds. The detection limits obtained ranged from 0.07 to 0.82 μg/mL for most of the analytes, the precision was good (relative standard deviation below 2.91% at the 5 μg/mL level and 4.75% at the limit of quantification), the recoveries for the majority of compounds varied from 70.6 to 118.9%, and the linear range was wide, which demonstrates the usefulness of the procedure. The developed procedure was used for the determination of oxygenated volatile organic compounds in samples of raw postoxidative effluents and in effluents after chemical treatment. In total, 23 compounds at concentration levels from 0.37 to 32.95 μg/mL were identified ...
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We present a new procedure for the determination of 32 volatile organonitrogen compounds in samples of industrial effluents with a complex matrix. The procedure, based on dispersive liquid-liquid microextraction followed by gas... more
We present a new procedure for the determination of 32 volatile organonitrogen compounds in samples of industrial effluents with a complex matrix. The procedure, based on dispersive liquid-liquid microextraction followed by gas chromatography with nitrogen-phosphorus and mass spectrometric detection, was optimized and validated. Optimization of the extraction included the type of extraction and disperser solvent, disperser solvent volume, pH, salting out effect, extraction, and centrifugation time. The procedure based on nitrogen-phosphorus detection was found to be superior, having lower limits of detection (0.0067-2.29 μg/mL) and quantitation as well as a wider linear range. The developed procedure was applied to the determination of content of volatile organonitrogen compounds in samples of raw effluents from the production of bitumens in which 13 compounds were identified at concentrations ranging from 0.15 to 10.86 μg/mL and in samples of effluents treated by various chemical m...
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The paper presents a new procedure for the determination of oxygenated volatile organic compounds in postoxidative effluents from the production of petroleum asphalt using dynamic headspace coupled to gas chromatography-mass spectrometry... more
The paper presents a new procedure for the determination of oxygenated volatile organic compounds in postoxidative effluents from the production of petroleum asphalt using dynamic headspace coupled to gas chromatography-mass spectrometry in SIM mode.
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This paper describes application of high-performance gel permeation/size-exclusion chromatography (GPC/SEC) for the determination of content of polymer modifiers in modified road bitumens. The obtained results were compared with the... more
This paper describes application of high-performance gel permeation/size-exclusion chromatography (GPC/SEC) for the determination of content of polymer modifiers in modified road bitumens. The obtained results were compared with the measurements based on the procedure recommended by the American Association of State Highway and Transportation Officials, which employs Fourier transform mid-infrared spectroscopy. Two most commonly used modifiers of paving bitumens, namely, styrene–butadiene–styrene and styrene–butadiene copolymers as well as modified bitumens sampled from various streets in the city of Gdansk (Poland), were investigated. This work confirmed the ability of GPC/SEC to distinguish modified road bitumens from unmodified ones. The developed methodology is particularly important in quality control of modified bitumens, as well as in arbitration analysis when there is a suspicion that the amount of modifier added to bitumen was lowered or that the material does not meet the specifications concerning the modifier content. GRAPHICAL ABSTRACT
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The paper describes a new procedure for the determination of boiling point distribution of high-boiling petroleum fractions using size-exclusion chromatography with refractive index detection. Thus far, the determination of boiling range... more
The paper describes a new procedure for the determination of boiling point distribution of high-boiling petroleum fractions using size-exclusion chromatography with refractive index detection. Thus far, the determination of boiling range distribution by chromatography has been accomplished using simulated distillation with gas chromatography with flame ionization detection. This study revealed that in spite of substantial differences in the separation mechanism and the detection mode, the size-exclusion chromatography technique yields similar results for the determination of boiling point distribution compared with simulated distillation and novel empty column gas chromatography. The developed procedure using size-exclusion chromatography has a substantial applicability, especially for the determination of exact final boiling point values for high-boiling mixtures, for which a standard high-temperature simulated distillation would have to be used. In this case, the precision of fina...
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ABSTRACT This work presents the procedures for monitoring volatile organic compounds during treatment of industrial effluents. The investigation was carried out for a specific effluent—caustic effluent from bitumen production. The... more
ABSTRACT This work presents the procedures for monitoring volatile organic compounds during treatment of industrial effluents. The investigation was carried out for a specific effluent—caustic effluent from bitumen production. The developed procedures enable more detailed control of the effectiveness of wastewater treatment than standard procedures. Caustic effluents from bitumen production have a complex physicochemical form and consist of an emulsion of an organic phase in a strongly alkaline aqueous phase. The occurrence of an emulsified organic phase in the aqueous phase of the effluents results in their high toxicity toward the activated sludge of a refinery wastewater treatment plant as well as strong malodorousness. Interpretation of analytical results reveals that the effluents contain over 400 organic compounds among volatile organic compounds (VOCs) alone. Using the developed procedures, 114 of the VOCs were identified in raw postoxidative effluents. The procedures described in this work allow detailed identification of VOCs as well as the determination of distribution of their concentrations for individual classes of chemical compounds. Monitoring changes in content of individual classes of VOCs, including highly malodorous volatile sulfur compounds, as well as changes in total VOC content, provides more information on the processes taking place during wastewater treatment.
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The paper describes a new procedure for the determination of boiling point distribution of high-boiling petroleum fractions using size-exclusion chromatography with refractive index detection. Thus far, the determination of boiling range... more
The paper describes a new procedure for the determination of boiling point distribution of high-boiling petroleum fractions using size-exclusion chromatography with refractive index detection. Thus far, the determination of boiling range distribution by chromatography has been accomplished using simulated distillation with gas chromatography with flame ionization detection. This study revealed that in spite of substantial differences in the separation mechanism and the detection mode, the size-exclusion chromatography technique yields similar results for the determination of boiling point distribution compared with simulated distillation and novel empty column gas chromatography. The developed procedure using size-exclusion chromatography has a substantial applicability, especially for the determination of exact final boiling point values for high-boiling mixtures, for which a standard high-temperature simulated distillation would have to be used. In this case, the precision of fina...