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Wyniki wyszukiwania dla: THERMAL DESORPTION
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Thermal decomposition of surface compounds for the generation of small quantities of acetaldehyde. Calibration of a thermal desorption gas chromatography flame ionization detection.
PublikacjaW pracy opisano sposób wytwarzania niewielkich ilości acetaldehydu w procesie termicznego rozkładu związku powierzchniowego uzyskanego w wyniku chemicznej modyfikacji żelu krzemionkowego.Proces rozkładu prowadzony jest w temperaturze 130-190 stopni Celsjusza.Przedstawiono również sposób syntezy prowadzący do uzyskania odpowiedniego związku powierzchniowego.
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Calibration of the thermal desorption-gas chromatography-mass spectrometry system using standards generated in the process of thermal decomposition of chemically modified silica gel
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Development of a solventless stir bar sorptive extraction/thermal desorption large volume injection capillary gas chromatographic-mass spectrometric method for ultra-trace determination of pyrethroids pesticides in river and tap water samples
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Thermal and physical properties of ZrO2–AlO(OH) nanopowders synthesised by microwave hydrothermal method
PublikacjaIndustrially relevant nanopowder was synthesised by microwave hydrothermal synthesis to obtain well-controlled composition (ZrO2–AlO(OH) system) which was found to determine a number of physical and thermal characteristics. This study reports variation of particle size, density, specific surface area (SSABET), as well as thermal behaviour of nanopowder mixtures of ZrO2–AlO(OH) in the whole range of compositions. It was found that...
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Reactions in nanofilms of trifluoroacetic acid (CF3COOH) driven by low energy electrons
PublikacjaBadano modyfikacje chemiczne indukowane przez niskoenergetyczne elektrony (0-20eV) w cienkich warstwach skondensowanych molekuł CF3COOH. Do badań zastosowano dwie metody: desorpcję jonów w wyniku bombardowania elektronami (ESD - Electron Stimulated Desorption) oraz termiczną desorpcję jonów (TDS - Thermal Desorption Spectroscopy).
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The new silica-based coated SPME fiber as universal support for the confinement of ionic liquid as an extraction medium
PublikacjaThe new silica-based SPME fiber coating is reported for the first time as universal support purposed to confinement of ionic liquid as an extraction medium. Fiber coating was prepared by the sol-gel process, using potassium silicate (K2SiO3) as a precursor and dimethylformamide (DMF) as a pore-forming medium. The concept of synthesis assumes obtaining a solid porous material on the surface of the glass rod and, being characterized...
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The role of hydrogen bonding on tuning hard-soft segments in bio-based thermoplastic poly(ether-urethane)s
PublikacjaThis work describes the preparation of bio-based thermoplastic poly(ether-urethane)s (TPU) via a prepolymer method and investigates the effect of varying the interphase hydrogen-bonding (H-bonding) on physicochemical, thermal and mechanical properties. This was achieved by varying the glycol type and molar ratio of [NCO]/[OH] groups used during the prepolymer chain extending step. The TPUs’ chemical structure was analyzed by Fourier...
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Development of SPME fiber coatings with tunable porosity for physical confinement of ionic liquids as an extraction media
PublikacjaExtending the use of ionic liquids in sample preparation techniques remains a challenge. This paper presents procedures enabling the easy application of ionic liquids to the SPME technique. For this purpose, two approaches for producing a porous silica coating on a metal rod were investigated. Two silica precursor and porogen systems were used in the research: K2SiO3 + Formamide and Tetramethyl-orthosilicate + Polyethylene oxide....
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Determination of Terpene Profile in Cape gooseberry (Physalis peruviana L.) with Use of HS-SPME/GCxGC-TOFMS Method
PublikacjaFresh fruits and products made of them, especially fruit juice, provide the basic energetic substances (simple and complex sugars) and are a source of health beneficial vitamins, macro and microelements, antioxidants and compounds which are classified together with essential oils (for example terpenes), which positively affect human s health. The terpenes profile of cape gooseberry was determined by headspace solid--phase microextraction...
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Application of passive sampling technique in monitoring research on quality of atmospheric air in the area of Tczew, Poland.
PublikacjaThis paper presents the results of atmospheric air quality research in Tczew (adjacent to the Vistula River) on the content of BTEX compounds. Analytical procedure applied during the sampling of the analytes from the air used the passive sampling technique (diffusive passive sampler, Radiello®). For determination of BTEX compounds in atmospheric air, two-stage thermal desorption technique combined with gas chromatography (TD-GC-FID)...
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Analysis of exhaled breath for dengue disease detection by low-cost electronic nose system
PublikacjaThis paper presents a procedure and a set-up of an electronic nose system analyzing exhaled breath to detect the patients suffering from dengue – a mosquito-borne tropical disease. Low-power resistive gas sensors (MiCS-6814, TGS8100) were used to detect volatile organic compounds (VOCs) in the exhaled breath. The end-tidal phase of patients exhaled breath was collected with a BioVOCTM breath sampler. Two strategies were assessed...
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Preparation and characterization of asphaltene based adsorbents for gas-solid adsorption systems
PublikacjaThe dissertation presents results of the experimental research on asphaltene-based adsorbents (support coated with asphaltene layer) for gas-solid adsorption systems, with special reference to volatile organic compounds (VOCs) removal from gas streams. Analysis of gas adsorption properties revealed that asphaltenes isolated from oxidized bitumen have strong affinity toward VOCs. Interactions with target gas molecules, and selectivity...
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Synthesis and characterization of novel renewable polyesters based on 2,5-furandicarboxylic acid and 2,3-butanediol
PublikacjaNovel polyesters from 2,5-furandicarboxylic acid or 2,5-dimethyl-furandicarboxylate and 2,3-butanediol have been synthesized via bulk polycondensation catalyzed by titanium (IV) n-butoxide, tin (IV) ethylhexanoate, or zirconium (IV) butoxide. The polymers were analyzed by size exclusion chromatography, nuclear magnetic resonance spectroscopy, Fourier transform infrared spectroscopy (FTIR), matrix-assisted laser ionization-desorption...
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α-Pinene, 3-carene and d-limonene in indoor air of Polish apartments: The impact on air quality and human exposure
PublikacjaMonoterpenes are among most ubiquitous volatile organic compounds (VOCs) to be detected in indoor air. Since the quality of indoor air is considered important for inhabitants' well-being, the present study aimed at investigating impact of human activity on levels of selected monoterpenes applying passive sampling technique followed by thermal desorption and gas chromatography coupled mass spectrometry. One of the objectives of...
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Membrane-SPME the best 'green' sample preparation technique for the gas chromatographic determination polar organic pollutants in polar media
PublikacjaOne of the most popular technique for sample preparation, which fulfill requirements of green analytical chemistry, is solid phase microextraction (SPME). Because of the undoubted advantages of SPME technique, solvent-free character of the extraction process and the enormous potential in analytical practice, a series of studies has been undertaken to develop new technical solutions, where improving the sensitivity and the extraction...
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Graphene oxide aerogels for adsorptive separation of aromatic hydrocarbons and cycloalkanes
PublikacjaEfficient separation of benzene and cyclohexane has critical importance for production of commodity chemicals, and is one of the most challenging separations in the industry. Physisorption by recyclable, porous solids has a significant potential in substituting energy-intensive azeotropic or extractive distillation methods. Reduced graphene oxide aerogels (rGOAs) are emerging materials holding great promise for connecting unique...
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Emission profile of butan-2-one oxime from commercially available neutral silicone sealant
PublikacjaThe paper presents results of research on emission profile of butan-2-one oxime (methyl ethyl ketoxime, MEKO) released from two types of commercially available neutral silicone sealants: silicone type ‘S’ and silicone type ‘T’. To determine the emissions from silicone samples, the system consists of a stationary emission chamber, and the thermal desorption-gas chromatography-mass spectrometry system was applied. First, the research...
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Investigation on air quality of specific indoor environments—spa salons located in Gdynia, Poland
PublikacjaDue to excessive application of essential oils and scented products in spa salons during aromatherapy and massage sessions, the elevated concentration of total volatile organic compounds (TVOCs), particularly terpenes, which are known as secondary organic aerosol (SOA) precursors, is expected there. This study was aimed at determination of VOCs with a particular regard to terpenes in air samples collected in selected spa salons...
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Concentration levels of selected analytes in the gas phase of an e-cigarette aerosol
PublikacjaThe aerosols generated from e-cigarettes are composed of liquid and gas phases resulting from vapourized e-liquid. The apportioning of substances from e-liquid into the liquid and gas phases during e-cigarette use has not been extensively studied. Partitioning of e-liquid components between the gas and the liquid phase of the aerosol influences the substances inhaled and exhaled by the users, leading to second-hand exposure. It...
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Concentrations of monoaromatic hydrocarbons in the air of the underground car park and individual garages attached to residential buildings
PublikacjaThe paper describes the characteristics of a two-level underground car park and three individual garages attached to residential buildings, differing by the resident utilization habits, located in North Poland (Tri-City agglomeration area). The strategy of collecting the analyte samples from air in mentioned enclosed areas, concerning the determination of benzene, toluene, ethylbenzene, o-xylene and p,m-xylenes (BTEX) concentrations...
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The dispersive micro-solid phase extraction method for MS-based lipidomics of human breast milk*
PublikacjaA simple and rapid microextraction method ensuring high lipidome coverage was developed for liquid chromatography mass spectrometry (LC-MS)-based lipidomics of human breast milk. The dispersive microsolid phase extraction (D-µ-SPE) technique, coupled with the design of experiment (DoE) method, enabled the study of the influence of several conditions (desorption solvent, stationary phase ratio, and sorption and desorption time)...
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Interfacial behaviour of human bile and its substitution for in vitro lipolysis studies
PublikacjaThis study examined the interfacial evolution of individual bile salts (BSs) and their blends with phosphatidylcholine (BS/PC) to simulate the complex behaviour of human bile (HB) during lipolysis at the triglyceride/water interface. Using adsorption and desorption cycles, mimicking exposure to small intestinal fluids, we demonstrate that the interfacial behaviour of real HB can be replicated using simple mixtures of BSs and PC....
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In-tube extraction for the determination of the main volatile compounds in Physalis peruviana L
PublikacjaAn analytical procedure based on in-tube extraction followed by gas chromatography with mass spectrometry has been developed for the analysis of 24 main volatile components in cape gooseberry (Physalis peruviana L.) samples. According to their chemical structure, the compounds were organized into different groups: one hydrocarbon, one aldehyde, four alcohols, four esters, and 14 monoterpenes. By single-factor experiments, incubation...
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Adsorption behavior of Methylene Blue and Rhodamine B on microplastics before and after ultraviolet irradiation
PublikacjaThe accumulation of microplastics (MPs) and dyes has attracted extensive attention because of their environ mental effects, which will be exacerbated especially after the aging of MPs. This study aimed at investigating the significance of Methylene Blue (MB) and Rhodamine B (RhB) adsorption behavior by PLA (polylactic acid) and PA66 (Polyamide 66) MPs after UV aging. After aging, there was an observed increase in the hydrophilicity,...
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Local atomic order in low Pt-content nanocatalysts investigated in situ by XAS
PublikacjaThe unique features of X-ray absorption spectroscopy allow investigations of nanosized catalysts for fuel cells under working conditions. We present the results of an experiment carried out on a low Pt content electrocatalyst supported by a mesoporous heteropolyacid salt and used at the cathode of a proton exchange membrane fuel cell (PEMFC). The analysis of the EXAFS signal at the Pt L3-edge indicates that upon operating the fuel...
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Formaldehyde detection with chemical gas sensors based on WO3 nanowires decorated with metal nanoparticles under dark conditions and UV light irradiation
PublikacjaWe report results of formaldehyde gas (CH2O) detection under dark conditions and UV light irradiation with pristine tungsten trioxide nanowires (WO3 NWs) and metal nanoparticles decorated WO3 NWs gas sensing layers. The resistive layers were deposited by one step aerosol assisted chemical vapor deposition (AACVD) on commercial alumina substrates with 10-pair interdigitated platinum electrodes. The elaborated gas sensors, based...
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Application of Headspace Solid-phase Microextraction with Poly(1-vinyl-3- Hexylimidazolium Chloride) Polymeric Ionic Liquid Coating using GC - MS to Determine Volatile Fatty Acids in Dairy Wastewater
PublikacjaVolatile fatty acids were determined in this study using headspace solid-phase microextraction (HS-SPME) with a poly(1-vinyl-3-hexylimidazolium chloride) polymeric ionic liquid coated fiber followed by gas chromatography - mass spectrometry. Experimental parameters such as extraction time and temperature, sample volume as well as desorption time and temperature were optimized. Detection limits of the method were in the range of...
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Perspectives of Fluctuation-Enhanced Gas Sensing by Two-Dimensional Materials
PublikacjaWe present the results of gas sensing using the fluctuation-enhanced sensing method in selected two-dimensional materials (2DMs). We claim that gas sensing selectivity can be improved further by considering semiconducting two-dimensional materials doped by noble metal nanoparticles. The 2DMs' structures exhibit some imperfections defined by their structure, occurring repeatedly there. These imperfections are adsorption-desorption...
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Synthetic Principles Determining Local Organization of Copolyesters Prepared from Lactones and Macrolactones
PublikacjaA highly effective and facile technique for catalytic ring-opening copolymerization (cROP) of lactones viz. ε- caprolactone and ε-decalactone with ω-pentadecalactone is being described. The reactions were mediated by Zn- and Cabased tridentate Schiff base complexes and benzyl alcohol as initiator. The catalysts were successfully employed for the preparation of numerous block and random copolymers. To unravel the composition of...
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The effect of 1,4-butanediol on the efficiency of CO2 absorption and inhibition of NH3 escape during the mineral carbonation of gypsum
PublikacjaThis study explored the optimal concentration of 1,4-butanediol for maximizing CO2 absorption and minimizing ammonia desorption. Mineral carbonation of gypsum slurry was carried out in a bubble reactor with a magnetic stirrer maintaining constant speed for 1 hour. The gas introduced to the reactor was a mixture of CO2 and air. The gas flow was controlled by the mass controllers. Gas sensors were used to determine the concentration...
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Combined chemoresistive and in situ FTIR spectroscopy study of nanoporous NiO films for light-activated nitrogen dioxide and acetone gas sensing
PublikacjaThe chemoresistive sensor response of nanoporous NiO films prepared by advanced gas deposition was investigated by combined resistivity and in situ FTIR spectroscopy, with and without simultaneous light illumination, to detect NO2 and acetone gases. The sensitivity towards NO2 increased dramatically under UV irradiation employing 275 nm light. Improved sensitivity was observed at an elevated temperature of 150 °C. In situ FTIR...
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Structure-rheology relationship of fully bio-based linear polyester polyols for polyurethanes - Synthesis and investigation
PublikacjaThe synthesis of polyols from renewable substances as an alternative for petrochemical-based polyols play important matter in the polyurethane industry. In this work, the fully bio-based linear polyester polyols with different catalyst amounts were synthesized via two-step polycondensation method. The effect of various catalyst content on the structure and rheological behavior were established. Fourier Transform Infrared Spectroscopy,...
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Solid phase microextraction–comprehensive twodimensional gas chromatography–time-of-flight mass spectrometry: a new tool for determining PAHs in airport runoff water samples
Publikacjafundamental aspect of airport operations is the pollution caused by airport runoff waters. Polycyclic aromatic hydrocarbons (PAHs) are one of the most important groups of xenobiotics which are commonly found in runoff water originating from airports. Only very limited data on the analysis of airport runoff water have been published until now. Therefore, a reliable and accurate analytical method based on headspace solid-phase microextraction...
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Dispersive Micro‐Solid Phase Extraction of Selected Metals in Water and Food Samples Followed by ICP‐OES Analysis: Method Development, Analysis of Real Samples and Greenness Evaluation
PublikacjaMultiwalled carbon nanotubes (MWCNTs) are well-known adsorbents because of their high surface area, layered and hollow architecture, hydrophobicity, and multiple and easily accessible adsorption sites. In this study, MWCNTs were used for dispersive micro-solid-phase extraction of various metal chelates in environmental and food samples. Different parameters such as concentration of the chelating reagent, the sorbent dosage, the...
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Application and optimization of headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography - flame-ionization detector (GC-FID) to determine products of the petroleum industry in aqueous samples
PublikacjaA simple and solvent-free analytical method has been optimized for the determination of hydrocarbons (C6 - C20) from products of the petroleum industry in aqueous samples. Extraction and analysis was carried out using headspace solid-phase microextraction (HS-SPME) and gas chromatography coupled with flame-ionization detector (GC-FID). A ZB-5 capillary column (30 m × 0.25 mm inner diameter, 0.25 µm film thickness) was used for...
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Preparation of Allyl Alcohol Oligomers Using Dipicolinate Oxovanadium(IV) Coordination Compound
PublikacjaCurrently, new precatalysts for olefin oligomerization are being sought in the group of vanadium(IV) complexes. Thus, the aim of our research was to examine the catalytic activity of the oxovanadium(IV) dipicolinate complex [VO(dipic)(H2O)2] 2 H2O (dipic = pyridine-2,6-dicarboxylate anion) in 2-propen-1-ol oligomerization as well as to characterize oligomerization products using matrix-assisted laser desorption/ionization–time-of-flight...
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Improving carbon dioxide capture in aqueous ammonia solutions by fine SiO2 particles
PublikacjaAmmonia solutions are considered to be effective solvents for carbon dioxide absorption. Despite the numerous advantages of these solvents, their high volatility is a significant technical and economic problem. Therefore, in this work, silica particles were used as additives to improve CO2 absorption and inhibit NH3 desorption. SiO2 microparticles and colloidal SiO2 particles in the concentration range of 0-0.15 wt.% were used...
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Optimization of a Fabric Phase Sorptive Extraction protocol for the isolation of six bisphenols from juice pouches to be analysed by high performance liquid chromatography coupled with diode array detector
PublikacjaFabric Phase Sorptive Extraction (FPSE) combined with high pressure liquid chromatography using to diode array detection (HPLC-DAD) was applied for the simultaneous determination of bisphenols (BPA, BPB, BPC, BPE, BPF, BPS) in juice pouches. The FPSE procedure was optimized with regards to the critical parameters that affect the performance of the method including the selection of the FPSE membrane type and size, adsorption time,...
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Organic semiconductor rubrene thin films deposited by pulsed laser evaporation of solidified solutions
PublikacjaOrganic semiconductor rubrene (C42H28) belongs to most preferred spintronic materials because of the high charge carrier mobility up to 40 cm2(V·s)-1. However, the fabrication of a defect-free, polycrystalline rubrene for spintronic applications represents a difficult task. We report preparation and properties of rubrene thin films deposited by pulsed laser evaporation of solidified solutions. Samples of rubrene dissolved in aromatic...
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Molybdenum sulfide modified with nickel or platinum nanoparticles as an effective catalyst for hydrogen evolution reaction
PublikacjaIn this study, we investigate the catalytic performance of molybdenum sulfide (MoS2) modified with either nickel (Ni) or platinum (Pt) nanoparticles as catalysts for the hydrogen evolution reaction (HER). The MoS2 was prepared on the TiO2 nanotube substrates via a facile hydrothermal method, followed by the deposition by magnetron sputtering of Ni or Pt nanoparticles on the MoS2 surface. Structural and morphological characterization...
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Gas selectivity enhancement by sampling-and-hold method in resistive gas sensors
PublikacjaCommercial resistive gas sensors exhibit various sensitivity to numerous gases when working at different elevated temperatures. That effect is due to a change in velocity of adsorption and desorption processes which can be modulated by temperature. Thus, to reach better selectivity of gas detection, we propose to apply a known method (called the sampling-and-hold method) of cooling down the gas sensor in the presence of the investigated...
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Green Sample Collection
PublikacjaThe term of “green sample collection” is directly associated with both passive and dynamic analytical tools which allow for simultaneous management of the stage of collection and isolation and/or enrichment of a broad spectrum of chemical compounds from environmental samples. The use of passive sampling techniques at the stage of sample collection makes it possible to obtain in a simple yet inexpensive manner an analytical information...
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Multi-residue method for the determination of 16 recently used pesticides from various chemical groups in aqueous samples by using DI - SPME coupled with GC-MS
PublikacjaA simple and solvent-free multi-residue method has been optimized to determine 16 currently used pesticides from different chemical groups in aqueous samples. The extraction of analytes was carried out with direct immersion solid-phase microextraction (DI-SPME) and for the identification and quantitative determination gas chromatography coupled with mass spectrometry (GC-MS) was applied. Two commonly used adsorbent coatings have...
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Dielectric properties of modified graphene oxide filled polyurethane nanocomposites and its correlation with rheology
PublikacjaThis study aims at investigating the dynamic mechanical, dielectric and rheological properties of reinforced polyurethane (PU) nanocomposites containing hydrophilic graphene oxide (GO) and/or hydrophobic modified graphene oxide (mGO) sheets. The organic modification of GO was performed with 4,4′-methylenebis (phenyl isocyanate) (MDI) and the samples were prepared by solvent mixing. We found that addition of mGO provides a more...
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Hydrogen Embrittlement and Oxide Layer E ect in the Cathodically Charged Zircaloy-2
PublikacjaThe present paper is aimed at determining the less investigated effects of hydrogen uptake on the microstructure and the mechanical behavior of the oxidized Zircaloy-2 alloy. The specimens were oxidized and charged with hydrogen. The different oxidation temperatures and cathodic current densities were applied. The scanning electron microscopy, X-ray electron diffraction spectroscopy, hydrogen absorption assessment, tensile, and...
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Effects of UV light irradiation on fluctuation enhanced gas sensing by carbon nanotube networks
PublikacjaThe exceptionally large active surface-to-volume ratio of carbon nanotubes makes it an appealing candidate for gas sensing applications. Here, we studied the DC and low-frequency noise characteristics of a randomly oriented network of carbon nanotubes under NO2 gas atmosphere at two different wavelengths of the UV light-emitting diodes. The UV irradiation allowed to sense lower concentrations of NO2 (at least 1 ppm) compared to...
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Interaction of 4-nitrothiophenol with low energy electrons: Implications for plasmon mediated reactions
PublikacjaThe reduction of 4-nitrothiophenol (NTP) to 4-4′-dimercaptoazobenzene (DMAB) on laser illuminated noble metal nanoparticles is one of the most widely studied plasmon mediated reactions. The reaction is most likely triggered by a transfer of low energy electrons from the nanoparticle to the adsorbed molecules. Besides the formation of DMAB, dissociative side reactions of NTP have also been observed. Here, we present a crossed electron-molecular...
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Rubrene Thin Films with Viably Enhanced Charge Transport Fabricated by Cryo-Matrix-Assisted Laser Evaporation
PublikacjaAmong organic semiconductors, rubrene (RB; C42H28) is of rapidly growing interest for the development of organic and hybrid electronics due to exceptionally long spin diffusion length and carrier mobility up to 20 cm2V−1s−1 in single crystals. However, the fabrication of RB thin films resembling properties of the bulk remains challenging, mainly because of the RB molecule’s twisted conformation. This hinders the formation of orthorhombic...
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Deep eutectic solvents – based green absorbents for effective volatile organochlorine compounds removal from biogas
PublikacjaVolatile organochlorine compounds (VOXs) presented in biogas can cause many technological and environmental problems. During the combustion of biogas containing VOXs, the corrosion of installation, as well as the formation of toxic by-products (polyhalogenated dioxins and furans) and further emission to the atmosphere, may occur. Therefore, in this study, a new procedure based on physical absorption was developed. In order to meet...
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Direct solid phase microextraction combined with gas chromatography – Mass spectrometry for the determination of biogenic amines in wine
PublikacjaA direct method based on immersion solid phase microextraction (DI-SPME) gas chromatography mass-spectrometry (GC-MS) was optimized and validated for the determination of 16 biogenic amines in Polish wines. In the analysis two internal standards were used: 1,7-diaminoheptane and bis-3-aminopropylamine. The method allows for simultaneous extraction and derivatization, providing a simple and fast mode of extraction and enrichment....