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Zenon Lukaszewski - One of the best experts on this subject based on the ideXlab platform.
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bacterial strains isolated from river water having the ability to split Alcohol Ethoxylates by central fission
Environmental Science and Pollution Research, 2016Co-Authors: Irena Budnik, Joanna Zembrzuska, Zenon LukaszewskiAbstract:Alcohol Ethoxylates (AE) are a major component of the surfactant stream discharged into surface water. The “central fission” of AE with the formation of poly(ethylene glycols) (PEG) is considered to be the dominant biodegradation pathway. However, information as to which bacterial strains are able to perform this reaction is very limited. The aim of this work was to establish whether such an ability is unique or common, and which bacterial strains are able to split AE used as a sole source of organic carbon. Four bacterial strains were isolated from river water and were identified on the basis of phylogenetic trees as Enterobacter strain Z2, Enterobacter strain Z3, Citrobacter freundii strain Z4, and Stenotrophomonas strain Z5. Sterilized river water and “artificial sewage” were used for augmentation of the isolated bacteria. The test was performed in bottles filled with a mineral salt medium spiked with surfactant C12E10 (10 mg L−1) and an inoculating suspension of the investigated bacterial strain. Sequential extraction of the tested samples by ethyl acetate and chloroform was used for separation of PEG from the water matrix. LC–MS was used for PEG determination on the basis of single-ion chromatograms. All four selected and investigated bacterial strains exhibit the ability to split fatty Alcohol Ethoxylates with the production of PEG, which is evidence that this property is a common one rather than specific to certain bacterial strains. However, this ability increases in the sequence: Stenotrophomonas strain Z5 < Enterobacter strain Z2 < Enterobacter strain Z3 = Citrobacter freundii strain Z4.
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separation and determination of homogenous fatty Alcohol Ethoxylates by liquid chromatography with mulitstage mass spectrometry
Journal of Separation Science, 2014Co-Authors: Joanna Zembrzuska, Irena Budnik, Zenon LukaszewskiAbstract:Alcohol Ethoxylates (AEs) are a significant component of a stream of surfactants directed to the aquatic environment. The aim of this work was the investigation of the dependence of the analytical signals of homogeneous AE homologues on liquid chromatography with tandem mass spectrometry conditions, as well as the separation of AEs from the water matrix and, on this basis, the development of an analytical procedure suitable for the determination of AEs in environmental samples. Homogeneous homologues containing dodecyl moiety and 2–9 oxyethylene subunits were investigated. The analytical signals of the investigated homologues were optimized in terms of concentration of ammonium acetate in the mobile phase (optimum 5 mM) and a column temperature (optimum 35°C) of the liquid chromatography with tandem mass spectrometry system. A separation of AEs from the water matrix by liquid–liquid extraction (ethyl acetate, chloroform) or solid-phase extraction (C18, styrene divinylbenzene, H-RX) was investigated. In a model investigation, the best recoveries (>90%) were obtained with a styrene divinylbenzene cartridge eluted with a 1:1 mixture of chloroform and methanol. However, much worse recoveries were obtained from the river water sample. Better results were obtained for liquid–liquid extraction with ethyl acetate. Recoveries of 62–80% were obtained for homologues having 4–9 oxyethylene subunits, at the lowest spike.
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biodegradation of oxo Alcohol Ethoxylates in the continuous flow activated sludge simulation test
Water Research, 2002Co-Authors: Andrzej Szymanski, Bogdan Wyrwas, Ewa Bubien, Tatiana Kurosz, Wieslaw Hreczuch, Wlodzimierz Zembrzuski, Zenon LukaszewskiAbstract:Abstract Biodegradation of two α -methyl branched oxo-Alcohol Ethoxylates (OAE) of different polydispersity: LIAL 125/14 BRD (LIALB) (broad M.W. distribution) and LIAL 125/14 NRD (LIALN) (narrow M.W. distribution), both having an average of 14 oxyethylene subunits (EO) and a C 12–15 alkyl moiety were tested under the continuous flow activated sludge conditions of the classical Husmann plant. Primary biodegradation and concentration of metabolites: free oxo-Alcohol fraction (FOA) and poly(ethylene glycols) (PEG), were measured. PEG were divided into two fractions: short-chained PEG (PEGshch) (1–4 EO) and long-chained PEG (PEGlch)(>4 EO). The indirect tensammetric technique combined with an adequate separation was used for analysis. Central fission was found to be a highly dominating pathway, as is the case with fatty Alcohol Ethoxylates. OAE are highly primarily biodegraded (above 95%). High concentrations of FOA and PEG are formed. Once formed the PEGlch are further fragmented into the PEGshch. Free Alcohol fraction compounds are biodegraded sooner when alkyl moiety is shorter. OAE polydispersity has an influence on the kinetics of biodegradation; PEG formed from LIALN are biodegraded slower and to a lower degree than those from LIALB.
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biodegradation of fatty Alcohol Ethoxylates in the continuous flow activated sludge test
Water Research, 2000Co-Authors: Andrzej Szymanski, Bogdan Wyrwas, Zbigniew Swit, Tymoteusz Jaroszynski, Zenon LukaszewskiAbstract:Abstract Biodegradation of two fatty Alcohol Ethoxylates: surfactant C12E10 (C 12 with an average 10 oxyethylene subunits (EO)) and Marlipal 1618/25 (C 16–18 with an average 25 EO) were tested under the continuous flow activated sludge conditions of the classical Husmann plant and a plant having a denitrifying chamber. Primary biodegradation and concentration of metabolites: free fatty Alcohol (FFA) and poly(ethylene glycols) (PEG) were measured. PEG were divided into two fractions: short-chained (1–3 EO) and long-chained PEG (>3 EO). Tensammetric methods were used for analysis. High primary biodegradation was found (96.8±0.5% for surfactant C12E10 (C12E10) and 99.6±0.1% for Marlipal 1618/25 (Marlipal)), though with a high concentration of metabolites: FFA and PEG. FFA concentration corresponded to 30–100% of theoretically predicted concentration (presuming central fission) and dependent on the chemical structure of surfactant and type of plant used for testing. Total PEG concentration was about 20% of that predicted on the basis of central fission, while the ratio of short-chained PEG in the total PEG varied from 20 to 70% and depended on the chemical structure of surfactant and type of plant used for testing.
Harald Pasch - One of the best experts on this subject based on the ideXlab platform.
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analysis of fatty Alcohol Ethoxylates regarding chain length and endgroups by maldi tof ms using collision induced dissociation
Macromolecular Chemistry and Physics, 2012Co-Authors: Valentina Mass, K Rode, Frank Rittig, Thomas Ostrowski, Harald PaschAbstract:MALDI-TOF MS is used to analyze the chain lengths and endgroups of fatty Alcohol Ethoxylates based on the fragmentation behavior in collision-induced dissociation. MALDI-CID-TOF2 of the Ethoxylates results in complex fragmentation patterns that mirror the fragmentation of the ethylene oxide oligomer chain and the fatty alocohol endgroups. Characteristic fragment patterns are obtained that facilitate the interpretation of the fragmentation behavior of the fatty Alcohol Ethoxylates. Linear and branched endgroups can be differentiated and specific fragments are identified that are characteristic for the cleavage between the polymer chain and the endgroup. These “marker” fragments are used to determine the oligomer chain length and the number of carbons per endgroup.
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two dimensional chromatography of complex polymers 8 separation of fatty Alcohol Ethoxylates simultaneously by end group and chain length
Journal of Separation Science, 2010Co-Authors: Jacquesantoine Raust, Wolf Hiller, Adele Bruell, Pritish Sinha, Harald PaschAbstract:A comprehensive two-dimensional liquid chromatography system was developed to precisely describe the molecular heterogeneity of fatty Alcohol Ethoxylates. The end-group functionality was analyzed by gradient HPLC while ethylene oxide oligomer distributions were characterized by liquid adsorption chromatography. A baseline separation of all functionality fractions irrespective of the ethylene oxide oligomer chain length was achieved on nonpolar X-Terra® C18 with a methanol–water gradient, whereas an isocratic flow of isopropanol–water on a polar Chromolith® Si column gave a separation according to the oligomer chain length without interference of the end-group distribution. The combination of these two methods to conduct online two-dimensional liquid chromatography experiments resulted in a comprehensive two-dimensional picture on the molecular heterogeneity of the sample.
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hplc nmr of fatty Alcohol Ethoxylates
Magnetic Resonance in Chemistry, 2005Co-Authors: Wolf Hiller, Adele Brull, Dimitris S Argyropoulos, Eberhard Hoffmann, Harald PaschAbstract:The application of HPLC–NMR for the analysis of a mixture of fatty Alcohol Ethoxylates (FAEs) is described. The use of the new generation, cryogenically cooled probes is investigated in respect of the sensitivity advantage that they provide. The FAE mixture is separated using liquid chromatography at the critical point of adsorption. The ability of the method to differentiate between the different end groups and the degree of polymerization of the mixture constituents is investigated. Both on-flow and stop-flow HPLC–NMR techniques were used together with two-dimensional NMR spectroscopy. The results are compared with those obtained by using an evaporative light scattering detector for the HPLC. Copyright © 2005 John Wiley & Sons, Ltd.
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matrix assisted laser desorption ionization mass spectrometry of synthetic polymers 7 analysis of fatty Alcohol Ethoxylates by coupled liquid chromatography at the critical point of adsorption and maldi tof mass spectrometry
Macromolecular Symposia, 2003Co-Authors: Karlheinz Spriestersbach, K Rode, Harald PaschAbstract:Fatty Alcohol Ethoxylates can be analyzed efficiently with respect to functionality and molar mass by coupled liquid chromatography and MALDI-TOF mass spectrometry. Both techniques are coupled via a robotic interface, where the matrix is coaxially added to the eluate and spotted dropwise onto the MALDI target. It is shown that liquid chromatography at critical conditions of adsorption coupled to MALDI-TOF yield useful structural information on oligomer masses and chemical composition. In particular, the analysis of technical fatty Alcohol Ethoxylates by LC-CC/MALDI-TOF reveals the presence of different functionality fractions in one sample. The oligomer distributions of all functionality fractions are determined.
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Matrix-assisted laser desorption/ionization mass spectrometry of synthetic polymers. 7. analysis of fatty Alcohol Ethoxylates by coupled liquid chromatography at the critical point of adsorption and MALDI-TOF mass spectrometry
Macromolecular Symposia, 2003Co-Authors: Karlheinz Spriestersbach, Karsten Rode, Harald PaschAbstract:Fatty Alcohol Ethoxylates can be analyzed efficiently with respect to functionality and molar mass by coupled liquid chromatography and MALDI-TOF mass spectrometry. Both techniques are coupled via a robotic interface, where the matrix is coaxially added to the eluate and spotted dropwise onto the MALDI target. It is shown that liquid chromatography at critical conditions of adsorption coupled to MALDI-TOF yield useful structural information on oligomer masses and chemical composition. In particular, the analysis of technical fatty Alcohol Ethoxylates by LC-CC/MALDI-TOF reveals the presence of different functionality fractions in one sample. The oligomer distributions of all functionality fractions are determined.
Bernd Trathnigg - One of the best experts on this subject based on the ideXlab platform.
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liquid exclusion adsorption chromatography a new technique for isocratic separation of nonionic surfactants iv two dimensional separation of fatty Alcohol Ethoxylates with focusing of fractions
Journal of Chromatography A, 2002Co-Authors: Bernd Trathnigg, Christina RappelAbstract:Abstract Fatty Alcohol Ethoxylates can be analyzed using a combination of liquid chromatography under critical conditions as the first dimension and liquid exclusion–adsorption chromatography as the second dimension. Transfer of fractions from the first to the second dimension is achieved using the full adsorption–desorption (FAD) technique. The peaks of interest in the first dimension are trapped on a short precolumn before injecting them into the second dimension. Full adsorption is achieved by increasing the water content in the mobile phase before the FAD column. When the fractions are desorbed by switching to the mobile phase of the second dimension, they are focused and reconcentrated. In this way, a full resolution of oligomers is achieved. As both dimensions are run in isocratic mode, density and refractive index detection can be applied, which allows an accurate quantitation.
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liquid exclusion adsorption chromatography a new technique for isocratic separation of nonionic surfactants iii two dimensional separation of fatty Alcohol Ethoxylates
Journal of Chromatography A, 2001Co-Authors: Bernd Trathnigg, Manfred Kollroser, Christina RappelAbstract:Abstract A quantitatively accurate mapping of lower fatty Alcohol Ethoxylates can be achieved using a combination of liquid chromatography under critical conditions as the first dimension and liquid exclusion–adsorption chromatography as the second dimension. With coupled density and refractive index detection in both dimensions, the contribution of preferential solvation can also be estimated. In most cases, however, the use of refractive index detection alone also yields satisfactory results.
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liquid exclusion adsorption chromatography a new technique for isocratic separation of nonionic surfactants ii quantitation in the analysis of fatty Alcohol Ethoxylates
Journal of Chromatography A, 2001Co-Authors: Bernd TrathniggAbstract:Abstract A new technique of liquid chromatography, which allows baseline separation of fatty Alcohol Ethoxylates with up to 15–20 ethylene oxide units under isocratic conditions allows an accurate quantitative analysis of single hydrophobic chain surfactants. Using density and refractive index detection, the accurate weight fractions of the individual oligomers are obtained. Moreover, the contribution of preferential solvation can be determined. With refractive index detection alone, good accuracy can also be achieved.
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liquid exclusion adsorption chromatography new technique for isocratic separation of nonionic surfactants i retention behaviour of fatty Alcohol Ethoxylates
Journal of Chromatography A, 2001Co-Authors: Bernd Trathnigg, Alexei GorbunovAbstract:A new technique of liquid chromatography is described, which allows a baseline separation of fatty Alcohol Ethoxylates with 15-20 ethylene oxide units under isocratic conditions. The new method is based on a combination of two different chromatographic modes for the individual structural units: size exclusion for the poly(oxyethylene) chain and adsorption interaction for the hydrophobic end fragments. A theory is provided for this mixed exclusion-adsorption mode of liquid chromatography. Chromatographic data are found to be in a good agreement with this theory.
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theory of liquid adsorption chromatography of macromolecules applied to polyethylene glycol and fatty Alcohol Ethoxylates
Journal of Chromatography A, 1997Co-Authors: Bernd Trathnigg, Alexei Gorbunov, B Maier, Alexander SkvortsovAbstract:Liquid adsorption chromatography retention modes of poly(ethylene glycol) (PEG), its mono- and dimethyl ethers (MMEs and DMEs) and also of fatty Alcohol Ethoxylates (FAEs) are studied both experimentally and theoretically. The experimental system under investigation was a Spherisorb S5W 80 A column and isopropanol–water as the mobile phase. At various compositions of the mobile phase (in the range of 75 to 87% of isopropanol) chromatograms exhibiting good peak resolution were obtained and the dependencies of the elution volume on the number of repeating EO units for both PEG and FAE samples evaluated on the basis of a closer inspection of the chromatographic data. The experiments did not reveal any differences between the chromatographic behavior of PEGs, MMEs and DMEs, while the FAEs gave substantially smaller values of elution volume at all mobile phase compositions. These data were interpreted by using a molecular-statistic theory of homopolymers (to describe both PEG, MME and DME) and two-block copolymers (for FAEs) based on a continuum Gaussian chain model of macromolecules and a slit-like model of pores of stationary phase, wide pore approximation and the adsorption chromatography mode for PEG molecules were assumed in the development of this theory. This theory described very well the experimental data obtained, and two thermodynamic parameters characterizing interactions of EO units of PEG and both EO and (CH2)n chains of FAE molecules with the adsorbent pore walls have been determined from the comparison of the theory and the experiments. Although the mean thickness of adsorbed oxyethylene chain, H, was estimated as being equal to about 3.5–4.5 A, H proved to be slightly decreasing with increasing isopropanol content in mobile phase. Chromatograms visualizing the adsorption of PEG and FAE molecules are presented, and the correspondence between the theoretical approach and the experimental situation under investigation is discussed.
Pablo A Laramartin - One of the best experts on this subject based on the ideXlab platform.
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partitioning of Alcohol Ethoxylates and polyethylene glycols in the marine environment field samplings vs laboratory experiments
Science of The Total Environment, 2014Co-Authors: Juan M Traversosoto, Bruce J Brownawell, Eduardo Gonzalezmazo, Pablo A LaramartinAbstract:Abstract Nowadays, Alcohol Ethoxylates (AEOs) constitute the most important group of non-ionic surfactants, used in a wide range of applications such as household cleaners and detergents. Significant amounts of these compounds and their degradation products (polyethylene glycols, PEGs, which are also used for many other applications) reach aquatic environments, and are eliminated from the water column by degradation and sorption processes. This work deals with the environmental distribution of AEOs and PEGs in the Long Island Sound Estuary, a setting impacted by sewage discharges from New York City (NYC). The distribution of target compounds in seawater was influenced by tides, consistent with salinity differences, and concentrations in suspended solid samples ranged from 1.5 to 20.5 μg/g. The more hydrophobic AEOs were mostly attached to the particulate matter whereas the more polar PEGs were predominant in the dissolved form. Later, the sorption of these chemicals was characterized in the laboratory. Experimental and environmental sorption coefficients for AEOs and PEGs showed average values from 3607 to 164,994 L/kg and from 74 to 32,862 L/kg, respectively. The sorption data were fitted to a Freundlich isotherm model with parameters n and log K F between 0.8–1.2 and 1.46–4.39 L/kg, respectively. AEO and PEG sorptions on marine sediment were also found to be mostly not affected by changes in salinity.
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environmental analysis of Alcohol Ethoxylates and nonylphenol ethoxylate metabolites by ultra performance liquid chromatography tandem mass spectrometry
Analytical and Bioanalytical Chemistry, 2012Co-Authors: Pablo A Laramartin, Eduardo Gonzalezmazo, Bruce J BrownawellAbstract:Surfactants and their metabolites can be found in aquatic environments at relatively high concentrations compared with other micropollutants due in part to the exceptionally large volumes produced every year. We have focused our attention here on the most widely used nonionic surfactants, Alcohol Ethoxylates (AEOs), and on nonylphenol ethoxylate (NPEO) degradation products (short-chain nonylphenol Ethoxylates, NP1-3EO, nonylphenol, NP, and nonylphenol ethoxycarboxylates, NP1-2EC), which are endocrine-disrupting compounds. Our main objective in this work was to develop a methodology aimed at the extraction, isolation, and improved analysis of these analytes in environmental samples at trace levels. Extraction recoveries of target compounds were determined for sediment samples after ultrasonic extraction and purification using HLB or C18 solid-phase extraction minicolumns. Recovery percentages were usually between 61 and 102% but were lower for longer AEO ethoxymers. Identification and quantification of target compounds was carried out using a novel ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC–MS-MS) approach, a combination that provides higher sensitivity and faster analysis than prior methods using conventional high-performance liquid chromatography–mass spectrometry. Limits of detection were usually below 0.5 ng/g, being higher for monoethoxylate species (>5 ng/g) because of poor ionization. The method was used for analyzing surface sediment samples collected at Jamaica Bay (NY) in 2008. The highest values (28,500 ng/g for NP, 4,200 ng/g for NP1-3EO, 22,400 ng/g for NP1-2EC, and 1,500 ng/g for AEOs) were found in a sampling station from a restricted water circulation area that is heavily impacted by wastewater discharges.
S K Huang - One of the best experts on this subject based on the ideXlab platform.
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the analysis of alkyl capped Alcohol Ethoxylates and Alcohol ethoxycarboxylates from Alcohol Ethoxylates by atmospheric pressure chemical ionization mass spectrometry
Rapid Communications in Mass Spectrometry, 1999Co-Authors: S K Huang, M H RoodAbstract:Alcohol Ethoxylates (AEs) are nonionic surfactants. They are industrially important compounds that have historically been difficult to analyze, with the best results to date achieved through derivatization (e.g., silylation) followed by analysis by gas chromatography/mass spectrometry (GC/MS). Recently, mass spectrometric techniques such as field desorption (FD), time-of-flight secondary ion mass spectrometry (TOF-SIMS), fast atom bombardment (FAB), electrospray ionization (ESI) and matrix-assisted laser desorption/ionization (MALDI) have been employed to analyze surfynol® 4xx. In an effort to produce low-cost alkyl-capped AEs and anionic detergents from AEs, a fast and reliable measure of the product yields and conversions from AEs is required in research. We found that the product yields and conversions from reactions of AEs, obtained by the employment of atmospheric pressure chemical ionization (APCI), were in good agreement with those obtained from proton nuclear magnetic resonance spectroscopy (1H−NMR). Therefore, APCI can be used as a validated tool for studying AE reactions. Mixtures that contain either silylated or unsilylated Ethoxylates and/or carboxylates yield the same APCI mass spectra. Copyright © 1999 John Wiley & Sons, Ltd.
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The analysis of alkyl‐capped Alcohol Ethoxylates and Alcohol ethoxycarboxylates from Alcohol Ethoxylates by atmospheric pressure chemical ionization mass spectrometry
Rapid Communications in Mass Spectrometry, 1999Co-Authors: S K Huang, M H RoodAbstract:Alcohol Ethoxylates (AEs) are nonionic surfactants. They are industrially important compounds that have historically been difficult to analyze, with the best results to date achieved through derivatization (e.g., silylation) followed by analysis by gas chromatography/mass spectrometry (GC/MS). Recently, mass spectrometric techniques such as field desorption (FD), time-of-flight secondary ion mass spectrometry (TOF-SIMS), fast atom bombardment (FAB), electrospray ionization (ESI) and matrix-assisted laser desorption/ionization (MALDI) have been employed to analyze surfynol® 4xx. In an effort to produce low-cost alkyl-capped AEs and anionic detergents from AEs, a fast and reliable measure of the product yields and conversions from AEs is required in research. We found that the product yields and conversions from reactions of AEs, obtained by the employment of atmospheric pressure chemical ionization (APCI), were in good agreement with those obtained from proton nuclear magnetic resonance spectroscopy (1H−NMR). Therefore, APCI can be used as a validated tool for studying AE reactions. Mixtures that contain either silylated or unsilylated Ethoxylates and/or carboxylates yield the same APCI mass spectra. Copyright © 1999 John Wiley & Sons, Ltd.