Repozytorim Annales UMCS Sectio AA - Chemia:
Liczba artykułów w bazie: 202 Format SWF: 159 Format DJVU: 161 Format PDF: 202 Razem plików: 522

Volume 70 - 2015

Article 000PL: Spis treści
EN: Table of contents
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Article 001EN: The 70th Birthday of Professor Bronisław Jańczuk
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Anna Zdziennicka

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Article 01EN: Experimental approach towards the water contact angle value on the biomaterial alloy Ti6Al4V
1-13

Margarita Hierro-Oliva 1;2, Amparo Maria Gallardo-Moreno 2;1, Abraham Rodríguez-Cano 2;1, Jose Morales Bruque 2;1, Maria Luisa González-Martín 2;1


1 Networking Research Center on Bioengineering, Biomaterials and Nanomedicine (CIBER-BBN), Badajoz, Spain
2 Dept. Applied Physics, Faculty of Sciences, University of Extremadura, Badajoz, Spain *email: mlglez@unex.es

In the biomedical field, water contact angle is a useful gauge to follow how a biomaterial surface would interact with the surrounding water-like physiological environment. Ti6Al4V alloy is widely used in orthopedic applications. Nevertheless, the values of its water contact angle reported in the literature show a large dispersion, from 40° up 80°. However, in addition to the expected dependence of the surface wettability on preliminary treatments, the values of the water contact angle on the pristine Ti6Al4V alloy suffers from an important variability and lack of reproducibility. The present research pays attention to this difficulty and proposes a simple experimental procedure to ensure adequate contact angle reproducibility. Controlled passivation growth in mild underwater conditions of freshly polished disks, followed by ultrasonic washing, avoiding the rubbing of the surface, gives average water contact angles of 80° with very low standard deviations also among samples from the same batch.
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  14. M. A. Pacha-Olivenza, A. M. Gallardo-Moreno, A. Méndez-Vilas, J. M. Bruque, J. L. González-Carrasco, M. L. González-Martín, Effect of UV irradiation on the surface Gibbs energy of Ti6Al4V and thermally oxidized Ti6Al4V, J. Colloid Interf. Sci., 320, 117, (2008).
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  26. F. Variola, J.-H. Yi, L. Richert, J. D. Wuest, F. Rosei, A. Nanci, Tailoring the surface properties of Ti6Al4V by controlled chemical oxidation, Biomaterials, 29, 1285, (2008).
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Article 02EN: On mechanism of the bubble bouncing from hydrophilic and hydrophobic solid surfaces
15-27

Jan Zawała, Piotr Zawała, Kazimierz Małysa


Jerzy Haber Institute of Catalysis and Surface Chemistry PAS, ul. Niezapominajek 8, Kraków *e-mail: nczawala@)cyf-kr.edu.pl

The kinetics of collision and bouncing of an air bubble on hydrophilic and hydrophobic solid surfaces immersed in distilled water is reported. We carried out the experiments and compared the bubble collision and bouncing courses on the stagnant and vibrating, with a controlled frequency and amplitude, solid/liquid interface. For stagnant interface differences in the outcome of the bubble collisions with hydrophilic and hydrophobic solid surfaces are resulting from different stability of the intervening liquid film formed between the colliding bubble and these surfaces. The liquid film was unstable at Teflon surface, where the three-phase contact (TPC) and the bubble attachment were observed, after dissipation of most of the kinetic energy associated with the bubble motion. For vibrated solid surface it was shown that kinetics of the bubble bouncing is independent on the hydrophilic/hydrophobic properties of the surface. Similarly like at water/glass hydrophilic interface, even at highly hydrophobic Teflon surface time of the bubble collisions and bouncing was prolonged almost indefinitely. This was due to the fact that the energy dissipated during the collision was re-supplied via interface vibrations with a properly adjusted acceleration. The analysis of the bubble deformation degree showed that this effect is related to a constant bubble deformation, which determined constant radius of the liquid film, large enough to prevent the draining liquid film from reaching the critical thickness of rupture at the moment of collision. The results obtained prove that mechanism of the bubble bouncing from various interfaces depends on interrelation between rates of two simultaneously going processes: (i) exchange between kinetic and surface energies of the system and (ii) drainage of the liquid film separating the interacting interfaces.
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Article 03EN: Wetting properties of biosurfactant (rhamnolipid) with synthetic surfactants mixtures in the context of soil remediation
29-39

Elżbieta Hallmann, Krystyna Mędrzycka


Gdańsk University of Technology, Chemical Faculty, Narutowicza 11/12, 80-233 Gdańsk *e-mail: elzbieta.hallmann@pg.gda.pl

Wetting properties of synthetic surfactant Rokanol NL6, biosurfactant JBR 425 and their mixture have been investigated. On the basis of these investigations, the ability of used surfactants to remove the synthetic base oil (PAO6) from sandy soil and clay loam was evaluated. Surfactant solutions were applied for soil flushing in batch experiments. The results show that synthetic surfactant addition worsens physicochemical properties of pure biosurfactant but exhibits much higher oil removal efficiency than biosurfactant does.
biosurfactant, nonionic surfactant, surfactants mixtures, soil remediation.
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Article 04EN: Effect of Pluronics and surfactant adsorption onto dolomite suspension zeta potential and stability
41-53

Anna Kozak, Zygmunt Sadowski


Wroclaw University of Technology, Wybrzeże Wyspiańskiego 27, 50-370 Wrocław *e-mail: zygmunt.sadowski@pwr.wroc.pl

Two kinds of Pluronics (PEO-PPO-PEO triblock copolymers) were used in these studies. They have mixed with anionic surfactant (sodium oleate). The adsorption isotherms of surfactant and copolymer-surfactant mixture onto dolomite have been determined. The adsorbed amount of the Pluronics increases with increasing concentration and reaches plateau. An increase of adsorbed amounts of anionic surfactant onto the mineral surfaces (dolomite) has been observed at the presence of Pluronic copolymers. The adsorption effect of triblock copolymers has been investigated on the zeta potential of dolomite at the water suspension. The interaction of anionic surfactant with copolymers causes a decrease of zeta potential to small amount due to the deformation of double electrical layer. The adsorbed non-ionic Pluronic layer partially screens the surface charge of mineral particles, and thus, reduces the zeta potential. On the other hand, the adsorption of anionic surfactant and copolymer caused a decrease of negative value of zeta potential both investigated minerals. The stability of dolomite suspension depends on the both copolymer and sodium oleate concentrations.
Pluronic, adsorption, synergism, zeta potential, dolomite, surfactant, sodium oleate
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Article 05EN: Reaction volume in aqueous solutions in problem solving
55-63

Marek Kosmulski


Lublin University of Technology, Laboratory of Electrochemistry, Nadbystrzycka 38, 20 618 Lublin, Poland email: m.kosmulski@pollub.pl

The volumes of reactions in solution are usually ignored in problem solving. Neglection of reaction volumes may lead to errors on the order of 1 % in the final result. Calculation of the volume of neutralization reaction based on the specific densities of solutions from chemical tables is demonstrated.
problem solving; physical chemistry; acid-base reactions; thermos-dynamics; chemical tables
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Article 06EN: Changes in surface properties of polymethylmethacrylate (PMMA) treated with air plasma
65-78

Diana Rymuszka, Konrad Terpiłowski, Lucyna Hołysz, Emil Chibowski


Department Interfacial Phenomena, Faculty of Chemistry, Maria Curie-Sklodowska University, 20-031 Lublin, Poland

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Article 07EN: Effect of phospholipid and (phospho)lipase modification on interfacial properties of oil/water emulsion
79-109

Agnieszka Ewa Wiącek


Department of Interfacial Phenomena, Faculty of Chemistry, Maria Curie-Skłodowska University, Maria Curie-Skłodowska Sq. 3, 20-031 Lublin, Poland, email: a.wiacek@poczta.umcs.lublin.pl

This review paper focused on the effect of typical phosphorlipid (or lecithin) and enzyme modification on electrokinetic parameters of oil/water emulsion. Physicochemical properties of the systems were investigated taking into account the effective diameter of the droplets as well as the zeta potentials using the dynamic light scattering technique. The effect of phospholipid and phospholipase modification on interfacial properties of o/w emulsion was examined as a function of temperature, pH and ionic strength (effect of Na+ or Ca2+ ions which occur in the physiological fluids). The particular role of Ca2+ ions in the dispersions with zwitterionic phospholipids (the main components of biological membrane) was confirmed.
The phospholipids dipalmitoylphosphatidylcholine, DPPC or dioleoylphosphatidylcholine, DOPC having the same headgroup bound to the apolar tail composed of two saturated or unsaturated chains were used as stabilizing agents. The effective diameters do not always correlate with the zeta potentials. A possible reason for such behaviour might a mechanism different from the electrostatic stabilization. Phospholipids and their mixtures (e.g. lecithin) may undergo spontaneous aggregation in aqueous solution and self organize into liposomes, which possess different sizes and surface affinities. These unique behaviours of phospholipid dispersion can be controlled using the investigated parameters. These findings are expected to increase in importance as phospholipid systems see more use in self-assembly applications.
The other aim of the paper was the comparison of the enzyme phospholipase influence on lipid hydrolysis in the o/w emulsion environment. The work is the study which presents the twofold effect of ethanol dipoles on phosholipid hydrolysis. It is believed that the enzyme effect on the phospholipid aggregation behaviour at the oil-water interface will be helpful for understanding different biological phenomena.
dynamic light scattering, phospholipid, phospholipase, zeta potential, effective diameter.
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Article 08EN: Activity coefficient at infinite dilution of aqueous solutions of nonionic hydrocarbon and fluorocarbon surfactants as well as their ternary mixtures
111-124

Katarzyna Szymczyk, Anna Taraba


Department of Interfacial Phenomena, Faculty of Chemistry, Maria Curie-Skłodowska University, Maria Curie-Skłodowska Sq. 3, 20-031 Lublin, Poland email: katarzyna.szymczyk@poczta.umcs.lublin.pl email: anna.taraba@poczta.umcs.lublin.pl

Activity coefficients at infinite dilution of the aqueous solutions of nonionic hydrocarbon surfactants, p-(1,1,3,3- tetramethylbutyl) phenoxypoly(ethylene glycols), Triton X-100 (TX100) and Triton X-165 (TX165), fluorocarbon surfactants, Zonyl FSN-100 (FSN100) and Zonyl FSO-100 (FSO100) and their ternary mixtures were determined from the Gracia-Fadrique et al. method for non-volatile compounds. The values of activity coefficients were calculated taking into account the surface tension data of the studied systems at 293K and compared to those determined on the basis of the values of the contact angle of solutions on the polytetrafluoroethylene (PTFE) and polymethyl methacrylate (PMMA) surfaces and the solid-liquid interface tension.
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Article 09EN: Influence of the ambient temperature on water and diiodomethane contact angle with quartz surface
125-136

Konrad Terpiłowski


Department of Interfacial Phenomena, Faculty of Chemistry, Maria Curie-Sklodowska University, Lublin, Poland

Wettability of solids is a key phenomenon in many processes. One should mentioned those which accompany us in our everyday life i.e. washing or cementing as well as those applied in industry e.g. flotation of minerals. Value of the contact angles are affected by many factors. One of them is temperature. In this paper monocrystaline quartz was used in the investigations which were carried out in the range 5−50°C with the step every 5°C. As follows the value of the contact angle of both water and diiodomethane changes with the increasing temperature. The change of its value for water is much larger than in case of another liquids of apolar character. Using Chibowski approach the apparent surface free energy was calculated in two ways with and without correction about temperature change of the surface tension. The calculation show difference between both results. Taking into consideration another value of the surface tension should not be neglected even if measurements is taken at a temperature close to 20°C which is the standard in one in such measurements
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Article 10EN: Wetting properties of the sodium bis(2-ethylhexyl) sulfosuccinate (AOT) and polyoxyethylene(23) lauryl ether (Brij 35) binary mixtures in the poly(tetrafluoroethylene)-solution-air system
137-148

Joanna Krawczyk


Department of Interfacial Phenomena, Faculty of Chemistry, Maria Curie-Skłodowska University, Maria Curie-Skłodowska Sq. 3, 20-031 Lublin, Poland e-mail: j.krawczyk@poczta.umcs.lublin.pl

Wettability of poly(tetrafluoroethylene) (PTFE) by aqueous solutions of binary mixtures composed of sodium bis(2-ethylhexyl) sulfosuccinate (AOT) with polyoxyethylene (23) lauryl ether (Brij 35) was considered on the basis of the measured values of contact angle and surface tension. It was shown that the value of the critical surface tension of PTFE surface wetting at the studied system (23.5 mN/m), does not depend on the concentration and composition of the binary mixtures of studied surfactants in water, and it was higer than the surface tension of PTFE (20.2 mN/m). The best wettability of polytetrafluoroethylene (PTFE) by studied aqueous solutions of binary surfactants mixtures occurs at the mixtures concentration corresponding to the critical micelle concentration of their solutions.
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Article 11EN: Ethanol behaviour at the solution-air interface in the presence of Triton X-100 and cetyltrimethylammonium bromide mixture
149-159

Magdalena Bielawska, Anna Zdziennicka


Department of Interfacial Phenomena, Faculty of Chemistry, Maria Curie-Skłodowska University, Maria Curie-Skłodowska Sq. 3,20-031 Lublin, Poland *email: amagdabielawska87@gmail.com

On the basis of the surface tension ( YLV ) data of the aqueous solutions of p-(1,1,3,3-tetramethylbutyl)phenoxypoly(ethylene glycol) (Triton X-100 or TX-100) and cetyltrimethylammonium bromide (CTAB) mixture with ethanol published in our previous paper, the process of ethanol adsorption was investigated. For that reason, the values of Gibbs surface excess concentration of ethanol at the solution-air interface and Gibbs standard free energy of its adsorption at that interface were calculated and compared with those determined for the aqueous solutions of ethanol. The surface excess concentration of ethanol at the solution-air interface was calculated with two different methods. The standard free energy of alcohol adsorption was determined from both the Gu and Zhu and Langmuir equations.
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Article 12EN: Sugar-based surfactants as alternative to synthetic ones
161-168

Diana Mańko, Anna Zdziennicka


Faculty of Chemistry, Department of Interfacial Phenomena, Maria Curie-Skłodowska University M. Curie-Skłodowskiej Sq. 3, 20-031 Lublin, Poland *e-mail: manko_diana@interia.pl

From year to year natural surfactants are gaining ever growing awareness because of their valuable properties (in the absence of negative impact on the environment, as with the use of synthetic surface active agents). In the group of surfactants of natural origin there are surface active agents produced by microorganisms (biosurfactants) or compounds having a natural part (hydrophilic head and/or hydrophobic tail) [1]. This review includes the short characteristic of surfactants with sugar-head group in their structure called sugar-based surfactants. The structure, properties and some applications of these surfactants are described in this paper.
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Volume 69 - 2014

Article 00PL: Spis treści
EN: Table of contents
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Article 01EN: Positronium as a probe of small free volumes in crystals, polymers and porous media
1-110

Tomasz Goworek

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Article 02EN: Thermal behaviour of light lanthanide(III) complexes with 2,3-pyridinedicarboxylic acid
111-126

Zofia Rzączyńska 1, Anna Danczowska-Burdona 1,Marek Drewniak 2


1 Department of General and Coordination Chemistry, Faculty of Chemistry, Maria Curie-Skłodowska University,M. Curie-Skłodowska Sq. 2, 20-031 Lublin, Poland
2 Central Laboratory, Faculty of Chemistry, Maria Curie-Skłodowska University, M. Curie-Skłodowska Sq. 3, 20-031 Lublin, Poland

The lanthanide(III) complexes with 2,3-pyridinedicarboxylate ligand (PDC) were obtained as crystalline compounds from the water solutions. These compounds form the series of Ln2(PDC)3 · nH2O. All compounds are stable in air and insoluble in both water and common organic solvents. The hydrated complexes have been characterized by elemental analysis, thermal analysis (TG/DSC/DTA, and TG−FT-IR), FT-IR spectroscopy and X-ray analysis. 2,3-pyridinedicarboxylates of lanthanides(III) are stable in air below 313−323 K. Upon heating, hydrated complexes lose crystallization and lattice water in two steps. The values of dehydration enthalpy complexes are calculated from the DSC curves. The anhydrous compounds are stable at the temperature from 473 K to about 623 K and when heated they decompose to lanthanide oxides. Thermal and spectroscopic studies are essential for further studies and classification of compounds as MOF-like structures.
Lanthanides, coordination polymer, 2,3-pyridinedicarboxylates, thermal behaviour
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Article 03EN: Aqueous phase fly-ash catalyzed [4+2] Diels-Alder reaction of aryl enones and cyclopentadiene: Synthesis and insect antifeedant activities of aryl bicyclo [2.2.1] heptene-2-yl-methanones
127-140

G. Thirunarayanan


Department of Chemistry, Annamalai University, Annamalainagar-608002, India e-mail: drgtnarayanan@gmail.com

A series containing ten aryl 3-(substituted phenyl) bicyclo [2.2.1] heptene-2-yl-methanone derivatives including 3- (substituted phenyl) bicyclo [2.2.1]hepten-2-yl-(pyren-1-yl)- methanones have been synthesized by aqueous phase fly-ash catalyzed [4+2] Diels-Alder cyclo addition reaction of cyclopentadiene and aryl chalcones. The yields of the methanones are more than 60%. The synthesized methanones are characterized by their physical constants and spectral data. The insect antifeedant activities of synthesized methanones have been studied using Dethler’s leaf-discs bioassay method.
Aqueous phase [4+2]Diels-Alder reaction; 1-pyrenyl chalcones; cyclopentadiene; Bicyclo [2.2.1] heptene-2-yl- Methanones; Insect antifeedant activities
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Article 04EN: Hydroxyapatite catalyzed cyclization of aryl enones: Solvent-free efficient synthesis of some 4-aryl-5,6-dihydro-6-(substituted phenyl)-4H-1,3-oxazine-2-amines
141-158

G. Thirunarayanan


Department of Chemistry, Annamalai University, Annamalainagar-608002, India. e-mail: drgtnarayanan@gmail.com

Some 4-aryl-5,6-dihydro-6-(substituted phenyl)-4H-1,3-oxazine- 2-amine derivatives including 4-(4-methyl-1-naphthyl)-5,6- dihydro-6-(substituted phenyl)-4H-1,3-oxazine-2-amines have been synthesised by hydroxyapatite catalyzed solvent-free cyclization of aryl chalcones and urea using microwave irradiation under solventfree condition. The yields of the oxazines were more than 85%. The synthesised oxazine amines have been characterized by their physical constants, analytical and spectroscopic data.
Oxazine-2-amines, Enones, Hydroxyapatite, Solventfree synthesis
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10.2478/umcschem-2013-0015
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Article 05EN: Perchloric acid catalyzed condensation of amine and aldehydes: Synthesis and antibacterial activities of some aryl (E)-imines
159-179

P. Mayavel, K. Thirumurthy, S. Dineshkumar, G. Thirunarayanana


Department of Chemistry, Annamalai University, Annamalainagar-608002, India.

A series of Schiff’s bases (aryl E-imines) have been derived from the perchloric acid catalyzed condensation of aryl amines and substituted benzaldehydes. The yield of the Schiff’s bases are more than 80%. The synthesized Schiff’s bases are characterized by their physical constants, analytical and spectroscopical data. The antibacterial activities of these Schiff’s bases have been studied using Bauer-Kirby method.
Schiff’s bases, Perchloric acid, IR and NMR spectra, Antibacterial activities
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10.2478/umcschem-2013-0016
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Volume 68 - 2013

Article 00PL: Spis treści
EN: Table of contents
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Article 01EN: Nanoporous silica-based materials for sorption of pharmaceuticals and biomolecules
1-12

Karolina Gdula 1, Mariusz Barczak 2


1 Department of Theoretical Chemistry, Faculty of Chemistry, Maria Curie-Skłodowska University Maria Curie-Skłodowska Sq. 3, 20-031 Lublin karolina.gdula@poczta.umcs.lublin.pl
2 Department of Theoretical Chemistry, Faculty of Chemistry, Maria Curie-Skłodowska University Maria Curie-Skłodowska Sq. 3, 20-031 Lublin mbarczak@poczta.umcs.lublin.pl

Our concern in this paper is to review four kinds of mesoporous silica materials which can be used as potential sorbents for pharmaceuticals. It is known that a continuous development of science, medicine and food industry has an effect on contamination of the natural environment. Moreover, many impurities, such as drugs, vitamins or proteins etc., which get into environment from urban and hospital wastes, can also influence on human organisms. Thus, there is a need to control an amount of those compounds, especially in the natural waters and wastewaters [1-4]. In this work, we present four types of silica materials which can be helpful in water purification by using adsorption process.
nanoporous silica-based materials, adsorption, pharmaceuticals, biomolecules, environmental protection
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10.2478/umcschem-2013-0001
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Article 02EN: Two-dimensional structures composed of cross-shaped molecules adsorbed on solid surfaces – a computational model
13-23

Adam Kasperski 1, Paweł Szabelski 2


1 Department of Theoretical Chemistry, Faculty of Chemistry, Maria Cure-Sklodowska University 3 Maria Curie-Slodowska Sq., 20-031 Lublin, Poland adam@vega.umcs.lublin.pl
2 Department of Theoretical Chemistry, Faculty of Chemistry, Maria Cure-Sklodowska University 3 Maria Curie-Slodowska Sq., 20-031 Lublin, Poland szabla@vega.umcs.lublin.pl

The ability of simple molecular building blocks to form extended ordered patterns by adsorption and self-assembly on solid substrates is an advantageous property that has been widely used to create nanostructured surfaces. In this contribution we demonstrate how the lattice Monte Carlo simulation method can be used to predict morphology of adsorbed overlayers comprising simple functional cross-shaped molecules resembling phthalocyanines and porphyrins. In particular, we focus on the influence of the distribution of active interaction centers within a model crossshaped molecule on the structure of the resulting molecular networks. Additionally, we investigate how using racemic mixtures of input prochiral molecules affects the chirality and porosity of the corresponding ordered patters. The obtained results show that suitable manipulation of the chemistry of cross-shaped building block allows for the controlled creation of largely diversified molecular porous networks.
adsorption, self-assembly, computer simulations, porous overlayers.
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Article 03EN: FT-IR/PAS study of surface EDTA-ZnO interactions
25-31

Marcin Kuśmierz 1, Sylwia Pasieczna-Patkowska 2


1Department of Environmental Chemistry, Faculty of Chemistry, Maria Curie-Sklodowska University, pl. M. Curie-Skłodowskiej 3, 20-031 Lublin, Poland marcin.kusmierz@poczta.umcs.lublin.pl
2Department of Chemical Technology, Faculty of Chemistry, Maria Curie-Sklodowska University, pl. M. Curie-Skłodowskiej 3, 20-031 Lublin, Poland

The interaction of EDTA disodium salt with zinc oxide was investigated by photoacoustic (PA) FT-IR. It was demonstrated that EDTA-III adsorbs on ZnO, and the process mimics behaviour of EDTA-oxide systems, in which IEPS of oxide catalytic supports is higher than 9. Model of the interaction, described in literature, was discussed.
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Article 04EN: Polymer dimensional changes in optical cables
33-49

Mateusz Lutomski 1, Barbara Gawdzik 2


1 Department of Polymer Chemistry, Faculty of Chemistry, Maria Cure-Sklodowska University Gliniana 33, 20-614 Lublin, Poland, Mateusz.lutomski@corning.com
2 Department of Polymer Chemistry, Faculty of Chemistry, Maria Cure-Sklodowska University Gliniana 33, 20-614 Lublin, Poland, bbarbara.gawdzik@poczta.umcs.lublin.pl

Optical cables and fibers are extremely sensitive for mechanical, thermal and environmental conditions, which can affect their optical performance. This article describes known reasons and mechanisms responsible for dimensional changes in temperatures cycling, which can influence optical and mechanical performance and properties of the cables, including internal cable components. Understanding all physical and chemical mechanisms which meet different manufacturing parameters, various materials properties and external conditions allows to control and reduction of cable shrinking and as a result, improving mechanical and optical performance of optical cables.
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10.2478/umcschem-2013-0004
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Article 05EN: Synthesis and characterization of activated carbons obtained from nutshells
51-62

Diana Mańko 1,3, Mariusz Barczak 2, Anna Zdziennicka 1


1 Faculty of Chemistry, Department of Interfacial Phenomena, M. Curie-Skłodowskiej Sq. 3, 20-031 Lublin, Poland
1 Faculty of Chemistry, Department of Theoretical Chemistry Maria Curie-Skłodowska University M. Curie-Skłodowskiej Sq. 3, 20-031 Lublin, Poland
3 manko_diana@interia.pl

Walnut and hazelnut shells were used to prepare activated carbons using potassium hydroxide as an activation agent. The obtained activated carbons presented a specific surface areas of 1661 and 1322 m2/g and pore total volumes of 0.80 and 0.65 cm3/g, respectively. Moreover, the obtained activated carbons presented high quantity of micropores in their structure and that is why they have a great potential for environmental applications and they could be an alternative to commercially available activated carbons from the viewpoint of adsorption capacity. This paper proves that walnut and hazelnut shells have got a large potential as precursors to obtaining activated carbons and they could be successfully converted into a well-developed porous materials by chemical activation.
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10.2478/umcschem-2013-0005
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Article 06EN: Statistical analysis of adsorption experimental data – the influence of the selection of error function on optimized isotherm parameters
63-73

Dawid Myśliwiec 1, Stanisław Chibowski 2


1 Department of Radiochemistry and Colloid Chemistry, Faculty of Chemistry, Maria Curie-Skłodowska University Pl. Marii Curie-Skłodowskiej 3, 20-031 Lublin, Poland d.k.mysliwiec@gmail.com
2 Department of Radiochemistry and Colloid Chemistry, Faculty of Chemistry, Maria Curie-Skłodowska University Pl. Marii Curie-Skłodowskiej 3, 20-031 Lublin, Poland ad.k.mysliwiec@gmail.com Experimental adsorption data were analysed by fitting, stanislaw.chibowski@umcs.lublin.pl

Experimental adsorption data were analysed by fitting them to nonlinear forms of Langmuir and Freundlich isotherms. Optimization of the parameters was performed by nonlinear least square regression with different forms of error function, namely: vertical, horizontal, orthogonal, normal and squared normal. The results showed, that isotherm parameters may be affected by the selection of error function and that they are more sensitive to its’ form in case of Langmuir equation. We did not find any correlation between a type of the function and performance of the regression – procedure requires optimization for every experimental dataset and every model being fitted.
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Article 07EN: Influence of the electrolyte type on the adsorption and electrokinetic properties of the ionic polyamino acids – Cr2O3 system
75-93

Iwona Ostolska, Małgorzata Wiśniewska


Maria Curie-Sklodowska University, Faculty of Chemistry, Department of Radiochemistry and Colloids Chemistry, M. Curie-Sklodowska Sq. 3, 20-031 Lublin, Poland, 1i_ostolska@wp.pl

The influence of a kind of support electrolyte on the ionic polyamino acids adsorption at the chromium (III) oxide – polymer solution interface was investigated. The NaCl and CaCl2 were used as the background electrolytes. In order to determine the effect of the electrolyte, the same value of ionic strength of the test solutions were taken. It was proved that formation of intermolecular and intramolecular complexes in the presence of divalent calcium ions is responsible for essential changes in polymer adsorption.
Related to the ionic character of polyamino acid two different adsorption behaviours can be observed. The increase of the ASP adsorption amount in the presence of calcium ions may be explained by formation of complexes between the dissociated carboxylic groups and Ca2+ ions. The opposite situation takes place in the case of polylysine – the application of CaCl2 results in the dramatic decrease in the polymer adsorption caused by blocking the active sites available for LYS macromolecules. In order to make a comprehensive analysis, the zeta potential and surface charge density measurements were performed taking into account the kind of the background electrolyte. The above-mentioned tests were carried out in the absence and presence of the polyamino acid at two different concentrations – 10 and 100 ppm respectively.
Polyamino acid, polyaspartic acid, polylysine, chromium (III) oxide, polymer adsorption, potentiometric titration, zeta potential.
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10.2478/umcschem-2013-0007
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Article 08EN: Analysis of cosmetic products using different IR spectroscopy techniques
95-106

Sylwia Pasieczna-Patkowska, Tomasz Olejnik


Sylwia Pasieczna-Patkowskaa and Tomasz Olejnik Department of Chemical Technology, Faculty of Chemistry, Maria Curie-Sklodowska University, pl. M. Curie-Skłodowskiej 3, 20-031 Lublin, Poland 1 sylwia.pasieczna@poczta.umcs.lublin.pl

This article describes the application of IR spectroscopic methods in the study of the composition of finished cosmetic products. Four spectroscopic techniques: TS (transmission spectroscopy), PAS (photoacoustic spectroscopy), ATR (attenuated total reflectance) and DRS (diffuse reflectance spectroscopy) were used for this purpose. Tested cosmetic products were of different consistency and application. The choice of spectroscopic techniques was dictated by the physical state and consistency of the sample.
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10.2478/umcschem-2013-0008
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Article 09EN: An application of microemulsion method for synthesis of copper-zinc materials
107-120

Justyna Pawlonka 1, Grzegorz Słowik 2, Wojciech Gac 3, Tadeusz Borowiecki 4


1 Faculty of Chemistry, Department of Chemical Technology, Maria Curie-Sklodowska University 3 M. Curie-Skłodowskiej Square, 20-031 Lublin, Poland ajustyna.pawlonka@gmail.com
2 Faculty of Chemistry, Department of Chemical Technology, Maria Curie-Sklodowska University 3 M. Curie-Skłodowskiej Square, 20-031 Lublin, Poland, grzesiek.slowik@gmail.com
3 Faculty of Chemistry, Department of Chemical Technology, Maria Curie-Sklodowska University 3 M. Curie-Skłodowskiej Square, 20-031 Lublin, Poland, wojtek.gac@poczta.umcs.lublin.pl
4 Faculty of Chemistry, Department of Chemical Technology, Maria Curie-Sklodowska University 3 M. Curie-Skłodowskiej Square, 20-031 Lublin, Poland, tadeusz.borowiecki@umcs.lublin.pl

Microemulsion method was used for preparation of copperzinc mixed oxides. Samples were prepared from the solutions containing zinc and copper nitrates. Sodium carbonate was used as a precipitant and hydrazine as reducing agent. Water-in-oil (W/O) microemulsions were formed by the application of cyclohexane, isopropyl alcohol, and hexadecyltrimethylammonium bromide (CTAB) as surfactant. The aim of the studies was determination of the influence of the sequence of synthesis stages on the formation of materials, their surface and structural properties. Thermal decomposition studies of materials were carried out by infrared spectroscopy. The physicochemical properties were characterized by nitrogen adsorption-desorption method, X-ray diffraction (XRD) and temperature-programmed reduction (TPR).
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10.2478/umcschem-2013-0009
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Article 10EN: Influence of volume drop on surface free energy of glass
121-132

Diana Rymuszka, Konrad Terpiłowski, Lucyna Hołysz


Department of Interfacial Phenomena, Faculty of Chemistry, Maria Curie-Skłodowska University, Lublin, Poland 1d_rymuszka@vp.pl

The aim of the research was to determine how the drop size affects the contact angle values and determine its optimal size for further contact angle measurements and comparison of the contact angle values measured for three probe liquids (water, formamide, diiodomethane) on the glass surface using the: sessile drop and tilting plate methods. Next, using the measured contact angles, the total surface free energy and its components were determined from the van Oss et al. (Lifshitz-van der Waals acid- base component, LWAB), Owens-Wendt, Neumann and contact angle hysteresis (CAH) approaches. The studies showed, that drop size is very important for contact angle measurements and consequently, for surface free energy estimation.
contact angle, surface free energy
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10.2478/umcschem-2013-0010
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Article 11EN: Enhancing the separation of enantiomers in adsorbed overlayers: a Monte Carlo study
133-141

Aleksandra Woszczyk 1, Paweł Szabelski 2


1 Department of Theoretical Chemistry, Maria Curie-Sklodowska University, M. Curie-Sklodowskiej Sq.3, 20-031 Lublin, Poland ola_w@vega.umcs.lublin.pl
2 Department of Theoretical Chemistry, Maria Curie-Sklodowska University, M. Curie-Sklodowskiej Sq.3, 20-031 Lublin, Poland szabla@vega.umcs.lublin.pl

The influence of external factors on the chiral resolution of enantiomers in adsorbed overlayes has been especially interesting form the perspective of creation of chiral surfaces. Chiral segregation of this type can be induced or enhanced, for example, by an external unidirectional fields such as magnetic or electric field. To explore the effect of an external field on the 2D chiral resolution of model enentiomers we performed cannonical Monte Carlo simulations on a square lattice of equivalent adsorption sites. The adsorbed molecules which are sensitive to the external field, were assumed to consist of four identical segments and they were able to adopt four possible orientations on a square lattice. Shortrange segment-segment interactions limited to the nearest neighbours on the lattice were allowed to account for the intermolecular interactions. The calculations were performed for two exemplary molecular structures and the strength of the external field was gradually increased in each case. The preliminary results described herein demonstrate that continuously changed external fields can induce chiral resolution of enantiomers of appropriate geometry. The insights from this study can be useful in developing strategies for 2D chiral separations in which external stimuli are used.
adsorbed overlayers, chiral resolution, selfassembly, external field
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Article 99PL: Recenzenci prac zamieszczonych w tym tomie
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Volume 67 - 2012

Article 01EN: Some aspects on the history of thermal analysis
1-29

Erich Robens 1, Shanath Amarasiri A. Jayaweera 2


1 Schlesierstraße 5, D-61381 Friedrichsdorf, Germany. Formerly: Battelle-Institut e.V., Frankfurt am Main, Germany, erich.robens@t-online.de
2 42 Tanton Road, Stokesley, Middlesbrough, TS9 5HR, UK, Formerly: Teesside University, School of Science & Engineering, Middlesbrough, UK, saajayaweera@yahoo.co.uk

The short survey covers invention and development of thermal and related analytical methods: calorimetry, thermoporometry, dilatometry, thermogravimetry, sorptometry, hygrometry.
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10.2478/v10063-012-0001-x
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Article 02EN: The limits of weighing
31-43

Shanath Amarasiri A. Jayaweera 1, Erich Robens 2, Andrzej Dąbrowski 3


1 42 Tanton Road, Stokesley, Middlesbrough, TS9 5HR, UK, Formerly: Teesside University, School of Science & Engineering, Middlesbrough, UK, saajayaweera@yahoo.co.uk
2 Schlesierstraße 5, D-61381 Friedrichsdorf, Germany. Formerly: Battelle- Institut Frankfurt am Main, Germany, erich.robens@t-online.de
3 Uniwersytet Marii Curie-Skłodowskiej, Pl. Marii Curie-Skłodowskiej 5, PL - 20-032 Lublin, Poland, andrzej.dabrowski@umcs.lublin.pl

Mass determination in the gravitational field covers a wide measuring range and, as a comparative method, facilitates very sensitive measurements. However, gravity is a very weak force. First by application of acceleration fields and with mass spectrometric methods, the measuring range could be extended towards atomic and sub-atomic masses. There are only practical limits of weighing heavy masses. The mass of celestial objects can be determined by means of Kepler’s Laws.
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10.2478/v10063-012-0002-9
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Article 03EN: Solid Fly-ash:PTS catalyzed synthesis, spectral studies and antimicrobial activities of some 1,3-diarylpropenones
45-77

R. Arulkumaran 1, G. Vanangamudi 1, D. Kamalakkannan 1, R. Sundararajan 1,S. Vijayakumar 1, K. Thirumurthy 2, P. Mayavel 2, G. Thirunarayanan 2


1 PG & Research Department of Chemistry, Government Arts College, C-Mutlur, Chidambaram-608102, India
1 Department of Chemistry, Annamalai University, Annamalainagar-608002, India, drgtnarayanan@gmail.com

The green catalyst Fly-ash:PTS has been prepared and characterized by IR and SEM analysis. Using this catalyst some aryl chalcones have been synthesized by aldol condensation of aryl methyl ketone and substituted benzaldehydes. It has been observed that this reaction yields more than 85% of the product. These chalcones have been characterized by their physical constants and spectral data following the procedures published in literature. The effect of substituents on the spectral data of the chalcones, synthesized, has been studied using single and multi-regression analysis with Hammett equation. The antibacterial and antifungal activities of these chalcones have been studied using Bauer-Kirby method.
Chalcones; Greener synthesis, Fly-ash:PTS; UV spectra, IR spectra, NMR spectra, Hammett correlation, antibacterial activity, antifungal activity
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10.2478/v10063-012-0003-8
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Article 04EN: Fly-ash:H2O Assisted Aldol Condensation: Effect of Solvents on the Synthesis of Some Aryl (E) 2-propen-1-ones
79-121

G. Thirunarayanan


Department of Chemistry, Annamalai University, Annamalainagar-608002, India, drgtnarayanan@gmail.com

Some series of aryl (E) 2-propen-1-ones have been synthesized by Fly-ash:H2O catalyzed aldol condensation of aryl methyl ketones and substituted benzaldehydes at reflux condition in atmospheric pressure. The yields of chalcones are higher than 60%. These chalcones were characterized by their physical constants and spectral data, for known compounds their purities were checked with the physical constants and spectral data earlier published in the literature. The effects of solvents on the product have been studied.
Aryl (E) 2-propen-1-ones, Fly-ash:H2O, IR and NMR spectra, Solvent effects
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10.2478/v10063-012-0004-7
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Article 05EN: A Modified Protocol for the Aldehyde Olefination Reaction using Ionic liquid as Reaction Medium
123-129

Vivek Srivastava


Pure Science: Chemistry, NIIT University, Neemrana, NH-8 Delhi-Jaipur Highway, District: Alwar, Rajasthan – 301 705, vivek.srivastava.chem@gmail.com

[Ru(COD)Cl2]n /CuCl2.2H2O/LiCl catalytic system was found highly active in ionic liquid medium for aldehyde olefination reaction in term of yield and selectivity. Aromatic aldehydes with more electron-donating groups on the phenyl ring gave higher yield than those with electron withdrawing groups. Reduced reaction time as well as 5 times recycling of catalytic system reflects the importance of this modified process.
[Ru (COD) Cl2]n /CuCl2.2H2O/LiCl, Ionic liquid, Aldehyde olefination.
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10.2478/v10063-012-0005-6
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Article 06EN: An effective scaling frequency factor method (ESFF): review and local factors transferability problem
131-153

Karolina Gdula, Mariusz Barczak, Piotr Borowski


Faculty of Chemistry, Maria Curie-Skłodowska University, Maria Curie-Sklodowska sq. 3, 20-031 Lublin, Poland

Scaling procedures are known to reproduce very accurate vibrational spectra provided that multiparameter scaling in conjunction with high-quality force fields is carried out. In contrast to purely theoretical approaches (variational and perturbational), they are applicable to large systems. In this work, a brief review of the scaling procedures is given. The emphasis is put on the recently proposed effective scaling frequency factor (ESFF) method [Chem. Phys. Lett., 446, 191, (2007), J. Mol. Spectr., 264, 66, (2010)] – the multiparameter frequency scaling method providing better scaled frequencies than the well-established scaled quantum mechanical (SQM) force field approach. In addition, the results of our calculations on the benzene-based related systems, i.e., benzene and most of its methyl derivatives, are presented. The calculations concern the middle- and low-frequency range of the vibrational spectra, where strong mixing of the local vibrations often takes place. The factors transferability problem is discussed.
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Article 07EN: The use of chromatographic and spectroscopic (colometric) methods for evaluation of quercetine in dietary supplements of plant origin
155-161

Małgorzata Kostecka


Department of Chemistry, University of Life Sciences in Lublin, ul. Akademicka 15, 20-950 Lublin, tel. (+48-81) 445 68 46, julka-portal@wp.pl

Recent years have witnessed a rapid increase in demand for dietary supplements which can be purchased over the counter and without medical consultation. They are widely advertised as panacea for all ailments that afflict the contemporary consumer. Products containing extracts from native and tropical plants as well as herbs have a growing share of the supplement market.
TLC is a simple and inexpensive method that can be used in preliminary analyses of product quality. Thin layer chromatography is also an effective technique for isolating biologically active substances from complex pharmaceutical products and supplements. Quantitative analysis shows that quantitative and qualitative inaccuracies and misstatements may occur in the case of dietary supplements.
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10.2478/v10063-012-0007-4
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Article 08EN: Stability indicating HPLCc method for impurities estimation of nevirapine in extended release tablet dose
163-173

Ch. Venkata Reddiah 1, P. Rama Devi 2, K. Mukkanti 3, P. Srinivasu 1


1 Analytical Development, Unit-III,E.O.U,Block-B, Hetero Drugs Ltd., Jeedimetla,Hyderabad-500055, India, Venkat.re2007@gmail.com
2 Analytical Research and Development , HRF,Balanagar, Hyderabad-500018, India.
3 J.N.T.U Institute of Science and Technology, Hyderabad-500072, India.

A novel, sensitive and selective Reverse phase High performance liquid chromatographic method was developed for quantitative determination of Nevirapine in its Extended Tablet dosage forms. The synthetic non-nucleoside reverse transcriptase inhibitor analogues (NNRTI) Nevirapine form one of the Extended dosage in HIV. It belongs to a group of anti-HIV medicines called non-nucleoside reverse transcriptase inhibitors (NNRTIs). The method is applicable to the quantification of related compounds of Nevirapine forming one of the fixed Extended dosage. Chromatographic separation of Nevirapine from the possible impurities and the degradation products was achieved on an Supelcosil LC-ABZ 150 x 4.6 mm, 5.0μm column; Ammonium Orthophosphate pH 5.0 as mobile phase A and Acetonitrile taken as mobile phase B in the ratio (85 : 15). The flow rate was 1.0 mL/min, and the detection was done at 220 nm. The above developed HPLC method was further subjected to hydrolytic, oxidative, photolytic and thermal stress conditions. The performance of the method was validated according to the present ICH guidelines for specificity, limit of detection, limit of quantification, linearity, accuracy, precision, and ruggedness.
Nevirapine XR, force degradation studies, validation
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  4. N. Kaul, H. Agarwal, A.R. Paradkar, and K.R. Mahadik, Talanta, 62, 843, (2004),
  5. K. Namita, K. Sateesh, and P. Ramesh, Anal. Chimica. Acta, 570, 41, (2006).
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  15. United States Pharmacopeia, United States Pharmacopoeia Convention, Rockville, MD, pp. 3539–3542, (2008).
  16. ICH Guidance on Analytical Method Validation, [in:] Proc. Int. Convention on Quality for the Pharmaceutical Industry, Toronto, Canada, September (2002)
  17. R.L. Murphy, J. Montaner, Drug Evaluations Anti-infectives: Nevirapine: A review of its development, pharmacological profile and potential for clinical use, Expert Opin. Investig. Drugs, 5, 1183, (1996), http://dx.doi.org/10.1517/13543784.5.9.1183.
  18. R.L. Murphy and J. Montaner. Nevirapine: a review of its development, pharmaceutical profile and potential for clinical use. Exp. Opin. Invest. Drugs 5, 1183, (1996).
  19. The year’s top ten medical advances. Health Mag. January/February: 132, (2000).
  20. R.M. Dinallo, W.C. Davidson, and G.E. Hansen. The characterization of synthetic by-products by B/E linked scanning and high-resolution thermospray mass spectrometry. Bio. Mass Spectrom., 20, 268, (1991).
  21. K.A. Cohen, J. Hopkins, R.H. Ingraham, C. Pargellis, J.C. Wu, D.E.H. Palladino, P. Kinkade, T.C. Warren, S. Rogers, J. Adams, P.R. Farina, and P.M. Grob. Characterization of the binding site for nevirapine (BI-RG-587), a nonnucleoside inhibitor of human immunodeficiency virus type-1 reverse transcriptase. J. Bio. Chem. 266, 14670, (1991).
  22. D.E.H. Palladino, J.L. Hopkins, R.H. Ingraham, T.C.Warren, S.R. Kapadia, G.J. van Moffaert, P.M. Grob, J.M. Stevenson, and K.A. Cohen. High-performance liquid chromatography and photoaffinity cross-linking to explore the binding environment of nevirapine to reverse transcriptase of human immunodeficiency virus type-1. J. Chromatogr. A, 676, 99, (1994).
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10.2478/v10063-012-0008-3
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Volume 66 - 2011

Article 01EN: The 65th Birthday of Professor Dobiesław Nazimek
1-3

Janusz Ryczkowski

10.2478/v10063-011-0001-2
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Article 02EN: Transformation of alumina supported nickel catalysts during hydrodechlorination of 1,2-dichloroethane
4-11

W. Juszczyk 1, Z. Karpiński 1;2


1 Institute of Physical Chemistry of PAS, ul. Kasprzaka 44/52, 01-224 Warszawa, Poland
2 Faculty of Mathematics and Natural Sciences - School of Science, Cardinal Stefan Wyszyński University, ul. Wóycickiego 1/3, 01-938 Warszawa, Poland

Our previous work with Sibunit carbon supported nickel catalysts investigated in the reaction of 1,2-dichloroethane hydrodechlorination showed the transformation of nickel to an fcc NiCx solution and/or even to an hcp Ni3C carbide phase during reaction. Carbon entering to nickel was considered to originate from the organic molecule, not from the carbon support. To substantiate this interpretation we decided to carry out the title reaction in the presence of alumina supported nickel catalysts. Hydrodechlorination of 1,2-dichloroethane performed on differently metal loaded Ni/Al2O3 catalysts resulted in a massive carbiding of nickel, leading to the Ni3C carbide phase. This effect was better marked for the catalysts with a higher Ni loading (≥2 wt.%). However, for very high Ni loading (20 wt.%) characterized by bigger metal crystallites (~30 nm), only a portion of Ni was carbided.
10.2478/v10063-011-0002-1
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Article 03EN: Synthesis of CrOx/Al2O3 catalyst in sol-gel conditions
12-22

P. Kirszensztejn, R. Przekop


Faculty of Chemistry, Adam Mickiewicz University, Grunwaldzka 6, 60-780 Poznań, Poland

A series of CrOx/Al2O3 samples with various Cr/Al molar ratios (0.1-1.0) have been synthesized by the sol-gel technique from Al(C3H7O)3 (aluminium isopropoxide) and chromic acid precursors. The synthesis applied allowed obtaining the final product in monolithic (nonfractured upon drying) form with no use of drying control chemical additives. All samples are characterized by thermal analysis, XRD, and TEM. The low temperature nitrogen adsorption measurements indicate the presence of mesopores. The use of the sol-gel technique permitted a high degree of homogeneity of binary systems up to the Cr/Al molar ratio of 0.5.
10.2478/v10063-011-0003-0
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Article 04EN: Li-ion batteries for electric vehicles
23-36

J. Molenda


Department of Hydrogen Energy, Faculty of Energy and Fuels, AGH University of Science and Technology, al. Mickiewicza 30, 30-059 Kraków, Poland

This paper presents brief outlook for Li-ion battery market for electric vehicles in comparison with that for portable electronics. The second part of the article presents electrochemical model as well as the main points of material issues in lithium batteries. Review of currently available and possible for future application cathode materials is provided. Stress is placed on importance transport properties of materials.
10.2478/v10063-011-0004-z
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Article 05EN: Synthesis and characterization of Pt/CeOx systems for catalytic CO oxidation reaction
37-46

R. J. Wróbel 1, S. Łagonda 1, U. Narkiewicz 1, R. Pełech 2, S. Becker 3, L. Szymaszkiewicz 4


1 Institute of Organic Chemical Technology, West Pomeranian University of Technology
2 Institute of Organic Chemical Technology, Institute of Chemical and Environment Engineering, Pulaskiego 10, 70-322 Szczecin, Poland
3 Chemisches Institut, Otto-von-Guericke Universität, Universitätsplatz 2, 39106 Magdeburg, Germany
4 Szczecin University, Institute of Mathematics, Wielkopolska 15, 70-451 Szczecin, Poland

Four different ceria supported catalyst were prepared by impregnation method with Pt(NO3)2 solution. The two supports are commercially available (MaTeck) and the other two were prepared by precipitation and microwave assisted hydrothermal method (MAH) respectively. The phase composition and average crystallite size of the catalysts were characterised with XRD technique. Finally the catalytic activity in CO oxidation reaction were determined in plug flow reactor in temperature range 300-900 K with 1 K resolution. The catalysts obtained in both precipitation and MAH methods exhibit catalytic activity at room temperature whereas catalysts obtained on MaTeck supports are not active at those conditions. In turn, catalysts based on MaTeck support are more active in temperature range 420-700 K. The different activities are attributed to difference in average crystallite sizes and in support morphology.
10.2478/v10063-011-0005-y
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Article 06EN: Thermal stability and pollutant adsorption efficiency of nanocomposites consisted of clay and polymeric quaternary ammonium salts
47-59

P. Natkański 1, P. Kuśtrowski 1, A. Kochanowski 1, A. Białas 1, Z. Piwowarska 1, M. Michalik 2


1 Faculty of Chemistry, Jagiellonian University, Ingardena 3, 30-060 Kraków, Poland
1 Institute of Geological Sciences, Jagiellonian University, Oleandry 2a, 30-063 Kraków, Poland

Polymer/layered silicate nanocomposites based on polymeric quaternary ammonium salts (ionenes) intercalated into the interlayer galleries of montmorillonite were synthesized. Zeta potential measurements were conducted to determine the amount of ionenes required to neutralize the negative charge of clay. The composition and structure of the obtained nanocomposites were examined by elemental analysis, ATR-FTIR and XRD. High dye sorption capacity was observed for the composite containing ionene 6,2.
10.2478/v10063-011-0006-x
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Article 07EN: Oxidation of methane over Ru/clinoptilolite catalysts
60-66

M. Kuśmierz


Department of Environmental Chemistry, Faculty of Chemistry, Maria Curie-Skłodowska University, M. Curie-Skłodowska Sq. 3, 20-231 Lublin, Poland.

This paper describes the activity of ruthenium catalysts based on clinoptilolite, prepared by the ion exchange method, in the reaction of total methane oxidation. It has been shown thath the activity of the catalysts higher than metal oxide based ones, and is directly proportional to ruthenium loading.
10.2478/v10063-011-0007-9
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Article 08EN: The studies of the natural zeolite - clinoptylolite in reduction of nitrogen
67-80

W. Ćwikła-Bundyra


Institution of Environmental Chemistry, UMCS Pl. Marii Skłodowskiej - Curie 3, 20-031 Lublin, Poland

This article presents the results of the research in the area of the possibilities of the utilization of natural zeolite- clinoptylolite for reduction of oxide nitrogen. The clinoptylolite type zeolite has the unique structure, high resistance against hydrothermal conditions and the ability to form strong acid centers. Various kinds of metals ions were inserted into the samples of zeolite using ion-exchange method. The effect of metals content was shown for clinoptylolite matrix and related to the performance of its pure hydrogen form. A comparison of the catalytic properties of Cu-, Co-, Fe-, Mn- and Ni-CLI was carried out for the NO reduction with methane. A eries of doubly substituted CoCu-CLI catalysts with different metal loading were studied too. Over the copper and cobalt-CLI was observed high nitric oxide conversion, especially at temperatures between 400 and 500°C. It was confirmed that the copper-cobalt-CLI catalysts have higher activity and durability than catalysts composed of iron, nickel and manganese supported on clinoptylolite. Moreover, the iron, nickel and manganese containing catalysts produced more nitrous oxide than nitrogen. The presence of both copper and cobalt species seems to be an indispensable condition for the high activity and selectivity in the NO reduction.
10.2478/v10063-011-0008-8
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Article 09EN: Surfactants removal from water and wastewater using Co modified TiO2/Al2O3 photocatalysts
81-93

B. Czech


Faculty of Chemistry, Department of Environmental Chemistry, Maria Curie-Skłodowska University, pl. M. Curie-Skłodowskiej 3, 20-031 Lublin, Poland

The photocatalytic oxidation of Triton X-100, its oxidation products: polyethylene glycol, phenol and also commercially available wash-up liquid in water in the band reactor of our construction with supported TiO2 catalysts was studied. As a photocatalyst Co-TiO2/Al2O3 was used. The main aim of these studies was the determination of catalytic activity of Co-TiO2/Al2O3 in pollutants removal from water and the effect of O2, H2O2 or UV addition on the photooxidation. It was found that the H2O2 addition has a detrimental influence on aerated wastewater containing surfactants, and UV has an increasing effect on process. 2 hours treatment of water is enough to obtain a significant COD reduction of all studied pollutants.
10.2478/v10063-011-0009-7
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Article 10EN: Scientific co-operation with professor Nazimek
94-105

J. Ryczkowski


Department of Chemical Technology, University of Maria Curie-Skłodowska, Pl. M. Curie-Sklodowskiej 3, 20-031 Lublin, Poland

In present paper there will be discussed examples of author's scientific co-operation with professor Nazimek. Generally all of them are from the area of heterogeneous catalysis including high dispersed metal phase mostly in the hydrogenolysis reactions of simple alkanes.
10.2478/v10063-011-0010-1
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Article 11EN: Investigations on hydrogenation of selected organic sulfur compounds on the Ni-Mo/Al2O3 catalyst in terms of natural gas desulfurization
106-116

K. Antoniak 1, P. Kowalik 1, R. Narowski 1, M. Konkol 1, J. Ryczkowski 2


1 Catalyst Department, Fertilizer Research Institute, Al. Tysiąclecia Państwa Polskiego 13A, 24-110 Puławy, Poland
2 Faculty of Chemistry, Department of Chemical Technology, Maria Curie-Sklodowska University, Pl. M. Curie-Sklodowskiej 3, 20-031 Lublin, Poland

Technological problems of natural gas desulfurization in syngases manufacturing plants have been discussed and the results of investigations on the activity of the model Ni-Mo/Al2O3 catalyst in hydrogenation of selected sulfur compounds have been presented. The HDS reaction rate is dependent on a compound structure. The hydrogenation rate on the Ni-Mo/Al2O3 catalyst for the given sulfur compound increases in the order: CS2(CH3)2S>C4H10S>C2H6S2C4H4S.
10.2478/v10063-011-0011-0
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Article 12EN: The effect of tetramethylthiourea on the Zn2+ ions electroreduction in the presence of different detergents
117-128

M. Klin, J. Nieszporek, D. Gugała-Fekner, D. Sieńko, J. Saba


Faculty of Chemistry, Maria Curie-Skłodowska University, Maria Curie-Skłodowska Sq.3, 20-031 Lublin, Poland

The effect of the mixed adsorption layers: tetramethylthiourea and chosen detergent on the Zn2+ ions electroreduction is described. The detergents concentration was 7.5·10-4 M, which was lower of its critical micellation point. Three detergents: cationic, neutral and anionic were chosen for this study. First two detergents inhibited the Zn2+ ions reduction at mercury electrode, the last detergent accelerated this process. Tetramethylthiourea eliminated the inhibiting effect of the detergent and accelerated the studied process stronger than in the detergents absence. Standard rate constants of Zn2+ ions electroreduction were determined by cyclic voltammetry and impedance measurements
10.2478/v10063-011-0012-z
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Article 13EN: Selected aspect in the separation of inorganic and organic species on ion exchangers and sorbents of various types
129-146

Z. Hubicki, M. Majdan, M. Gęca, A. Gładysz-Płaska, D. Kołodyńska, M. Makarska-Białokoz, M. Wawrzkiewicz, A. Wołowicz, G. Wójcik


Department of Inorganic Chemistry, Faculty of Chemistry, Maria Curie-Skłodowska University, Maria Curie-Skłodowska Sq. 2. 20-031 Lublin, Poland

In the paper the example papers from the Department of Inorganic Chemistry are presented. They are connected with the research of sorption and separation of inorganic and organic species on ion exchangers and sorbents of various types are presented. The main subjects include physicochemical studies of metal ions removal on anion exchangers, chelating and modified ion exchangers as well as zeolites, sorption and separation of rare earth elements, recovery of noble metal particularly from chloride solutions by ion exchange or extraction method, application of the anion exchangers of various types in dyes removal from aqueous solutions and wastewaters and chemistry of porphyrins in the aspect of environmental protection.
10.2478/v10063-011-0013-y
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Article 14EN: Solute permeation through lipid membrane: Statistical Rate Theory approach
147-158

W. Piasecki 1, R. Charmas 2


1 Department of Biochemistry, Faculty of Physical Education and Sport in Biala Podlaska, The Josef Pilsudski University of Physical Education in Warsaw, Poland
2 The State College of Computer Science and Business Administration in Łomża, Poland

A new model describing transport across lipid membrane was developed based on the Statistical Rate Theory (SRT) of interfacial transfer. In our calculations we replaced lipid membrane with well-defined octanol membrane. According to SRT the rate of solute transfer across water/octanol interface depends on the ratio of solute concentration in the both phases and the water/octanol partition coefficient. In the case of thick membranes and thick diffuse layers our model predicts almost linear dependence of flux on concentration gradient. However, for thin membranes and thin diffuse layers flux becomes nonlinear function of concentration gradient, especially for more polar solutes and higher gradients.
10.2478/v10063-011-0014-x
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Volume 65 - 2010

Article 01EN: Synergistic effects in hydrodechlorination of organic compounds catalyzed by metals
1-8

M. Bonarowska 1, A. Śrębowata 1, Z. Karpiński 1;2


1 Institute of Physical Chemistry of PAS, ul. Kasprzaka 44/52, 01-224 Warszawa, Poland
1 Faculty of Mathematics and Natural Sciences - School of Science, Cardinal Stefan Wyszyński University, ul. Wóycickiego 1/3, 01-938 Warszawa, Poland

The search for the most suitable hydrodechlorination catalysts should consider both the C-Cl bond strength in a molecule subjected to reaction and the metal-chlorine bond, which should be neither too strong nor too weak. An improvement of Pd- and Pt-based catalysts can be achieved by alloying with metals which bind chlorine even less strongly, e.g. with gold. Addition of platinum to palladium would also be beneficial because of metal-chloride bond energy considerations. Analogous effects occur in the hydrodechlorination of dichlorodifluoromethane and 1,2-dichloroethane, the molecules characterized by stronger carbon-chlorine bonds.
10.2478/v10063-010-0001-7
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Article 02EN: Transmission Electron Microscopy as indispensable tool for imaging and chemical characterization of heterogeneous catalysts
9-19

L. Kępiński


Division of Nanomaterials Chemistry and Catalysis, Institute of Low Temperature and Structure Research, Polish Academy of Sciences, Okólna 2, 50-412 Wrocław, Poland

Transmission Electron Microscopy (TEM) and its mutation Scanning Transmission Electron Microscopy (STEM) is one of the most important methods providing unique information on structure and chemistry of solid catalysts at length scale down to level. The principal reason is its high spatial resolution (below 0.1 nm) but also universality, i.e., ability of observation of both images and diffraction patterns of individual nanometer size objects. Recent advances in TEM in particular application of image and beam correctors, possibility of studying specimens at non vacuum conditions (environmental TEM) and possibility of dynamic (time resolved) studies even further broadened the applicability of the method in catalysis.
10.2478/v10063-010-0002-6
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Article 03EN: Decomposition of ethylene on iron catalyst to obtain carbon nanotubes and the way of their purification
20-30

I. Pełech, K. Owodziń, U. Narkiewicz


Institute of Chemical and Environmental Engineering, West Pomeranian University of Technology, Pułaskiego 10, 70-310 Szczecin, Poland

This paper describes preparation and characterization of carbon nanotubes obtaining using ethylene as a carbon source and iron as catalyst. Additionally purification procedure of carbon nanomaterials is presented. Purification was conducted in two stages. In the first one hydrogen or air was used in order to gasify unwanted carbon forms. In the second one - various reactants (nitric, hydrochloric or nitro-hydrochloric acids) were applied to remove metal particles. Obtained materials were characterized using X-ray diffraction, transmission electron microscopy and thermogravimetry.
10.2478/v10063-010-0003-5
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Article 04EN: Surface modification of bioceramics by PEG grafting
31-44

K. Adamska, M. Woźniak, A. Voelkel


Institute of Chemical Technology and Engineering, Poznań University of Technology, PL. M. Skłodowskiej-Curie 2, 60-965 Poznań, Poland

Surface modification of Hydroxyapatite (HAp) and β-Tricalcium phosphate (β-TCP) powders was performed using hexamethylene diisocyanate (HMDI) as a coupling agent. Polyethylene glycol (Mw = 2000) was grafted to the surface of these ceramic materials. Different methods were used to characterize modified surfaces. Fourier transform infrared (FT-IR) and Attenuated Total Reflection Fourier Transform Infrared (FTIR/ATR) technique analyses confirmed the modification reaction on HAp and β-TCP surfaces. BET isotherm analysis showed the changes in textural properties of materials after modification. Elemental analysis was performed to confirm a presence of selected elements from modifier and coupling agent. Examination of dispersion stability of materials in different solvents show better stability for samples of β-TCP than HAp.
10.2478/v10063-010-0004-4
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Article 05EN: Studies of Zn-Al-Ce mixed oxides as catalysts for diesel soot combustion
45-54

L. Chmielarz 1, A. Węgrzyn 1, A. Kowalczyk 1, S. Witkowski 1, R. I. Walton 2, A. Matusiewicz 3


1 Faculty of Chemistry, Department of Chemical Technology, Jagiellonian University, Ingardena 3, 30-060 Kraków, Poland
1 Department of Chemistry, The University of Warwick, Coventry, CV4 7AL, UK
1 Glass and Building Materials Division, The Institute of Ceramics and Building Materials, Cementowa 8, 31-983 Kraków, Poland

A series of Zn-Al-Ce mixed oxides was synthesized by a co-precipitation method. The obtained samples were characterized with respect to composition (XRF), structure (XRD, FT-IR) and texture (BET). Zn-Al-Ce mixed oxides were tested as catalysts of diesel soot combustion. The best catalytic activity was found for Zn2Ce oxide system, which operated in the temperature range of 350-500°C.
10.2478/v10063-010-0005-3
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Article 06EN: A study of iron catalyst for ammonia synthesis by electron spectroscopy methods
55-67

W. Arabczyk, D. Moszyński, M. Dłużewska


Institute of Chemical and Environment Engineering, West Pomeranian University of Technology, Szczecin ul. Pułaskiego 10, 70-322 Szczecin, Poland

A concise review of former studies into iron catalyst using electron spectroscopy methods is presented. A model of iron catalyst's surface, the so-called double layer model is presented. On the basis of this model both a method of determining surface content of a real iron catalyst and a method of determining the rate of potassium surface diffusion were developed. A double layer model was used to interpret thermal stability loss of potassium atoms on iron surface subjected to sulphur compounds' exposure.
10.2478/v10063-010-0006-2
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Article 07EN: Determination of the active phase structure in CuO/γ-Al2O3 catalysts by TPR kinetic model discrimination
68-78

P. Kuśtrowski 1, A. Białas 1, J. Surman 1, B. Dudek 1


1 Faculty of Chemistry, Department of Chemical Technology, Jagiellonian University, Ingardena 3, 30-060 Kraków, Poland

The results of temperature-programmed reduction with hydrogen of alumina supported copper oxide catalysts were used to find the best model describing the kinetics of Cu ions' reduction. On the basis of the rate determining step of this reaction the structure of copper oxide was revealed. This kinetic approach was compared with BET and UV-vis-DRS results. The catalytic activity of various copper oxide forms was tested in toluene combustion.
10.2478/v10063-010-0007-1
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Article 08EN: The effect of calcination temperature on properties and activity of Cu/ZnO/Al2O3 catalysts
79-87

P. Kowalik, W. Próchniak


Catalysts Department, Fertilizers Research Institute, Al. Tysiąclecia Państwa Polskiego 13A, 24-110 Pulawy, Poland

The paper presents the results of the investigation on the influence of calcination temperature of Cu-Zn-Al catalyst precursor, on physicochemical properties and catalytic activity for water gas shift reaction. A model precursor of chemical composition corresponding with a typical commercial catalyst and prepared by coprecipitation method was studied. It has been shown that the temperature of calcination step determines the surface properties of the final catalyst, the active phase dispersion, and thus significantly affects the catalytic activity.
10.2478/v10063-010-0008-0
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Article 09EN: The study on alkali-promoted Co-Mo/Al2O3 catalysts for water-gas shift process
88-95

K. Antoniak 1, P. Kowalik 1, J. Ryczkowski 2


1 Catalysts Department, Fertilizers Research Institute, al. Tysiąclecia Państwa Polskiego 13A, 24-110 Puławy, Poland
2 Faculty of Chemistry, Department of Chemical Technology, Maria Curie-Sklodowska University, Pl. M. Curie-Sklodowskiej 3, 20-031 Lublin, Poland

The following contribution presents the results of studies on the effects of alkali metals on the physicochemical properties and the effectiveness of a Co-Mo/Al2O3 catalyst for the water gas shift reaction. It has been shown that the addition of alkali metals modifies the properties of Co-Mo catalysts, resulting in a significant increase in activity of catalysts in water gas shift reaction. The greatest effect was observed in the case of sodium-promoted reaction.
10.2478/v10063-010-0009-z
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Article 10EN: Effectiveness diffusion coefficient in nickel catalyst grain determined by measurements of catalytic reaction rate
96-99

K. Stołecki, K. Michalska, R. Narowski, A. Gołębiowski


Fertilizers Research Institute Puławy

10.2478/v10063-010-0010-6
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Article 11EN: The influence of gold on the properties of silica mesoporous materials
100-120

W. Gac 1, S. Pasieczna-Patkowska 1, L. Kępiński 2


1 Department of Chemical Technology, University of Maria Curie-Skłodowska, Maria Curie-Sklodowska Sq. 3, 20-031 Lublin, Poland
2 Institute of Low Temperature and Structure Research, PAS, Okólna 2, 55-422 Wrocław, Poland

The properties of gold modified silica mesoporous materials were investigated on the successive preparation stages. Samples were obtained by the direct introduction of HAuCl4 aqueous solution to the synthesis mixture of silica. It was stated that partial substitution of -Cl with -OH ligands occurred in the diluted solutions of HAuCl4. The replacement of -Cl with -Br groups in gold complexes took place in the synthesis mixture containing hexadecyltrimethylammonium bromide surfactant molecules. It was found that gold species influenced the removal of organic templates from the channels of silica materials. Pore arrangement was not strongly distorted by the presence of small amounts of gold. Heat treatment led to the pronounced changes of the nature of gold species.
10.2478/v10063-010-0011-5
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Article 12EN: Spectroscopic studies of alumina supported nickel catalysts precursors: Part II - catalysts prepared from alkaline solutions
121-131

S. Pasieczna-Patkowska, J. Ryczkowski


Faculty of Chemistry, Department of Chemical Technology, Maria Curie-Skłodowska University, Maria Curie-Skłodowska Sq. 3, 20-031 Lublin, Poland

Nickel alumina supported catalysts were prepared from alkaline solutions of hexaamminenickel nitrate by CIM and DIM methods (classical and double impregnation, respectively). The catalysts exhibited different nickel species due to the existence of various metal-support interaction strengths. As a consequence, the reducibility and other surface properties changed as a function of the preparation method. The aim of this work was to study the interaction between the metal precursor and alumina surface by means of FT-IR (Fourier transform infrared) and FT-IR/PAS (FT-IR photoacoustic spectroscopy).
10.2478/v10063-010-0012-4
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Article 13EN: Scientific co-operation with professor Borowiecki
132-154

J. Ryczkowski


Department of Chemical Technology, University of Maria Curie-Skłodowska, pl. M. Curie-Sklodowskiej 3, 20-031 Lublin, Poland

In present paper there will be discussed examples of author's scientific co-operation with professor Borowiecki. Generally all of them are from the area of heterogeneous catalysis with a feedback to chemical technology and an environmental protection.
10.2478/v10063-010-0013-3
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Article 14EN: Syntheses, structures and properties of halogenanilides derivatives of trichlorophenoxyacetic acids
155-168

B. Tarasiuk


Faculty of Chemistry Department of Organic Chemistry Gliniana, Maria Curie-Skłodowska University, 33, 20-614 Lublin, Poland

The results of the study on the syntheses and properties of halogenanilides derivatives of trichloro- phenoxyacetic acids are presented. Compounds were synthesized during the reaction of trichlorophenoxyacetic chlorides with halogenaniline and N, N-diethylaniline or trichlorophenoxyacetic acids with halogenanilines and phosphorus oxychloride. The chemical derivatives were isolated with high yield and identified on the basis of elemental analysis, FTIR, 1H NMR and 13C NMR spectroscopy as well. Their physico-chemical properties were examined, along with their fungicidal, insecticidal, acaricidal and herbicidal activity. It was found that the highest herbicidal activity characterizes the derivatives of 2,4,5-trichlorophenoxyacet-4-fluoroanilide, 2,4,5-trichlorophenoxyacet-4-chloro-3-(trifluoromethyl) anilide, 2,4,5-trichlorophenoxyacet-3-(trifluoromethyl)anilide and 2,4,5-trichlorophenoxyacet-4-chloro-3-fluoroanilide.
10.2478/v10063-010-0014-2
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Volume 64 - 2009

Article 01EN: The 65th Birthday of Professor Roman Leboda
VII-IX

Vladimir Gun'ko, Vladimir Turov, J. Skubiszewska-Zięba

10.2478/v10063-008-0001-z
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Article 02EN: Synthesis and structure of ethylene bridged polysilsesquioxanes functionalized with different groups
1-10

M. Barczak, Andrzej Dąbrowski


Faculty of Chemistry, Maria Curie-Skłodowska University, pl. Marii Curie-Skłodowskiej 5, 20-031 Lublin, POLAND

Amino-, thiol-, urea-, and acethoxy- functionalized polysilsesquioxane xerogels have been obtained by co-condensation of 1,2-bis(triethoxysilyl)ethane with trifunctional silanes. The structural and chemical characterization of the xerogels was done by means of IR, 13C NMR, 29Si NMR spectroscopy, AFM, elemental analysis and nitrogen adsorption measurements. The resulting xerogels have a porous structure (SBET in the range 500-800 m2/g) and a high content of functional groups (2.3-2.7 mmol/g). Majority of these groups are accessible on the surface generating specific adsorption sites. The nature of the functional group introduced by co-condensation substantially influences the porous structure - the resulting samples can be microporous or mesoporous depending on the type of the group used.
10.2478/v10063-008-0002-y
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Article 03PL: The study of the properties of the hydroxyapatite/electrolyte interface
11-20

W. Janusz, E. Skwarek


Faculty of Chemistry, Maria Curie-Sklodowska University, pl. Marii Curie-Skłodowskiej 3, 20-031 Lublin, Poland

A physicochemical property of hydroxyapatite (HAP) [Ca10(OH)2(PO4)6] surface was studied and parameters of electrical double layer of the hydroxyapatite/NaCl solution system were described. The study sample of hydroxyapatite was synthesized. The structure of the hydroxyapatite was confirmed using X-ray diffraction (XRD), its particle size by PCS (photon correlation spectroscopy) AFM and SCM microscope and its surface properties by means of adsorption-desorption of nitrogen (ASAP), Raman spectra,. Then the point of zero charge and the isoelectirc point were measured.
10.2478/v10063-008-0003-x
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Article 04EN: Titania deposits on nanosilicas
21-48

V. M. Gun'ko 1, V. M. Bogatyrev 1, R. Leboda 2, J. Skubiszewska-Zięba 2, L. V. Petrus 1, Y. M. Nychiporuk 1, O. I. Oranska 1, O. A. Dudarko 1, V. D. Osovskii 3, Y. G. Ptushinskii 3


1 Institute of Surface Chemistry, 17 General Naumov Street, 03164 Kiev, Ukraine
2 Faculty of Chemistry, Maria Curie-Skłodowska University, 20-031 Lublin, Poland
3 Institute of Physics, Prospect Nauki 46, 02-022, Kiev, Ukraine

Titania (content CTiO2 = 2.7-20.0 wt%) was synthesized on different fumed silica substrates (A-50, A-100, A-380) using Ti[OCH(CH3)2]4 as a precursor interacting with silica/adsorbed water in 2-propanol or CCl4 medium, dried and then heated at 1073 K for 1 h. Initial and pretreated nanosilicas and titania/silicas were studied using XRD, adsorption, FTIR, TEM, AFM, and TPD-MS methods. The morphology of grafted titania (anatase/rutile/amorphous phase composition, particle size distribution, aggregation, textural porosity) depends on the types of a nanosilica matrix and a solvent, suspension treatments and reaction conditions.
10.2478/v10063-008-0004-9
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Article 05EN: Argon adsorption studies of porous structure of nongraphitized carbon blacks
49-63

L. Gardner, M. Jaroniec


Department of Chemistry, Kent State University, Kent, OH 44-242, USA

Structural properties of a series of commercial nongraphitized carbon blacks were studied by means of argon adsorption at 87 K and 77 K. The specific surface area of the samples was calculated using the standard BET method. The micropore volume and external surface area were both calculated by the αs-plot method. Pore volume and adsorption energy distributions were calculated numerically by using the regularization method. The above mentioned quantities obtained from argon adsorption isotherms were compared with those evaluated from nitrogen adsorption at 77 K.
10.2478/v10063-008-0005-8
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Article 06EN: Preparation of nanostructured carbons for solid phase extraction
64-74

A. M. Puziy 1, O. I. Poddubnaya 1, B. Gawdzik 2, M. Sobiesiak 2, C. A. Reinish 1, M. M. Tsyba 1, T. P. Segeda 1, M. I. Danylenko 3


1 Institute for Sorption and Problems of Endoecology, NAS of Ukraine, General Naumov St. 13, 03-164 Kiev, Ukraine
1 Department of Polymer Chemistry, Maria Curie-Skłodowska University, ul. Gliniana 33, 20-614 Lublin, Poland
1 Institute for Problems of Materials Science, NAS of Ukraine, Krzhizhanovsky St. 3, 03-142 Kiev, Ukraine

Nanostructured carbons have been obtained by the template method using silica gel and zeolite as structure directing agents. Carbons were characterised by nitrogen adsorption, acid-base titration, XRD and TEM, thermogravimetric analysis and IR spectroscopy. All carbons show developed and uniform porous structure with the mean size range mesopore 3.4 and 4.8 nm for silica gel derived carbons and in the micropore range 1.1 nm for zeolite derived carbon. The BET surface area of silica gel derived carbons is in the range 1230-1280 m2/g while zeolite derived carbon possesses very high BET surface area 3000 m2/g. Acid-base titration shows that carbons obtained by the template method contain a significant number of surface groups. Silica gel derived carbons possess mainly carboxylic and phenolic groups with small contribution of lactone/enol groups which totals 1.1-1.5 mmol/g. Extremely high number of surface groups (mainly phenolic) demonstrates carbon derived from zeolite - 11.3 mmol/g. The presence of phenolic groups was confirmed by IR spectroscopy. To study adsorption-desorption properties of nanostructured carbons towards phenol and chlorophenols a solid phase extraction method was used. High recoveries of chlorophenols were obtained (75-93%) at the breakthrough volumes 1200-1400 mL. The recoveries are much higher these that obtained with commercially available carbon ACC (Supelco).
10.2478/v10063-008-0006-7
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Article 07EN: Synthetic carbon adsorbents - the method of their preparation and application in adsorption and chromatography
75-85

A. Gierak


Institute of Chemistry, Jan Kochanowski University, ul. Świętokrzyska 15G, 25-404 Kielce, Poland

This paper is devoted to the methods of preparation of the synthetic carbon adsorbents by carbonization of different polymer precursors and the research into the structural and surface properties of the obtained carbon adsorbents. The paper describes the research into the preparation of active carbons by carbonization of: polysufonated cation-exchanged resin, polyvinyl chloride and porous copolymer (4,4-diphenyl sulfone dimethacrylate). The carbonization of polymers was carried out in inactive atmosphere under the supervised conditions. The spherical shape of grains is a result of carbonization. The obtained carbon adsorbents were subjected to additional modification processes, i.e. hydrothermal activation in steam atmosphere, oxidation with nitric acid (6M HNO3) and heated in hydrogen (H2) atmosphere. The adsorption from aqueous solutions of the chosen organic compounds on the modified synthetic active carbons, the adsorption of organic compounds in relation to water as well as structural characteristics of carbon adsorbents are discussed in this paper. The interaction of the organic substances and the synthetic active carbons in aqueous solutions depends on the structural properties of carbons (volume of micro- and meso-pores, distribution of pore sizes, specific surface area) and their chemical properties (i.e. concentration of functional oxygen groups, presence of mineral admixtures).
10.2478/v10063-008-0007-6
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Article 08EN: Synthesis of mesoporous ZrO2-SiO2 and WO3/ZrO2-SiO2 solid acids
86-95

V. V. Brei, A. V. Melezhyk, S. V. Prudius, N. S. Bodul, P. A. Mutovkin


Institute for Sorption and Endoecology Problems, National Academy of Sciences of Ukraine, General Naumov Str., 13, 03-164 Kiev, Ukraine

The method for preparation of mesoporous ZrO2-SiO2 and WO3/ZrO2-SiO2 oxides with silicic acid sol is proposed. It was shown that these acidic oxides demonstrate high activity in the reaction of tetrahydrofuran oligomerization.
10.2478/v10063-008-0008-5
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Article 09EN: Physico-chemical methods for the chromatographic materials heterogeneity evaluation
96-135

M. Michel 1, M. Sprynskyy 2, B. Buszewski 2


1 Pesticide Residue Department, Plant Protection Institute, ul. Węgorka 20 W., 60-318 Poznań, Poland
2 Chair of Environmental Chemistry and Bioanalytics, Faculty of Chemistry, Nicolaus Copernicus University, ul. Gagarina 7, 87-100 Toruń, Poland

The characterization methods used in the analysis of the chemical structure, microstructure and morphology, as well as the physical properties, of the chromatographic support are varied. This paper will focus on some techniques often used for the investigation of polymer/silica stationary phases. Many of these techniques are specific for characterization of particular properties of phases, and the properties of phases are also discussed correspondingly. To fully understand structure-property relationships, several characterization techniques are presented.
10.2478/v10063-008-0009-4
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Article 10EN: Advantages and risk related with carbon nanomaterials (CNMs) application for water remediation. Mini review
136-146

P. Oleszczuk 1;2


1 Institute of Soil Science and Environmental Management, University of Life Sciences, ul. Leszczyńskiego 7, 20-069 Lublin, Poland
1 Department of Soil, Plant and Insect Science, University of Massachusetts, 12B Stockbridge Hall, Amherst, MA 01-003, USA

Water is one of the most valuable substances in the world and its availability in the form of potable and drinking water is of great importance for any society. Conventional water treatment methods have been reported to be ineffective in removing some kinds of organic pollutants including endocrine disrupting chemicals (EDCs), personal care products (PCP), pharmaceuticals, etc. Nanotechnology - especially application of the carbon based nanomaterials (CNMs) to water decontamination - is promising technology. The physico-chemical properties of CNMs (e.g. high surface area to volume ratio, high equilibrium rate) make them an excellent adsorbent which can be effectively used to remove pollutants from water. The present mini-review provides an overview of the research progress about organic chemical adsorption on CNMs in relation to water decontamination. The paper also discussed the possible risk related with desorption pharmaceuticals from CNMs.
10.2478/v10063-008-0010-y
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Article 11EN: Chromatographic characterisation of acceptor-donor properties of MCMs
147-158

H. Grajek 1, J. Paciura-Zadrożna 1, Z. Witkiewicz 1;2;3


1 Institute of Chemistry, Military University of Technology, Warsaw
2 Institute of Chemistry, Jan Kochanowski University, Kielce
3 University of Arts and Sciences, Kielce

The values of the specific retention volumes of non-polar and polar adsorbates chromatographed on the ordered mesoporous silica adsorbents (MCMs) were determined under their infinite dilution conditions. Two methods were employed for the calculation of the standard free energy of adsorption, ΔGads, of the chromatographed adsorbates on the basis of the specific retention volumes. The ΔGads values were employed for the estimation of the van der Waals contribution and specific contribution of the free surface energy for the MCMs and the parameters characterising their ability to act as acceptors, KA, and donors, KD, of electrons.
10.2478/v10063-008-0011-x
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Article 12EN: Mechanochemical synthesis of barium titanate and its photocatalytic properties
159-168

V. Sydorchuk, S. Khalameida, V. Zazhigalov


Institute for Sorption and Problems of Endoecology, NAS of Ukraine, 13 General Naumov Str., 03164 Kyiv, Ukraine

The nano-dispersed barium titanate was synthesised by mechanochemical treatment of barium titanyl oxalate and mixture of BaO and TiO2. Prepared barium titanate demonstrates higher photoactivity in comparison to the same sample obtained by traditional solid state reaction. Shift of absorption edge in the visible region and respective narrowing of the band gap for the milled samples were observed.
10.2478/v10063-008-0012-9
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Article 13EN: Properties of materials as determined by inverse gas chromatography
169-183

A. Voelkel, K. Adamska


Institute of Chemical Technology and Engineering, Poznań University of Technology, pl. M. Curie-Skłodowskiej 2, 60-965 Poznań, Poland

The application of inverse gas chromatography (IGC) in the determination of the physicochemical properties of various materials is presented and discussed. The special attention is focused on the determination of solubility parameters.
10.2478/v10063-008-0013-8
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Article 14EN: Clusterization of water at a surface of nanosilica A-380
184-196

A. Yu. Petin 1, V. M. Gun'ko 1, A. V. Turov 2, V. V. Turov 1, R. Leboda 3


1 Institute of Surface Chemistry, 17 General Naumov Str., Kiev 03-164, Ukraine
2 Taras Shevchenko University, Kiev 01-030, Ukraine
3 Maria Curie-Skłodowska University, 20-031 Lublin, Poland

Thermodynamic and structural characteristics of water (0.07-1 g per 1 g of silica) bound to nanosilica A-380 (SBET = 378 m2/g, primary particle diameter 7.2 nm) alone or on co-adsorption with chloroform alone or in the mixture with DMSO or acetonitrile were determined using 1H NMR spectroscopy with layer-by-layer freezing-out of water at 200-273 K and NMR-cryoporometry.
10.2478/v10063-008-0014-7
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Article 15EN: Ceria-zirconia supported gold catalysts
197-217

J. M. Rynkowski 1, I. Dobrosz-Gómez 2


1 Institute of General and Ecological Chemistry, Technical University of Łódź, 90-924 Łódź, Żeromskiego 116, Poland
1 Facultad de Ciencias Exactas y Naturales, Universidad Nacional de Colombia, Sede Manizales

This paper presents the most important achievements and conclusions coming from the contributions concerning ceria-zirconia supported Au catalysts for low temperature water gas-shift reaction and low-temperature CO oxidation. The usefulness of CeO2-ZrO2 mixed oxides as supports for Au nanoparticles has been reviewed, mainly from the point of view of their contribution to those reactions. A special attention was paid to the active sites of CO oxidation and WGS reaction over Au/ceria-zirconia systems. Some aspects of the reactions mechanisms are also discussed. Ceriazirconia supported gold catalysts appear to be very promising systems, which have a potential to create a new quality in the catalysis of WGS reaction. Ceria-zirconia mixed oxides also seem to be very promising supports for Au nanoparticles in CO oxidation. They could find a practical application in ambient conditions, especially in air purification systems and a breathing apparatus. It is possible that gold could be usefully incorporated into automobile catalysts, considering that the price of other noble metals is rising rapidly. Their use in this application will, however, require demonstration of adequate stability at operating temperatures.
10.2478/v10063-008-0015-6
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Article 16EN: Specific control parameters in the technology of aerosol nanocatalysis
218-226

I. M. Glikina, M. A. Glikin, S. A. Kudryavtsev


Technological Institute (Severodonetsk), Vladimir Dal Eastern-Ukrainian National University, av. Sovetskiy, 59A, 93-400, Severodonetsk, Ukraine

This article shows the benefits of new technology for the implementation of gas-phase chemical reactions by aerosol nanocatalysis. The influence of new managing factors such as the concentration of catalyst, frequency, amplitude of motion of catalyst particles, dispersive material, etc. This enhances the process management and increases the rate of reaction per mass of catalyst in the 104-106 times. The selectivity of chemical transformations increases by 10-20%. Sometimes, new valuable products of the reaction are formed.
10.2478/v10063-008-0016-5
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Article 17EN: Application of novel complexing agent in sorption of heavy metal ions from wastewaters on ion exchangers of various types
227-245

D. Kołodyńska, Z. Hubicki


Department of Inorganic Chemistry, Faculty of Chemistry, Maria Curie-Skłodowska University, pl. Marii Curie-Skłodowskiej 2, 20-031 Lublin, Poland

Ethylenediaminetetraacetic acid (EDTA) and nitrilotriacetic acid (NTA) are very effective chelating agents used in many branches of industry. However, they are characterized by low biodegradability (EDTA) and carcinogenic effect (NTA), additionally they are quite persistent in the environment. The search for a cost effective alternative to these two most frequently used chelating agents has long been an industry target. One of them is N, N-bis(carboxylmethyl)-L-glutamic acid whose tetrasodium salt known as Dissolvine GL-38. The aim of our work was to investigate Dissolvine GL-38 as a potential alternative for EDTA or NTA in effective removal of heavy metal ions from waters and wastewaters. In the presented paper there were used for the sorption of of heavy metal ions two commercially available ion exchangers: Lewatit MonoPlus MP 64 and Purolite S-920. A series of experiments was conducted to optimise the method for the Cu(II), Zn(II), Ni(II) and Cd(II) removal from industrial effluents. It was found that the sorption efficiency of the monodisperse polystyrene anion exchanger as well as the chelating ion exchanger varied depending on metal ions concentration, pH, phase contact time, agitation, temperature and properties of ion exchangers.
10.2478/v10063-008-0017-4
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Article 18EN: Preparation of matrix-free reference materials of volatile analytes based on the controlled decomposition of surface compounds: a new concept
246-258

K. Kupiec, P. Konieczka, J. Namieśnik


Chemical Faculty, Department of Analytical Chemistry, Gdanśk University of Technology, ul. Narutowicza 11/12, 80-952 Gdańsk, Poland

The use of reference materials in analytical laboratories is on the increase. Undoubtedly, the reason for this is the need for traceable and therefore comparable results of measurements. The use of reference materials is necessary in all analytical laboratories and especially in those which examine environmental samples characterised by: - low or very low concentration levels of analytes, - complex matrices - temporal and spatial variability of samples, and - the possibility of interference. The development of analytical techniques for measuring components of gaseous media (outdoor air, indoor air, workplace air) has been going on for many years. This trend is closely associated with the need to obtain results of high quality, which necessitates the use of matrix-free (standard gaseous mixtures) as well as matrix reference materials. The use of reference materials with matrix compositions and analyte concentrations close to those of real samples yields more reliable measurement results. This article presents a new approach to the problem of generating standard gaseous mixtures: the analyte is generated during the thermal decomposition of compounds immobilised on (i.e. chemically bonded to) the surface of an appropriate support material.
10.2478/v10063-008-0018-3
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Article 19EN: Soft-templating synthesis of nanoporous carbons with incorporated alumina nanoparticles
259-272

J. Choma 1, A. Żubrowska 2, J. Górka 2, M. Jaroniec 2


1 Institute of Chemistry, Military Technical Academy, 00-908 Warsaw
2 Department of Chemistry, Kent State University, Kent, OH 44242, USA

Soft-templated microporous-mesoporous carbons with embedded alumina nanoparticles were synthesized using resorcinol and formaldehyde as carbon precursors, different inorganic acids as a catalyst and poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) block copolymer as a soft template. The carbons studied have very good adsorption properties such as high specific surface area, uniform pore size distribution and a large total pore volume. The choice of catalyst seems to play an important role for the incorporation of aluminum species to the carbon framework, which after thermal treatment form aluminum oxide nanoparticles. This simple approach seems to be very promising for the design of carbon-based materials for a broad range of applications.
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Article 20EN: SPE and GC methods of preconcentration and determination of phenol, o-chlorophenol, and benzene by means of chemically modified silica
273-281

I. Rykowska, W. Wasiak


Faculty of Chemistry, Adam Mickiewicz University, Grunwaldzka 6, 60-780 Poznań, Poland

In the paper preparation, characteristics and potential applications of two new sorbents with chemically bonded transition metal complexes have been presented. The sorbents have been synthesized by attaching copper (II) chlorides to the silica surface through ketoimine groups. The suggested application area of the proposed sorbents is related with solid-phase extraction (SPE) of aromatic compounds of different structure, e.g., phenol, 2-chlorophenol, and benzene from water matrix. The experiments proved high efficiency of the sorbents, the ranging recovery rates from 88% to 96% and the LOD values from 0.2 for phenol, and 1.0 for o-chlorophenol. Basic characteristics of the sorbents synthesized were determined by the use of elemental analysis and UV-VIS spectroscopy.
10.2478/v10063-008-0020-9
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Article 21EN: Zipf's law in concentration distributions
282-290

M. Kosmulski


Department of Electrochemistry, Lublin University of Technology, 20-618 Lublin, ul. Nadbystrzycka 38, Poland

Concentrations of impurities in fluids often follow Zipf's law, that is, relatively few impurities occur at high concentrations and numerous impurities occur at low concentrations. The concentrations of compounds in air and of elements in ocean water are examples of such distributions. This principle can be used to predict the number of components in a mixture, which occur above certain concentration level, also beyond the range of analytical methods. In most practical applications the existence of minor components can be ignored, but the level of concentration, at which certain component can be ignored depends on the specific problem.
10.2478/v10063-008-0021-8
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Article 22EN: Comparision of methods used for estimation of lipophilicity of biologically active phenylthioamides
291-299

M. Kostecka


Departament of Chemistry, University of Nature, ul. Akademicka 15, 20-031 Lublin, Poland

Effectiveness of compound actions on living organisms depends on optimal lipophilicity. For studied 2,4-dihydroxyphenylthioamides of microbiocidal properties there were determined the values of lipophilicity parameters: log kw, using high performance liquid chromatography and log P - the theoretical distribution coefficient in the n-octanol/water system. The search for a theoretical method was made which could replace chromatographic methods in preliminary choice of compounds of presumably high fungicidal activity. The obtained results point to the Crippens and Ghose method and the values log P determined in this way correlate well with log kw and allow to choose a lipophilicity range in which the biological activity is the largest.
10.2478/v10063-008-0022-7
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Volume 63 - 2008

Article 01EN: The 65th Birthday of Professor Emil Chibowski
VII-IX

Lucyna Hołysz

10.2478/v10063-008-0023-6
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Article 02EN: Is the world basic? Lessons from surface science
1-16

K. Mittal 1, F. M. Etzler 2


1 P.O. Box 1280, Hopewell Junction, NY 12533-1280
1 Boehringer-Ingelheim Pharmaceuticals, 900 Ridgebury Road Ridgefield, CT 06877

In this work the authors review various definitions of acids and bases. Furthermore, the application of these theories to surface and adhesion science is discussed. It is clear that application of various acid-base theories may not always lead to consistent conclusions on the acid-base character of surfaces. Possible reasons for the inconsistency include the nature of the scale, the choice of reference points, and the use of either poor or inconsistent statistical procedures in addition to experimental difficulties. The present authors recommend a future careful study and comparison of the various acid-base theories when applied to surface and adhesion science. The limited studies already preformed suggest this activity would be worthwhile.
10.2478/v10063-008-0024-5
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Article 03EN: Influence of the electrolyte concentration on interaction between silica particles
17-30

W. Wójcik, B. Jańczuk, Robert Ogonowski


Department of Interfacial Phenomena, Faculty of Chemistry, Maria Curie-Skłodowska University, pl. Marii Curie-Skłodowskiej 3, 20-031 Lublin, Poland

The destruction time of the sediment column structure was measured for different fractions of silica particles in NaCl and CaCl2 solutions whose concentrations were varied from 0.25 M to 2.0 M. A linear relationship between the reciprocal of the destruction time of the silica sediment column structure and average diameter of the silica fraction, the density and work of cohesion of the solutions was found. The determined values of the particle diameter, the cohesion work and density of the solution calculated from these linear dependences for the time equal to infinity (1/t = 0) were named critical. Using the above critical parameters the detachment force of one particle from another was calculated. For the system whose components had critical values the detachment force was found to be equal to the attachment force resulting from the interfacial interaction. On the basis of our earlier study and Derjaguin's approximation the radius of the contact plane and the attachment force between two silica particles were calculated. The detachment force decreased with increasing salt concentration, but the attachment force was nearly constant. It was found that for a given salt concentration the relationship of the reciprocal of the destruction time as a function of the difference between the detachment and attachment forces was also linear. It appeared that for the silica column structure having critical parameters the values of the difference between the detachment and attachment forces were negative. This means that in the calculation of the attachment force between silica particles in the studied solutions an additional interaction should be taken into account.
10.2478/v10063-008-0025-4
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Article 04EN: On the stability of magnetic colloids
31-46

M. T. López-López 1, G. R. Iglesias 1, J. D. G. Durán 1, F. González-Caballero 2


1 Department of Applied Physics, Faculty of Sciences, University of Granada, c/Campus de Fuentenueva s/n 18071 Granada. Spain
2 Maria Curie-Skłodowska University, Lublin, Poland

In this paper, the preparation of fluids belonging to ferrofluid (FF) and magnetorheological (MR) categories is described. Furthermore, the effect of different stabilizing additives (thixotropic agents, surfactants, magnetic nanoparticles) and carrier liquids on the sedimentation of these fluids is analyzed. These studies are conducted using: (i) optical and electromagnetic induction techniques for monitoring the stability of dilute and concentrated suspensions, respectively; (ii) contact angle and pendant drop measurements to explain the observed stability in different carriers. The results of these experiments are analyzed in detail and magnetic fluids with improved stability properties are prepared accordingly.
10.2478/v10063-008-0026-3
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Article 05EN: Biomedical applications of the Langmuir monolayer technique
47-60

K. Hąc-Wydro, P. Dynarowicz-Łątka


Faculty of Chemistry, Jagiellonian University, Ingardena 3, 30-060 Kraków, Poland

The modeling of natural membranes is a consequence of their complex structure. The paper describes different approaches used to model biomembranes, and emphasizes the advantages of applying the Langmuir monolayer technique in this aspect.
10.2478/v10063-008-0027-2
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Article 06EN: Equilibrium of counterion association in micellar systems: cetyltrimethylammoniumbromide
61-67

N. Kallay, T. Glušac, T. Preočanin, A. Čop, D. Kovačević, S. Žalac


Laboratory of Physical Chemistry, Department of Chemistry, Faculty of Science, University of Zagreb, Horvatovac 102a, 10000 Zagreb, Croatia

Surface Complexation Model was applied for the analysis of counterion association in the micellar systems. The equilibrium in cetyltrimethylammoniumbromide (CtaBr) solution was examined. Thermodynamic equilibrium constant was calculated using experimental data obtained with ion-selective electrodes (silver/silver bromide and surfactant electrode).
10.2478/v10063-008-0028-1
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Article 07EN: Graphite flotation in the presence of sodium acetate
68-72

B. Grabowski, J. Drzymała


Wrocław Technical University, Wybrzeże Wyspiańskiego 27, 50-370 Wrocław, Poland

Graphite was subjected to flotation in the presence of increasing concentration of sodium acetate. A comparison of graphite flotation with the surface tension, both as a function of the sodium acetate concentration in the aqueous solution, revealed a similar pattern of both relations. It seems to confirm one of the theories of salt flotation claiming that for hydrophobic materials the change of flotation recovery with the salt concentration is mostly determined by the surface tension of the aqueous solution. It was found that graphite recovery increases when the surface tension of the solution and decreases as the surface tension decreases. At a low salt concentration this rule is not obeyed due to, very likely, the socalled Jones-Rey effect.
10.2478/v10063-008-0029-0
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Article 08EN: Surface characterization of clay particles via dielectric spectroscopy
73-86

M. L. Jiménez 1, A. V. Delgado 1, U. Kaatze 2


1 Department of Applied Physics, University of Granada, 18071 Granada, Spain
2 Drittes Physikalisches Institut, Universitat Goettingen, Goettingen, Germany

This work deals with the high frequency dielectric relaxation of clay (sodium montmorillonite, or NaMt) suspensions. By high frequency it is meant that the permittivity will be determined in the region where the Maxwell-Wagner-O'Konski relaxation takes place, roughly, the MHz frequency range. The applicability of dielectric determinations for the characterization of the electrical properties of these complex systems is demonstrated. In fact, standard electrophoresis measurements only allow to detect that the charge of the particles becomes slightly more negative upon increasing pH. Much more information is obtained from the high frequency electric permittivity for different concentrations of solids and pHs. From the characteristic frequencies of the relaxation it is possible to detect separate processes for parallel and perpendicular orientations of the clay platelets, modelled as oblate spheroids with a high aspect ratio. In addition, using a suitable model the surface conductivity of the clay particles can be estimated. Our data indicate that this quantity is minimum around pH 7, which is admitted as representative of the isoelectric point of the edges of the clay platelets. Data are also obtained on the amplitude (value of the relative permittivity at low frequency minus that at high frequency) of the relaxation, and it is found that it depends linearly on the volume fraction of solids, and that it is minimum at pH 5. These results are considered to be a manifestation of the fact that particle interactions do not affect the electric conduction inside the electric double layer, while the special behaviour at pH 5 is related to the existence of aggregates at pH 5, which increase the effective size of the particles and provoke a reduction of their effective conductivity.
10.2478/v10063-008-0030-7
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Article 09EN: Atmospheric oxidation of ascorbic acid in nonionic surfactant systems
87-93

Jolanta Narkiewicz-Michałek 1, M. Szymula 1, K. A. Wilk 2


1 Faculty of Chemistry, Maria Curie Skłodowska University, M.C. Skłodowska Sq. 3, 20-031 Lublin, Poland
2 Department of Chemistry, Wroclaw University of Technology, Wybrzeże Wyspiańskiego 27, 50-370 Wrocław, Poland

In our study we investigated the kinetics of atmospheric oxidation of ascorbic acid in the aqueous solutions of two non-ionic surfactants TRITON X-100 and commercial sugar ester C1616 (the most suitable emulsifier for food). For each surfactant the concentrations below and above the CMC were investigated. It was found that the micellar solutions of both surfactants showed faster oxidation rate than pure water. Less pronounced effects were observed with particular surfactant concentration change.
10.2478/v10063-009-0001-7
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Article 10EN: Energy & climate
94-110

E. Robens 1, H. M. El_Nokraschy 2, A. Dąbrowski 3


1 Institut für Anorganische Chemie und Analytische Chemie, Johannes Gutenberg-Universität, Duesbergweg 10-14, D - 55099 Mainz, Germany
1 Nokraschy Engineering GmbH, An de Masch 24, D - 25488 Holm. Germany
1 Faculty of Chemistry, Uniwersytet Marii Curie-Skłodowskiej, pl. M. Curie-Skłodowskiej 2, 20-031 Lublin, Poland

Based on published reports a short survey is presented on climatic change. Considering world's increase in temperature the use of fossil energy should be replaced as far and as quickly as possible by alternatives. Actual methods for energy production are discussed. At present, only nuclear power plants and concentrating solar power plants are able to meet the large requirements. Regarding the limited resources of nuclear fuel, costs and problems of nuclear techniques urgently solar techniques should be developed for an extended application.
10.2478/v10063-009-0002-6
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Article 11EN: Biomodification of plastic surfaces and depression process
111-121

I. Polowczyk, Z. Sadowski, D. Smoczyńska


Faculty of Chemistry, Wrocław University of Technology, Wybrzeże Wyspiańskiego 27, 50-370 Wrocław, Poland

Plastics from the municipal waste must be recycled on a large scale. This contribution describes the initial work to determine the surface energy of plastic waste. Results of such investigations were correlated with both sedimentation and flotation data. The penetration rate of a liquid into the horizontal powder layer was measured; basing on the rate of liquid penetration, the effective radius of the porous bed was calculated. For modification of the surface of plastics, tannic acid, sodium lignin sulfonate and microbial broth from Pseudomonas aeruginosa growth were used. In order to determine the effect of these reagents on the surface energy of plastic powders, the penetration and flotation experiments were carried out. For polystyrene and polyethylene the estimated surface energy was 28.6 [mJ/m2] and 24.5 [mJ/m2], respectively. These results were correlated with the sediment height extreme of plastic powders in solvent pairs. The adsorption of tannic acid, sodium lignin sulfonate and biosurfactants from microbial filtrate caused an increase of the surface energy of plastic particles. For instance, the free energy of polyethylene particles was 34.9 [mJ/m2] after the sodium lignin sulfonate treatment, and 35.57 [mJ/m2] for the tannic acid adsorption. The natural flotation of plastic particles in the presence of modifying reagents was shown to be dependent on the concentration of these reagents.
10.2478/v10063-009-0003-5
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Article 12EN: Synthesis and characterization of a superhydrophobic surface from cyclic olefin copolymer
122-129

E. Doganci, H. Y. Erbil


Department of Chemical Engineering, Gebze Institute of Technology, Cayirova, Gebze 41400, Kocaeli, Turkey

Cyclic olefine copolymer (COC) which is an engineering plastic was tried to form a superhydrophobic surface by a phase separation process using solvent + non solvent mixtures. The cloud points of the COC + solvent + non-solvent mixtures were determined and evaluated by using Hansen 3-solubility parameter approach. It was determined that the amorphous COC polymer is not suitable to prepare a superhydrophobic surface when used alone. However, a superhdrophobic surface with a water contact angle of 158±2° was obtained when COC is mixed with crystalline polypropylene homopolymer. The water contact angle and surface morphology of the polymer coatings were examined.
10.2478/v10063-009-0004-4
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Article 13EN: Kinetics of multi-site-occupancy adsorption at the solid/solution interfaces. The absolute rate theory approach
130-143

Władysław Rudziński 1;2, W. Płaziński 2


1 Polish Academy of Sciences, Institute of Catalysis and Surface Chemistry, Cracow, Poland
1 Department of Theoretical Chemistry, Faculty of Chemistry, Maria Curie-Skłodowska University, pl. M. Curie-Skłodowskiej 3, 20-031 Lublin, 031 Poland

The kinetic approach based on the absolute rate theory and the model of a two-site-occupancy adsorption has been proposed to describe the kinetics of sorption of solute at the solid/solution interfaces. The obtained general kinetic equation reduces to the popular empirical formulas (i.e. the Lagergren equation and the pseudo-second order equation) depending on the values of physical and technical parameters which characterize the adsorption system. here, for the case when the adsorption kinetics is governed by the rate of surface reactions. The features of this general equation are shown by presenting some simple model investigations, and its applicability is tested by presenting the analysis of some experimental data reported in literature.
10.2478/v10063-009-0005-3
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Article 14EN: Investigation of surface properties of lunar regolith - Part IV
144-168

E. Robens 1, A. Dąbrowski 2, E. Mendyk 2, J. Goworek 2, K. Skrzypiec 2, M. Drewniak 2, M. Dumańska-Słowik 4, W. Gac 2, R. Dobrowolski 2, S. Pasieczna-Patkowska 2, M. Huber 3, M. Iwan 2, K. J. Kurzydłowski 5, T. Płociński 5, J. Ryczkowski 2, Z. Rzączyńska 2, J. W. Sobczak 6


1 Institut für Anorganische Chemie und Analytische Chemie, Johannes Gutenberg-Universität, Duesbergweg 10-14, D-55099 Mainz, Germany
2 Faculty of Chemistry, Maria Curie-Skłodowska University, pl. Marii Curie-Skłodowskiej 2, 20-031 Lublin, Poland
3 Department of Geology and Protection of Litosphere. Institute of Earth Science, Maria Curie-Skłodowska University, Al. Kraśnicka 2cd, 20-718 Lublin, Poland
4 Department of Mineralogy, Petrography and Geochemistry. Faculty of Geology, Geophysics and Environmental Protection, AGH-University of Science and Technology, 30-059 Kraków, Al. Mickiewicza 30
5 Warsaw University of Technology, Pl. Politechniki 1, 00-661 Warszawa, Poland
6 Polish Academy of Sciences, Institute of Physical Chemistry, Kasprzaka 44/52, PL-01-224 Warszawa, Poland

We investigated three lunar regolith powder samples from the Apollo missions. Apollo 11 and Apollo 12 samples come from lunar maria and Apollo 16 sample from a highland region. In the present paper we summarise in brief results of measurements using photoelectron spectroscopy (XPS), micro-Raman spectroscopy (RM), x-ray diffraction (XRD), x-ray fluorescence spectroscopy (XRF), temperature programmed reduction and oxidation (TPRO), thermogravimetry (TG), differential thermal analysis (DTA) and nitrogen adsorption. Parts of samples are visualised by means of scanning electron microscopy (SEM/EDX) and atomic force microscopy (AFM).
10.2478/v10063-009-0006-2
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Article 15EN: Some peculiarities in stability of nanodispersions
169-179

W. Nowicki


Faculty of Chemistry, UAM, Grunwaldzka 6, 60-780 Poznań, Poland

The stability of some classes of dispersion systems, extensively studied in modern material sciences and nanotechnology, is discussed in terms of the classical colloid chemistry laws. Some limitations of the technologies resulting from the specificity of the nanodispersed systems, utilized in nowadays applications, are pointed out.
10.2478/v10063-009-0007-1
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Article 16EN: Some problems of the optimization of the separation process in liquid chromatography
180-200

J. K. Różyło, I. Malinowska


Department of Planar Chromatography, Faculty of Chemistry, Maria Curie-Skłodowska University, pl. M. Curie Skłodowskiej 3, 20-031 Lublin, Poland

One of the optimization theory worked out by Ościk has been used for some physicochemical studies and optimization of chromatographic process. On the basis of the theoretical equations a retention in binary mobile phases can be predicted with good agreement for a lot of chromatographic systems. The influence of the different properties of chromatographic systems can be determined by use of the discussed optimization theory. The possibilities of the use of the theory for some physicochemical studies as determination of the hydrophobicity have been demonstrated too.
10.2478/v10063-009-0008-0
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Article 17EN: DPPC monolayers as simple models of biological membranes for studies of interactions with perfluorinated compounds
201-210

D. Matyszewska, R. Bilewicz


Faculty of Chemistry, University of Warsaw, ul. Pasteura 1, 02093 Warsaw, Poland

Langmuir monolayers of 1,2-dipalmitoyl-sn-glycero-3-phosphocholine (DPPC) formed at the air-water interface were used as simple models of biological membranes to study interactions with two selected perfluorinated compounds: perfluorooctanoic acid (PFOA) and perfluorooctanesulphonic acid (PFOS). The presence of those common pollutants in the subphase led to the formation of more fluidic monolayer possessing different surface and barrier properties. The observed increase in the area per molecule in the Langmuir monolayer spread at the air-water interface was attributed to the incorporation of perfluorinated compounds into the layer. Moreover, perfluorooctanesulphonic acid was found to interact with DPPC monolayers transferred onto the electrode surface. Exposure of DPPC modified electrode to PFOS solution led to changes in electrode capacitance and in the efficiency of electron transfer rate observed for selected electroactive probes added to the solution.
10.2478/v10063-009-0009-z
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Article 18EN: Electrochemical study of corrosion of copper in 1-alkyl-3-methylimidazolium tetrafluoroborates
211-222

K. Marczewska-Boczkowska 1, M. Kosmulski 1, J. Olchowik 2


1 Department of Electrochemistry, Lublin University of Technology, Lublin, Poland
2 Institute of Physics, Lublin University of Technology, Lublin, Poland

Copper is resistive to corrosion in dry and chloride-free 1-alkyl-3-methylimidazolium tetrafluoroborates at room temperature, and the corrosion rate decreases with the chain length of the substituent in imidazolium ring and increases with the temperature. The activation energies of corrosion are on the order of 50 kJ/mole. The corrosion in enhanced in the presence of traces of chlorides.
10.2478/v10063-009-0010-6
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Article 19EN: Influence of relative humidity on the wettability of silicon wafer surfaces
223-239

L. Hołysz, M. Mirosław, K. Terpiłowski, A. Szcześ


Department of Physical Chemistry - Interfacial Phenomena, Faculty of Chemistry, Maria Curie-Skłodowska University, 20-031 Lublin, Poland

Investigation of wetting properties of the original silicon wafers and modified by oxidation was carried out by contact angles measurements of water at varying relative humidity (RH) of the atmosphere present in the measuring chamber. At three selected humidities (10, 30 and 50%) contact angles of diiodomethane and formamide were also determined for the original silicon wafer only. The topography of the tested surfaces was determined with the help of atomic force microscopy (AFM). Using the measured contact angles the total apparent surface free energy and its components of studied silicon wafers were determined using two models: the contact angle hysteresis (CAH) and Lifshitz-van der Waals acid-base (LWAB) approaches. In the former approach the advancing and receding contact angles are employed, and in the latter only the advancing angles. It was found that in the case of original silicon wafer the contact angels and surface free energy depend on the humidity only in the RH range from 10 to 40% with a minimum at 30% RH, and then they fluctuate around a mean value. For the oxidized silicon wafer the changes in the contact angles and the surface free energy depend on the relative humidity and change periodically with increasing RH. These changes can result from water adsorption on the hydrophilic silicon surface.
10.2478/v10063-009-0011-5
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Article 20EN: Spontaneous spreading of liquids on substrates with contrasting two types of substrates: that of liquids and that of solids
240-243

J. Leja


Prof. emeritus UBC, Vancouver, Canada

10.2478/v10063-009-0012-4
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Article 21EN: Modeling of adsorption in pores with strongly heterogeneous walls. Computer simulations approach
244-256

B. Kuchta 1, L. Firlej 2


1 Laboratoire des Matériaux Divises, Revêtement, Electrocéramiques (MADIREL), Université de Provence, Centre de Saint-Jérôme, 13397 Marseille, France
2 Laboratoire des Colloïdes, Verres et Nanomatériaux (LCVN), Université Montpellier II, 34095 Montpellier, France

We discuss the state of art in computer simulation of adsorption in nanopores with strongly heterogeneous rough wall structures. As an example, we review the recent models used in simulations of MCM-41 adsorbent and discuss their capacity to reproduce experimental adsorption isotherms, in the whole range of relative pressures. The conclusions of previous studies are compared with our recent model of heterogeneous pores characterized by separately energetic or structural heterogeneity, or both of them. On this basis we identify the main factors responsible for the mechanism of adsorption and discuss their influence on the results of simulations of adsorption. Some possibilities of further improvements of the model are also suggested.
10.2478/v10063-009-0013-3
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Article 22EN: Enhancement of three-phase kinetic studies of complex reaction systems by semibatch reactor technology
257-270

T. Salmi, D. Yu. Murzin, P. Mäki-Arvela, J. Wärnå, K. Eränen, J.-P. Mikkola, A. Denecheau, K. Alho


Åbo Akademi, Process Chemistry Centre, FI-20500 Turku/Åbo, Finland

A semibatch reactor concept was proposed for the determination of the kinetics in complex catalytic liquid and gas-liquid systems with reactions of highly varying rates. The method is based on continuous removal of liquid phase from the reactor, while the catalyst remains inside the reactor. The concept was demonstrated by catalytic hydrogenation of citral on Ni catalyst. The primary product (citronellal) is formed very rapidly, while the secondary (citronellol) and tertiary (3,7-dimethyloctanol) products appear much more slowly. With the proposed semibatch concept, the formation of the ultimate products was considerably accelerated and all of the rate parameters were successfully estimated by nonlinear regression analysis. The proposed approach can be extended to fixed beds with recycling as demonstrated by computer simulations.
10.2478/v10063-009-0014-2
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Article 23EN: The interaction of water vapor and hydrogen water mixtures with a polycrystalline uranium surface
271-286

E. Tiferet 1;2, M. H. Mintz 1;2, S. Zalkind 1, N. Shamir 1


1 Nuclear Research Centre-Negev, POB 9001, Beer-Sheva 84190, Israel
1 Dept. of Nuclear Eng., Ben-Gurion Univ. of the Negev, POB 653, Beer-Sheva, 84104, Israel

The initial room-temperature interactions of water vapor with polycrystalline bulk annealed uranium surfaces were studied by combined measurements utilizing Direct Recoil Spectrometry (DRS) and X-ray Photoelectron Spectroscopy (XPS). It was found that the water goes through a complete dissociation into oxidic oxygen and two neutral H atoms throughout the whole exposure range. The process proceeds by two consecutive stages: (i) below about 80% monolayer coverage, the dissociation products chemisorb mainly on the remaining non-reacted metallic surface by a simple Langmuir-type process; (ii) Between about 80% and full coverage, three dimensional oxide islands (that start to form at 50-60% coverage) cover most of the surface and full dissociation continues on top of them, with part of the hydrogen staying on top of the oxide. It was also found that traces of about 2% water vapor are sufficient to inhibit hydrogen dissociation and chemisorption on uranium surfaces, under low pressure exposures, at room temperature. The efficiency of the inhibition increases with temperature in the range of 200 - 400 K. The inhibition effect is also influenced by the extent of residual strain of the sample, with increasing inhibition efficiencies exhibited by a less strained surface. O2, in contrast to H2O, is not an inhibitor to surface adsorption and dissociation of hydrogen. Three types of mechanisms are discussed in order to account for the above inhibition effect of water. It is concluded that the most probable mechanism involves the reversible adsorption of water molecules on hydrogen dissociation sites causing their "blocking".
10.2478/v10063-009-0015-1
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Article 24EN: Adsorption of dyes on mesoporous carbons
287-299

A. Deryło-Marczewska 1, A. W. Marczewski 2, Sz. Winter 1


1 Department of Physicochemistry of Solid Surface, Faculty of Chemistry, Maria Curie-Skłodowska University, 20-031 Lublin, Poland
2 Department of Radiochemistry and Colloid Chemistry, Faculty of Chemistry, Maria Curie-Skłodowska University, 20-031 Lublin, Poland

Mesoporous carbonaceous materials were synthesized by applying the method of impregnation of mesoporous silica being the pore creating template. The isotherms of adsorption of methylene blue and methyl orange were measured from aqueous solutions. The kinetics of methylene blue adsorption was studied. The adsorption isotherms and kinetic dependence were discussed.
10.2478/v10063-009-0016-0
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Volume 61 - 2006

Article 01EN: On the utilization of industrial/municipal sludges as a source of desulfurization adsorbents
3-24

Teresa J. Bandosz


Department of Chemistry, The City College of CUNY, 138th Street and Convent Ave. New York, NY 10031; Tel: (212) 650-6017; Fax (212) 650-6107; E-mail: tbandosz@ccny.cuny.edu

Adsorbents for desulfurization of moist air were prepared from mixtures of sewage sludge, industrial sludges, and other carbonaceous wastes by their pyrolysis at 650 oC and 950 oC. The resulting inorganic/organic composite materials were characterized using sorption of nitrogen, thermal analysis, pH measurements, ICP, and X-ray diffraction. Their catalytic performance for hydrogen sulfide oxidation from air was evaluated in a dynamic test. The sludge-derived adsorbents have very high capacity for hydrogen sulfide removal and high selectivity of its conversion to elemental sulfur. While surface chemistry enhances oxidation, the developed volume of mesopores provides space for storage of elemental sulfur. Within that sulfur deposit in large pores secondary pore space is formed. The excellent performance in desulfurization process is governed by synergetic effects between the components of the sludges, which leads to the unique surface chemistry. This surface chemistry is a result of solid-state reactions in the reduced atmosphere during pyrolysis at high temperature.
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Article 02EN: Mineral surface monitoring, understanding and modification at molecular level
25-41

Jerzy Mielczarski, Ela Mielczarski


Laboratoire Environnement et Minéralurgie. U.M.R. 7569 du C.N.R.S. INPL/ENSG, 15 Avenue du Charmois, BP 40, Vandoeuvre-lès-Nancy 54501, Cedex, France Tel.: 33 3 83 59 62 83, Fax: 33 3 83 59 62 55 e-mail:jerzy.mielczarski@ensg.inpl-nancy.fr

Determination of the adsorbed layer composition and structure at molecular and atomic levels and understanding adsorption mechanisms and dynamics are vitally important for the preparation of surface layers with specific functions. Direct information at a molecular level about mineral surface composition, its structure and surface distribution is crucial to perform an efficient separation processes for mineral beneficiation. This information is equally important for modification of surface properties of industrial minerals for various specific applications such as: fillers, composites, weathering resistance, etc. The understanding of the mechanisms and kinetics of interaction of the first adsorbed organic molecules with mineral surfaces is the fundamental requirement to make possible the prediction and control of the macroscopic surface properties that govern the efficiency of separation technologies or new material formulations. The developed infrared external reflection technique has a very unique ability to study interface phenomena at a molecular level on heterogeneous substrates. The variety, precision and reliability of information about interface phenomena delivered by this technique are superior to other single techniques. The experiments are fast and non-destructive. High sensitivity (starting from 20% of monolayer), in situ collected information in a multiphase system even in the region of a strong absorption of substrate, makes this technique a very valuable experimental tool. The complexity of the recorded reflection spectra, their sensitivity to any variations of the optical properties of all bulk and surface components and their spatial distribution in the system under investigation, are in fact the major strength of the technique. In this presentation a few examples of application of this multidiagnostic technique for monitoring surface modifications of semisoluble minerals for selective flotation will be discussed in detail.
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Article 03EN: Application of the regularization method to the analysis of the TPD spectra carried out under quasi-equilibrium conditions
42-55

Tomasz Piotr Warzocha 1, Tomasz Panczyk 2, Władysław Rudzinski 1;2


1 Department of Theoretical Chemistry, Faculty of Chemistry, UMCS, pl. M. Curie-Sklodowskiej 3, 20-031 Lublin, Poland
2 Institute of Catalysis and Surface Chemistry, Polish Academy of Sciences, ul. Niezapominajek 8, 30-239 Cracow, Poland

The paper deals with the problem of determination of the adsorption energy distribution function from the thermodesorption spectra recorded under the quasi-equilibrium conditions. It is shown that such quasi-equilibrium may be assumed for the majority of thermodesorption experiments carried out under the flow conditions. A mathematical model of the quasi-equilibrium thermodesorption is presented and discussed. Also, implementation of the regularization procedure based upon the quasi-equilibrium model is presented. The accuracy of this procedure is discussed by its application for the analysis of the quasi-equilibrium thermodesorption data obtained from simulations.
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Article 04EN: Phase behavior of short chains adsorbed on crystalline surfaces
56-68

Małgorzata Borówko, Wojciech RYsko


Department for the Modelling of Physico-Chemical Processes, Faculty of Chemistry, Maria Curie-Skłodowska University,20-031 Lublin, Poland

This review summarizes the results of the Monte Carlo simulation study of phase behavior of dimers and trimers on crystalline solids. The molecules are assumed to be composed of segments A and B. We discuss here the parameters relevant to vapor-liquid coexistence in adsorbed monolayers, including shapes of molecules, their chemical structure, a degree of flexibility, the strength of interactions between similar and dissimilar segments, a type of lattice and surface eterogeneity. The illustrative examples of phase diagrams are presented. The model is mapped on the Ising-like single-occupancy models used previously for magnetic systems and gas molecules with internal degree of freedom.
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Article 05EN: Theoretical studies of enantiospecific adsorption on surfaces with chiral patterns of active sites
69-74

Paweł Szabelski


Department of Theoretical Chemistry, Maria Curie-Skłodowska University, pl. Marii Curie-Skłodowskiej 3, 20-031 Lublin, Poland

Adsorption of a racemic mixture of enantiomers of 1,2-dimethylcyclopropane on a patterned chiral surface is studied using Grand Canonical Monte Carlo technique. The adsorbing surface is assumed to be completely flat and composed of two types of sites one of which is more strongly adsorbing (active sites) than the other (inert sites). A key point of the model is a special spatial distribution of the active sites leading to enantioselectivity towards one of the enantiomers. In particular, we study the case when the surface as well as its mirror image are exposed to the racemic mixture. The obtained results which include adsorption isotherms and the corresponding selectivities suggest that even flat surfaces with chiral patterns of active sites can lead to effective enantioseparation.
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Article 06EN: Adsorption kinetics on geometrically irregular structures studied using the Statistical Rate Theory approach
75-84

Tomasz Panczyk 1, Władysław Rudzinski 1;2


1 Institute of Catalysis and Surface Chemistry, Polish Academy of Sciences, ul. Niezapominajek 8, 30-239 Cracow, Poland
2 Department of Theoretical Chemistry, Faculty of Chemistry, UMCS, pl. Marii Curie-Skłodowskiej 3, 20-031 Lublin, Poland

In this work some preliminary results are reported on the adsorption kinetics in the systems with geometrically irregular surfaces. It is assumed that the adsorption kinetics is governed by the molecular transport to the interior of the fractal structure and the rate of adsorption on the surface. It appears that both these processes are strongly affected by the fractal dimension of the surface. Some model calculations are presented witch show how the fractal dimension influences the adsorption kinetics, i.e., the uptake curves and the sticking probability curves. It is concluded that increasing value of the fractal dimension makes the sticking probability functions coverage independent with the initial sticking equal to unity (when the adsorption in not activated). That means all the molecules entering the interior of the fractal structure are adsorbed and the probability of escape to the bulk is almost zero. Generally, the increasing value of the fractal dimension makes to adsorption slower and entirely controlled by the rate of transport to the interior of the fractal structure.
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Article 07EN: Theoretical studies of the heat effects accompanying mixed-gas adsorption by using Vacancy Solution and Regular Adsorbed solution theories
85-95

Krzysztof Nieszporek


Department of Theoretical Chemistry, Faculty of Chemistry, UMCS, pl. Marii Curie-Skłodowskiej 3, 20-031 Lublin, Poland

The theoretical studies of the enthalpic effects accompanying mixed-gas adsorption equilibria by using Vacancy Solution Theory are presented. Besides heterogeneity the interaction effects by using the Regular Adsorbed Solution theory are taken into account. The theoretical predictions of adsorption phase diagrams and accompanying them calorimetric effects requires only the knowledge of single-gas adsorption and calorimetric data. It is shown that, in general, the VST approach gives the results that are in good agreement with experimental data.
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Article 08EN: Bridged polysilsesquioxane xerogels containing amineand thiol- groups: structural properties as a function of synthesis conditions
96-103

Mariusz Barczak, Andrzej Dąbrowski


Department of Theoretical Chemistry pl. Marii Curie-Skłodowskiej 3, 20-031 Lublin, Poland

Amino- and thiol- functionalized polysilsesquioxanes were obtained by hydrolytic polycondensation of 1,2-bis(triethoxysilyl)ethane or 1,4-bis(triethoxysilyl)benzene and trifunctional silane bearing amine- or thiolgroups in the presence of a fluoride-ion catalyst in an ethanol solution. All the xerogels obtained have a porous structure (500-1000 m2/g) and a high content of functional groups (1.2-2.8 mmol/g). AFM data show that xerogels are formed by aggregation of spherical primary particles. The main factors influencing structural characteristics of these materials are: the nature of the functional group, the spacer flexibility, and in some cases – the ratio of reacting alkoxysilanes.
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Article 09EN: Theoretical description of surfactant aggregation at the solid/liquid interface – comparative study
104-113

Anna Andrzejewska, Mateusz Drach, Jolanta Narkiewicz-Michałek


Department of Theoretical Chemistry, Faculty of Chemistry, Maria Curie-Skłodowska University, 20-031 Lublin, Poland Email: theor@hermes.umcs.lublin.pl

The comparison of two surfactant adsorption models is presented. In both models, the adsorbed phase is assumed to be a mixture of single monomers and aggregates of different shapes and sizes. These surface aggregates are assumed to behave as a 2D fluid of hard disks, i.e. only “excluded area” interactions are allowed in the adsorbed layer. The effects of surface heterogeneity on monomer adsorption are also taken into account. The main difference between the compared models lies in assuming different structures of the surface aggregates. In the first model the aggregates are assumed to be monolayered and symmetrical bilayered disks (hemimicellar and admicellar aggregates model HAM). In the second model the adsorbed surfactant molecules are assumed to form spherical and globular aggregates (SGM), similar to those in the bulk solution. The theoretical expressions for adsorption isotherms and heats of adsorption corresponding with these two models are compared with experimental data for three zwitterionic surfactants adsorbed on the silica surface. The advantages and faults of the two models are discussed.
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Article 10EN: 1-pK and 2-pK model of oxide surface protonation. Are they equivalent?
114-122

Wojciech Piasecki


Group for Theoretical Problems of Adsorption Institute of Catalysis and Surface Chemistry Polish Academy of Sciences ul. Niezapominajek 8, Kraków, 30-239 Poland

Simple mechanism of charge formation on metal oxides in electrolyte solution was outlined. Two basic surface protonation models (1-pK and 2-pK) were presented. It was shown that it is impossible to obtain exactly the same results using both of them when we analyzed together surface charge, electrokinetic potential, and isotherms of electrolyte ions adsorption.
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Article 11EN: Theoretical study of proton binding behavior at the rutile (001) (1x1) crystal face
123-133

Piotr Zarzycki


Group for Theoretical Problems of Adsorption Institute of Catalysis and Surface Chemistry Polish Academy of Science, Kraków, Poland e-mail: piotrek@vega.umcs.lublin.pl

The quantum chemistry methods are employed to study the singly coordinated surface oxygens on the rutile unreconstructed (001) crystal face. The ab-initio predicted charges and proton affinity constants are combined with the Grand Canonical Monte Carlo simulations of the proton binding in order to obtain H+ ions adsorption isotherms. The experimental study of this crystal face is impossible due to its instability, but the same surface sites can be find on the most stable (110) surface. In both quantum chemistry calculations and simulations the solvent is included by using the reaction field approach. In the ab-initio calculations it was achieved by employing the COSMO-RS model while in the simulation procedure by using the Borkovec [1] interaction potential (which includes the polarization effects). The theoretical predictions are very close to the experimental ones, even if the size of the clusters is relatively small.
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Article 12EN: Heterogeneity of activated carbons based on adsorption of phenols from aqueous solutions
134-151

Przemysław Podkoscielny 1, Andrzej Dabrowski 1, Krzysztof Nieszporek 1, Krisztina László 2


1 Department of Theoretical Chemistry, Faculty of Chemistry, Maria Curie-Skłodowska University, pl. M. Curie-Skłodowskiej 3, 20-031 Lublin, Poland
2 Department of Physical Chemistry, Budapest University of Technology and Economics, H-1521 Budapest, Hungary

The heterogeneity of activated carbons (ACs) prepared from different precursors is investigated on the basis of adsorption isotherms of phenol and 2,3,4- richlorophenol from dilute aqueous solutions at various pH values. The Langmuir-Freundlich equation as well as the Dubinin-Astakhov one have been used to estimate the parameters characterizing adsorption from aqueous phenol solutions on heterogeneous carbon surfaces. Adsorptionenergy distribution (AED) functions have been calculated by using an algorithm based on a regularization method. Analysis of these functions for activated carbons provides significant comparative information about their heterogeneity. Besides, literature data on enthalpy values for the transfer of phenol from a solution to surfaces of ACs confirm the correctness of the adsorption energies obtained in our study. The AED functions for phenol on activated carbons, generated by a utilization of the regularization method have been verified. As a verification tool, the Grand Canonical Monte Carlo simulation method carried out on a square lattice has been chosen.
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Article 13EN: Carbon monoxide hydrogenation on bifunctional iron-HZSM5 zeolite catalysts
153-167

Andrzej Machocki, Bogusław Chmiel


Department of Chemical Technology, Faculty of Chemistry, Maria Curie-Skłodowska University, pl. Marii Curie-Skłodowskiej 3, 20-031 Lublin, Poland

The HZSM5 zeolite with the SiO2-to-Al2O3 ratio lower than 200, used as a support of the iron phase or in a physical mixture with the silica supported iron catalyst, increases few times the conversion of carbon monoxide and decreases the rate of the catalyst coking in comparison with those achieved on the zeolite-free Fe/SiO2 catalyst. The reasons of these phenomena have been explained on the basis of disturbance of an adsorption-desorption equilibrium of olefins on the iron phase, resulting from immediate, subsequent conversion of olefins on the zeolite. Their presence in hydrocarbons formed is strongly suppressed. The synthesis of C5+ hydrocarbons is changed in the opposite way to that of olefin amounts. The hydrocarbons derived from carbon monoxide hydrogenation on the HZSH5 zeolite supported iron catalysts contain the aromatic fraction and branched hydrocarbons.
The HZSM5 zeolite with the SiO2-to-Al2O3 ratio below 200 present in the bifunctional catalyst composition may be sufficient when C5+ hydrocarbons production is targeted, but for high contents of branched and aromatics hydrocarbons in the liquid product, the SiO2-to-Al2O3 ratio equal to 30-40 should be preferred.
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Article 14EN: Syntheses and properties of novel 1-[2-(polyhalogenophenoxy)acyl]-3,5-dimethyl-1H-pyrazole
171-185

Bogdan Tarasiuk


Department of Organic Chemistry and Technology Faculty of Chemistry, Maria Curie-Skłodowska University ul. Gliniana 33, 20-614 Lublin, Poland

The results of the study on the syntheses and properties of new 3,5-dimethyl-1H-pyrazole derivatives of 2-[polychloro- (bromo)phenoxy]alkane acids are presented. The compounds were synthesised during the reaction of 2-(polyhalogenoaryloxy)alkanoic chlorides with an on 3,5-dimethylpyrazole and N,N-diethylaniline. The compounds are characterized by means of FTIR, 1H NMR and 13C NMR spectrum using a nuclear magnetic resonance spectrometer, and elemental analysis. Their physical-chemical properties were examined, along with their fungicidal, insecticidal, acaricidal and herbicidal activity. It was found that he highest herbicidal activity characterised the derivatives of 1-(2,4-ichlorophenoxyacetyl)-3,5-dimethyl-1H-pyrazole, 1-[2-(2,4-ichlorophenoxy)propanoyl]-3,5-dimethyl-1H-pyrazole, 1-(2,4,5-trichlorophenoxyacetyl)-3,5-dimethyl-1H-pyrazole and 1-[2-(2,4,5-trichlorophe-noxy)propanoyl]-3,5-dimethyl-1H-pyrazole.
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Article 15EN: Synthesis of thiourea derivatives of 1H-isoindole-1,3 (2H)-dione as potential antiviral agents
186-192

J. Kossakowski, M. Struga


Department of Medical Chemistry, The Medical University, ul. Oczki 3, 02-007 Warsaw

The first antiretroviral agents approved for the treatment of AIDS were nucleosidic inhibitors of reverse transcriptase such as Zidovudine. Later, the human immunodeficiency virus (HIV) protease inhibitors (e.g. saquinavir) were introduced as therapeutics. Recently, a third class of antiretroviral agents, the non-nucleosidic reverse trancriptase inhibitors (NNRTIs) (i.e. nevirapine, delavirdine, efavirenz) have been marketed (1).
From all the active compounds, some common characteristics have emerged. First, NNRTIs interact with a non-substrate binding site that is located in the close vicinity of the substrate binding site of HIV-1. As a consequence, all these compounds are deprived of activity against HIV-2.
Furthermore, structural studies have shown that these derivatives contain a central hydrophilic parts and two hydrophobic moieties, generally an aromatic cycle forming a butterfly-like conformation (2). Finally, most of these compounds contain urea or thiourea function in their structure (3). Searching for new compounds with predictable antiviral properties, our attention was drawn to a group of thiourea derivatives of 1H-isoindole-1,3 (2H)- dione. Imides obtained in Diels-Alder reaction were used as starting materials. These were reacted with hydrazine (80% aqueous solution). The compounds were subjected to the reaction with benzyl, allyl, benzoyl isothiocyanate to be transformed into the corresponding thiourea derivatives.
All of the final compounds were characterized by 1H NMR spectra which were in accordance with the proposed structures.
The general synthetic pathway is given in Scheme 1.
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Volume 60 - 2005

Article 01EN: Conductivity of a concentrated colloidal suspension of spherical particles in an alternating electric field
1-22

F. J. Arroyo 1, F. Carrique 2, M. L. Jiménez 3, Angel V. Delgado 3


1 Departamento de Física, Facultad de Ciencias Experimentales, Universidad de Jaén, 23071 Jaén, Spain
2 Departamento de Física Aplicada I, Facultad de Ciencias, Universidad de Málaga, 29071 Málaga, Spain
3 Departamento de Física Aplicada, Facultad de Ciencias, Universidad de Granada, 18071 Granada, Spai

In this paper the complex (ac) conductivity of a concentrated suspension of spherical colloidal particles is considered in the light of a cell model. Previous works have dealt with the study of the conductivity of a concentrated colloidal suspension for general conditions, including arbitrary zeta potential, particle volume fraction, double-layer thickness, and ionic properties of the solution, but only the static case (dc electric fields) was addressed. In this contribution, the complex conductivity of a concentrated suspension is studied for the same general conditions as in the static case. The numerical data presented in this paper cover a wide range of typical situations including the special case of overlap of double layers of adjacent particles. Like in the static case, the treatment is based on the use of a cell model to account for hydrodynamic and electrical interactions between particles. The two relaxation processes occurring in the frequency range of interest (alpha and Maxwell-Wagner- O’Konski) are analyzed for different values of the ionic strength, particle radius, zeta potential and particle concentration. Roughly speaking, these two relaxations tend to overlap in frequency as the volume fraction of solids increases for otherwise general conditions; in such cases, no clear distinction can be established between them. On the other hand, considerable attention has also been devoted to the numerical analysis of the complex conductivity for those special situations where overlapping between double layers is nonnegligible. Finally, a comparison between theoretical predictions and some experimental results is shown, revealing a general good agreement.
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Article 02EN: Adsorption and structural properties of small-pore mesoporous silicas synthesized using mixed short-chain surfactants as templates
23-33

Jerzy Choma 1, Mieczysław Jaroniec 2, Michal Kruk 2;3


1 Instytut Chemii, Wojskowa Akademia Techniczna, ul. Kaliskiego 2, 00-908 Warszawa, Poland, e-mail: jchoma@wat.edu.pl
2 Department of Chemistry, Kent State University, Kent, OH 44 242, USA e-mail: jaroniec@kent.edu
3 Present address: Department of Chemistry, Carnegie Mellon University 4400 Fifth Avenue, Pittsburgh, PA 15213, USA, e-mail: mkruk@andrew.cmu.edu

Small-pore silicas were synthesized by employing two short-chain surfactants (octyl- and decyl-trimethylammonium bromides) as well as their mixtures as templates. Nitrogen adsorption and powder X-ray diffraction were used to characterize adsorption and structural properties of these materials. The samples exhibited the BET specific surface areas of 770-1040 m2 g-1, and the primary mesopore volumes of 0.34-0.59 cm3 g-1. They had low external surface areas and volumes of secondary pores. The samples had narrow pore size distributions (PSDs) with maxima at 2.3-2.8 nm, and exhibited one strong peak at their XRD patterns. The interplanar spacings corresponding to these XRD peaks were in the range from 2.6 to 3.3 nm. The position of the maximum of PSD changed rather systematically with the average length of alkyl chain of the surfactant or surfactant mixture used as a template, whereas the interplanar spacing values for samples synthesized using single surfactant templates were lower than those for the samples synthesized using surfactant mixtures. These results show that the use of mixtures of short-chain surfactants allow one to tailor the diameter of mesopores of small-pore surfactant-templated silicas.
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Article 03EN: The influence of Ca2+ and La3+ and magnetic field on the surface free energy components of alumina
34-46

Lucyna Hołysz, Aleksandra SzczeŚ, Emil Julian Chibowski


Department of Physical Chemistry–Interfacial Phenomena, Faculty of Chemistry, Maria Curie-Skłodowska University, 20-031 Lublin, Poland, karol@hermes.umcs.lublin.pl; aszczes@hermes.umsc.lublin.pl; emil@hermes.umcs.lublin.pl

A novel method based on the imbibition and drainage of the probe liquid into a porous bed was applied to determine surface free energy components of alumina. Apolar Lifshitz-van der Waals component, and electron-donor and electron-acceptor parameters of polar (acid base) component were determined from weight of probe liquids remained in the porous bed of bare alumina. The influence of Ca2+ and La3+ ions and magnetic field effect on these components were investigated. Both, the presence of deposited ions and magnetic field, influence on changes in electron-donor and electronacceptor parameters, which resulted from the presence of hydrogen bonding on the alumina surface. The observed changes in acid-base interactions (hydrogen bonding) result from changes in the structure of the water film at the surface.
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Article 04EN: Effect of electrolytes on the electroneutrality at the interface
47-64

Nikola Kallay, Ana Čop, Tajana Preočanin, Davor Kovačević


Chemistry, Department of Chemistry, Faculty of Science, University of Zagreb, Marulićev trg 19, P.O. Box 163, 10001 Zagreb, Croatia nkallay©chem.pmf. hr

Recently, the measurements of the electrostatic potential at the inner plane of the electrical interfacial layer (surface potential ϕ0) were introduced by using metal oxide electrodes. The evaluation of the surface potential from the electrode potential requires the knowledge of the point at which the surface potential is zero, i.e. the point of zero potential (p.z.p., pHpzp). The numerical analysis based on the 2-pK mechanism of the Surface Complexation Model showed that pHpzp approximately coincides with pHiep if the ionic strength is kept enough low. At higher ionic strengths the values of pHiep and pHpzc might be different and pHpzp lies between these two point and is still close to the original value at low ionic strength, i.e. the point of electroneutrality pHeln. The experimental results of electrode potential dependence on pH measured with hematite electrode showed appreciable reproducibility in the acidic region. The slope of the ϕ0(pH) function is found to be significantly lower in magnitude than the Nernstian which is more pronounced at higher ionic strengths.
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Article 05EN: Nitrogen and argon adsorption on non-graphitized carbon black: Application of Density Functional Theory*
65-78

E. A. Ustinov 1, D. D. Do 2


1 On leave from Saint Petersburg State Technological Institute (Technical University), 26 Moskovsky Prospect, 198013, Russia
2 (corresponding author), Department of Chemical Engineering, University of Queensland, St. Lucia, Queensland 4072, Australia

Analysis of adsorption equilibria of nitrogen at 77 K and argon at 77 and 87.3 K on non-graphitized carbon black (NGCB) is considered with a Non- Local Density Functional Theory (NLDFT). It was shown that nitrogen and argon adsorption isotherms could be quantitatively correlated with a version of NLDFT accounting for the amorphous nature of NGCB and its surface roughness. Instead of being calculated from some standard equations, such as the 10-4-3 Steele equation, the solid-fluid potential is obtained experimentally from adsorption isotherms and it was found to be a fast decaying function that becomes negligibly small at a distance of about two collision diameters from the surface. The model presented in this paper implicitly accounts for the energetic heterogeneity of the disordered graphite surface and yet it retains the simplicity of the conventional NLDFT as applied to graphitized thermal carbon black. The approach may be further extended to slit pores whose walls are non-graphitized surface, and such an approach will raise questions on the conventional aproach where pore walls are assumed to behave like a graphite surface.
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Article 06EN: Monte Carlo simulation of binary mixture adsorption of methane and carbon dioxide in carbon slit pores
79-92

Y. Kurniawan, S. K. Bhatia, V. Rudolph


Department of Chemical Engineering, The University of Queensland, Brisbane, QLD 4072, Australia

In this article we utilise Grand Canonical Monte Carlo (GCMC) simulation to investigate the adsorption of binary mixture of methane and carbon dioxide in slit-shaped carbon pores, ranging from around 0.75 to 7.5 nm in width, for high pressure up to 300 bar and temperature range of 308 – 348 K, as a preliminary study for the CO2 sequestration problem that remains a serious challenge to humanity. For the binary adsorption, the selectivity of carbon dioxide relative to methane is lower at higher slitwidths or higher temperatures or lower bulk mole fraction of carbon dioxide. Upon increase of pressure the selectivity initially increases to a maximum value, and subsequently drops before attaining a constant value at pressures higher than 300 bar for any bulk mole fraction of carbon dioxide. While the selectivity increases with temperature in the initial pressure-sensitive region, the constant high-pressure value is temperature independent. Optimum selectivity at any temperature is attained at a pressure of approximately 35 bar at high bulk mole fraction of CO2, increasing to 90-100 bar at low bulk mole fractions.
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Article 07EN: Development and validation of a methodology for the reliable characterization of porous materials
93-118

Lourdes F. Vega 1, C. Herdes 1, M. A. Santos 2


1 Institut de Ciència de Materials de Barcelona, (ICMAB-CSIC), Consejo Superior de Investigaciones Científicas, Campus de la U.A.B., Bellaterra, 08193 Barcelona, Spain
2 Center for Computational Biology. The Hospital for Sick Children. Toronto, Ontario, Canada M5G 1X8

This article summarizes the application of a methodology for Pore Size Distribution (PSD) calculations in which a regularization procedure is combined with individual adsorption isotherms obtained from Grand Canonical Monte Carlo simulations. The methodology combines mathematical and physical requirements in order to obtain reliable PSDs. A protocol is proposed to isolate the different effects contributing to the obtained PSD function, in a systematic manner. The PSD robustness is measured imposing random errors over the experimental data. The methodology is first applied to a member of the MCM-41, chosen for its particular structure, in which the adsorption takes place in noninterconnected pores. The accuracy of the results shows the precision of the method for this case, validating the independent pore model. The method is next applied to a SBA-15 material, as representative of materials with both, meso- and micropores, checking the reliability of the method for materials with connected pores. Excellent agreement is also found in this case. In addition, molecular simulations provide new insights into the studied systems, pointing out the need of high-resolution isotherms to describe the presence of complementary microporosity in the SBA material.
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Article 08EN: Wettability of polymeric solids by aqueous solution of surfactants
119-133

K. Szymczyk, B. Jańczuk, A. Zdziennicka, W. Wójcik


Departament of Interfacial Phenomena, Faculty of Chemistry, Maria Curie-Skłodowska University, pl. M .C. Skłodowskiej 3, 20-031 Lublin, Poland Fax: (48-81) 533-3348, e-mail:bronek@hermes.umcs.lublin.pl

Advancing contact angle (q) measurements were carried out for aqueous solutions of cetyltrimethylammonium bromide (CTAB), cetylpyridinium bromide (CPyB), sodium dodecyl sulfate (SDS), sodium hexadecyl sulfonate (SHS) and Triton X-100 (TX-100) on polytetrafluoroethylene (PTFE) and polymethyl methacrylate (PMMA). The obtained results indicate that there were only small contact angle changes over the range of surfactant concentrations in the solution, corresponding to the unsaturated surfactant layer at the aqueous solution-air interface. However, when saturation of the surfactant layer was reached a considerable decrease in the contact angle as a function of concentration was observed. The obtained results also indicate that in the range of small concentrations of surfactants the contact angle, with exception of TX-100, does not depend on the type of the surfactant, but in the concentration range corresponding to the saturated layer at solution-air interface, it depends on the type of surfactant. On the basis of the values of contact angle and surface tension of aqueous solution of surfactants a linear dependence between the adhesional tension (gLV cosq) and surface tension (gLV) was found. The slope of gLV cosq vs gLV lines for PTFE does not depend on the type of surfactant and is equal -1, which suggests that the surface excess of the surfactant concentration at the PTFE-solution interface is the same as that at the solution-air interface for a given bulk concentration. It was also found that the work of adhesion of aqueous solution of surfactants to PTFE surface does not depend on the type of surfactant and its concentration, which suggests that the Lifshitz-van der Waals forces interact only at solution-air and PTFE-solution interfaces, and that the contribution of these forces in surface tension of aqueous solution of surfactants studied does not depend on the surfactant concentration. In the case of PMMA the slope of gLV cosq vs gLV lines depends on the type of surfactant and is considerable different from -1, which suggests that the surface excess of surfactant concentration for a given bulk concentration at solution-air interface is higher than at PMMAsolution interface. Also the work of adhesion of solution of surfactant to PMMA surface depends on the type of surfactant and its concentration, which suggests that across PMMA-solution interface van der Waals and polar interactions take place. Basing on the dependence between the adhesional tension and surface tension the critical surface tension of PTFE and PMMA wetting was found.
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Article 09EN: Size effect of binding energy of the hydrogen atom on Ptn(100) clusters
134-144

Piotr Matczak, Stanisław Romanowski


Chair of Theoretical Chemistry, University of Łódź, Pomorska 149/153, PL-90-236 Łódź, Poland

In this paper we have employed the semiempirical PM5 method to investigate a size effect of the binding energy of the H atom on a variety of platinum clusters. The examined clusters of the (100) face symmetry have included up to 101 platinum atoms placed from one to six layers. Our theoretical model of the H atom chemisorption on the Ptn(100) clusters can be treated as a platinum (100) surface with almost zero coverage of hydrogen. A comparison of PM5 results with the Analytical Cluster Model has been also done.
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Article 10EN: Operando spectroscopy: new methodology or new name?
145-150

Janusz Ryczkowski


Faculty of Chemistry, Department of Chemical Technology, Maria Curie-Sklodowska University, pl. M. Curie-Skłodowskiej 3, 20-031 Lublin, Poland tel. +48-81 537-55-96; fax: +48-81 537-55-65; e-mail: ryczkows @ hermes. umcs. lublin.pl

This paper describes bases of the operando methodology. Moreover, indicates similarities as well as differences between classical in situ studies and operando spectroscopy. Infrared in situ studies in catalysis are given as an example that operando methodology was successfully applied in the past under the classical name - in situ studies.
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Article 11EN: Improving fundamental ideas of Dubinin, Serpinsky and Barton - further insights into theoretical description of water adsorption on carbons*
151-182

Sylwester Furmaniak, Piotr A. Gauden, Artur P. Terzyk, Radosław P. Wesołowski, Gerhard Rychlicki


Nicolas Copernicus University, Department of Chemistry, Physicochemistry of Carbon Materials Research Group, ul. Gagarina 7, 87-100 Toruń, Poland

The purpose of the current study is the review the most important papers related to water adsorption on carbons, and published in four different fields, namely: computer simulations (CS), quantum methods (QM), analytical adsorption isotherm formulas (AF) and adsorption calorimetry (AC). The special attention is paid to the (AF) inspired by the pioneering papers of Dubinin, Serpinsky, Barton and co-workers. We present the concept of “the decrease in the number of adsorption sites” and we assign a physical meaning to ac,B2. - the empirical parameter of Barton’s adsorption isotherm equation. Moreover, we discuss the applicability, advantages and defects of the most important (AF) presenting some new approaches in this field. Next, we solve some of the deficiencies of previous studies considering the mechanism of water adsorption on solids, by taking into account the possibility of the existence of various types of the hydrophilic centers. At the start we improve the original D’Arcy and Watt equation taking into account the dependence of the concentration of the surface primary sites on the amount of the secondary ones. Next, we assume that the surface of an adsorbent consists of regions of heterogeneity at the molecular level, and the multi-site generalized D’Arcy and Watt model is proposed. Finally we improve the Barton model and the original DW relationship, respectively. It can be noticed that for the both cases we propose to take into account the finite adsorption space via the term (1–kGB1an). Moreover, the chemisorption of water molecules on the various types of the primary high-energy adsorption sites is considered. For all presented new models we show the corresponding adsorption enthalpy equations.
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Article 12EN: The influence of the closest approach to the wall distance on phase behavior of ionic fluids in slit-like pores: a density functional approach for the restricted primitive model
183-195

Katarzyna Bucior, Andrzej Patrykiejew, Stefan Sokołowski, Grzegorz UkociSki


Department for the Modelling of Physico-Chemical Processes, Faculty of Chemistry, Maria Curie-Skłodowska University, 20-031 Lublin, Poland, kbucior@elrond.umcs.lublin.pl, andrzej@pluto.umcs.lublin.pl, stefan@zool.umcs.lublin.pl

We apply density functional theory to investigate changes in the phase behavior of ionic fluid in narrow slit-like pores, caused by the difference in the distances of the closest approach to pore walls of two species, Ds. This difference causes that the point of zero surface charge of the walls does not coincide with the zero value of the electrostatic potential at the wall. Our calculations demonstrate that an increase of Ds increases slightly the value of the critical temperature and lowers the density of the coexisting liquidlike phase.
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Article 13EN: Computer analysis of microporous adsorbents with adsorption models of LBET class
196-217

Mirosław Kwiatkowski 1, Jan Tadeusz Duda 2, Janina Milewska-Duda 1


1* faculty of Fuels and Energy, AGH-University of Science and Technology al. Mickiewicza 30, 30-059 Kraków, Poland tel. (48 12) 617 41 73; e-mail: kwiatków@agh.edu.pl 7*tel. (48 12) 617 21 17; e-mail: milewska@agh.edu.pl
2 Faculty of Management, AGH-University of Science and Technology al. Mickiewicza 30, 30-059 Kraków, Poland tel. (48 12) 617 45 06; e-mail: jdu@ia.agh.edu.pl

The reported research concerns applicability of new LBET models for heterogeneous multilayer adsorption to examination of microporous carbonaceous adsorbents. The models are based on a generalized BET theory presented in our earlier papers. They are aimed at drawing information on pore structure and capacity by analysis of adsorption isotherms of small molecule adsorbates. In the theory adsorption of small, a nearly spherical molecules in irregular pores of molecular size is considered with side adsorbate-adsorbate interactions have being neglected. The molecules are located in pores by forming clusters, the size of which is limited by geometry of pores. The set of adsorbate molecules, which were adsorbed mainly due to adhesive interactions with the adsorbent matter, is treated as the first layer adsorption.
Joining further molecules is viewed as the second, third, and following layer adsorption. The main idea of the presented approach to modelling of microporous structure consists in introducing of realistic relationships between geometrical properties of pores and adsorption energy.
The paper shows that a multivariant identification of adsorption isotherms, employing the LBET type formulas, gives an insight into pore size distribution and dominant pore shape, and provides more reliable evaluation of material surface area than the classical models.
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Article 14EN: TAED – IR studies of bleach activator for peroxide-based detergents
218-229

Janusz Ryczkowski, Sylwia Pasieczna


Faculty of Chemistry, Department of Chemical Technology, Maria Curie-Sklodowska University, pl. M. Curie-Skłodowskiej 3, 20-031 Lublin, Poland tel. +48-81 537-55-96; fax: +48-81 537-55-65; e-mail: ryczkows @ hermes. umcs. lublin.pl

In the present work IR studies are discussed. The studies concerned TAED (tetraacetyl ethylenediamine) bleach activator applied for peroxide-based detergents. It was stated that infrared spectra of the coloured TAED granules available in the washing powders are of the same nature as the spectrum of commercial chemical reagent, and there is no influence of the colourant applied. Depending on the temperature treatment an alkaline TAED solutions can undergo transformation and degradation. Moreover, the presence of hydrogen peroxide in the alkalined TAED solution accelerates its transformation. There can be observed TAED-inorganic support interaction, which nature depends on the pH of the solution.
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Article 15EN: Application of Monte Carlo simulations for the calculation of differential capacitance of double electrical layer formed at the metal oxide/electrolyte interface
230-244

Piotr Zarzycki 1, Paweł Szabelski 2, Wojciech Piasecki 1, Robert Charmas 3


1 Laboratory for Theoretical Problems of Adsorption, Institute of Catalysis and Surface Chemistry, Polish Academy of Science, Cracow, Poland
2 Department of Theoretical Chemistry, Faculty of Chemistry Maria Curie-Skłodowska University, Lublin, Poland
3 Department of Biochemistry, Faculty of Physical Education in Biała Podlaska, The Józef Piłsudski Academy of Physical Education, Warsaw, Poland

Mathematical relations between fundamental quantities describing double electrical layer (surface potential, surface charge density and differential capacitance) were derived by analyzing the definition of the differential capacitance. The obtained relations make it possible to calculate one of these quantities from two others as a function of pH.
We used these relations combined with the Monte Carlo simulation results for surface charge to calculate differential capacitance. Additionally we verified the equations by using experimental data for surface potential. Finally we discussed the pH-dependence of differential capacitance of double layer formed at the metal oxide/electrolyte interface.
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Article 16EN: Pore size distributions of complex systems
246-255

Vladimir Gun’Ko 1, Roman Leboda 2


1 Institute of Surface Chemistry, 17 General Naumov Street, 03164 Kiev, Ukraine
2 Maria Curie-Skłodowska University, 20-031 Lublin, Poland

An approach based on the sum of integral adsorption isotherm equations including independent distribution functions for each component of complex adsorbents and solved by using self-consistent regularization was developed and tested for mechanical mixtures of carbon and silica adsorbents. For individual adsorbents, e.g. carbons or silica gels, the developed procedure gives the pore size distributions close to those calculated using the DT method.
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Article 17EN: The kinetics of sorption of a CO2 and CH4 mixture on hard coals due to the selective sorption of carbon dioxide
256-273

Grażyna Ceglarska-Stefańska, Katarzyna Zarębska


AGH University of Science and Technology, Faculty of Fuels and Energy, al. Mickiewicza 30, 30 - 059 Cracow, Poland tel./fax : +48 (012) 617 20 66; e-mail:zarebska@uci.agh.edu.pl

The influence of the physical and chemical properties and the composition of the sorbed gas on the sorption capacity of hard coal must be taken into account in an analysis of such coals as specific collectors of mine gases. It follows from studies of CO2 and CH4 sorption on hard coals that the sorption process for CH4 is slower than for CO2. On the basis of analysis of sorption kinetics for these gases it might be assumed that when gases flowing through the bed are mixed, as a rule the gas flowing out from the bed is enriched with CH4. The analysis presented was based on a comparison of the results of sorption studies of single gases (CO2 and CH4) and their mixtures in two hard coals (81.1% C and 90.12% C). Knowledge of these effects should facilitate further investigation of the relationship between the properties of a hard coal and methane evolution to establish those factors that enhance the rate and effectiveness of the process.
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Article 18EN: Influence of nonionic surfactant concentration on the removal of the finest grains on gas bubbles
274-281

Kazimierz Jurkiewicz


Department of Interfacial Phenomena, Faculty of Chemistry, Maria Curie-Skłodowska University, 20-041 Lublin, Poland e-mail: kjurkiew@hermes.umcs.lublin.pl

In this paper, the influence of surfactant (Span 20) concentration (within 10-7–10-3 M, in aqueous solution) on the removal of the marble finest grains in water sheath of gas bubbles as well as on the grain aggregations in the solution has been studied. There could have been observed the irregular changes of water and grains removal depending on the surfactant concentration. The marble grain aggregation does also change irregularly with the increase of the surfactant concentration. During the experiments, pH of the suspension increased (from initial pH 5.8) or decreased (from pH 10). DpH changes irregularly with the change of surfactant concentration. The suspension tends to achieve a pH value, close to that of pH PZC. The higher is the grain aggregation the lower is the grain removal in case of a hardly significant water removal, up to 10-5 M of Span 20. For the higher concentrations there is a higher removal of grains and water as well as a more considerable aggregation of the grains.
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Article 19EN: Influence of diluent composition on the porous structure of 4,4’-diphenyl dimethacrylate - divinylbenzene copolymers
282-295

Barbara Gawdzik, Beata PodkoŚcielna


Faculty of Chemistry, Maria Curie-Skłodowska University, pl. Marii Curie-Skłodowskiej 5, 20-031 Lublin, Poland, tel./fax +48-815242251 barbarag@hermes.umcs.lublin.pl

Synthesis of the copolymer of 4,4’-diphenyl dimethacrylate and divinylbenzene is presented. To obtain these copolymers in the form of the porous beads suspension-emulsion polymerization was applied. As a poreforming diluent, the mixture of toluene (good solvent) and 1-decanol (nonsolvent) was used. The influence of the composition of two-component diluent on the porous structure of the copolymers has been examined. For copolymer prepared in the presence of larger concentration of toluene in the mixture with 1-decanol more regular porous structure was obtained.
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Article 20EN: Preparation of synthetic carbon adsorbents by polyvinyl chloride (PVC) carbonization
296-310

M. Seredych 1, Andrzej Gierak 2


1 European Collegium of Polish and Ukrainian Universities, 20-031 Lublin, Poland
2 Faculty of Chemistry, Maria Curie-Skłodowska University, 20-031 Lublin, pl. M.C. Skłodowskiej 3, Poland

Preparation of synthetic carbon adsorbents by carbonization of polyvinyl chloride (produced by Anwil, Włocławek, Poland) is described in the paper. The influence of polyvinyl chloride (PVC) carbonization conditions on the porous structure of the obtained carbon was studied. Part of the prepared carbonizates was activated in the atmosphere of in water vapour and carbon dioxide (600 – 800 oC). The influence of individual processes on structural properties of the obtained synthetic carbons was studied. Structural characteristics were determined by means of nitrogen adsorption (-196oC, BET method) and relative isotherms adsorption as.
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Article 21EN: Recognition elements for metal ions as parts of optical chemical sensors
RU: 2013-05-30
311-327

Andrzej M. Kłonkowski, Krzysztof Kledzik, Marcin Gwiazda, Maja Orłowska


Faculty of Chemistry, University of Gdańsk, Gdańsk, Poland

This paper focuses on chromoionophores and fluoroionophores immobilized or covalently attached in/on a matrix or support, respectively. Silica xerogel serves as the matrix and amino-modified silicate or mesoporous silicate (MCM-48) as the support. The studied materials prepared by sol-gel procedure can be treated as potential recognition elements for optical chemical sensors. Action of the recognition elements is based on absorption spectra changes or template effect for the chromoionophores and photoinduced electron transfer (PET) effect in the case of the fluoroionophores.
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Article 22EN: Electric properties of composite materials based on porous ceramics and low temperature ionic liquids
328-335

Marek Kosmulski, M. Szafran, P. Żukowski, K. Marczewska-Boczkowska, Cz. Kozak, Cz. Saneluta


Faculty of Electrical Engineering and Computer Science, Lublin University of Technology, Nadbystrzycka 38 A, 20-618 Lublin, Poland and Faculty of Chemistry, Warsaw University of Technology, Noakowskiego 3, 00-664 Warsaw, Poland.

Composite materials were obtained by saturation of pores of a monolithic porous ceramic matrix with low temperature ionic liquids. Tetrafluoroborates, hexafluorophosphates, and triflates (trifluoromethanesulfonates) of 1-alkyl-3- -methylimidazolium (alkyl=butyl, hexyl, octyl or decyl) were studied. The above ionic liquids have a broad electrochemical window (up to 5.5 V), and the electrochemical window of the composite materials is even broader. The conductivity of the ionic liquids is approximately proportional to their reciprocal viscosity. The composites (porous material with porosity of 27 %) show a conductivity only slightly lower than the corresponding ionic liquid with a few exceptions.
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Article 23EN: Application of biosurfactants for the mineral surfaces modification
336-346

Zygmunt Sadowski, Izabela Polowczyk, Ewa Jażdżyk, Agnieszka Szubert


Wrocław University of Technology Wybrzee Wyspiaskiego 27, 50-370 Wrocław, Poland zygmunt.sadowski@pwr.wroc.pl

Modification of surface properties of various minerals can be a key for the mineral separation. Biomodification of the mineral properties was realised by the adsorption of biosurfactants, which were produced by Pseudomonas aeruginosa. In this study, it is shown that Pseudomonas can grow in the presence of minerals and produce a biosurfactant with substantially changes of the surface tension of supernatant. Measurements confirmed that an interaction of all used minerals with the supernatant caused a decrease of zeta potential. As expected, the ieps of mineral particles were shifted to lower pH values after the interaction with biosurfactant. Bio-pretreatment of the minerals has affected on the settling properties of mineral suspension. The settling results showed a strong flocculation for investigated suspensions at the present of the small biosurfactant concentration (2 % v/v).
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Article 24EN: Waksmundzki’s tube – a device for studying a dispersion system
347-358

Wiesław Wójcik, Bronisław Jańczuk, Robert Ogonowski


Department of Interfacial Phenomena, Faculty of Chemistry Maria Curie-Skłodowska University, pl. M. C. Skłodowskiej 3 20-031 Lublin, Poland

The goal of the paper is to review the results of the destruction time of the solid sediment column structure measurements using a simple device which was elaborated by Waksmundzki and co-workers. The authors and Russian researchers used the device to determine the influence of the flotation reagents on the stability of the dispersion system and the obtained results are shortly described. Next, we summarized the results of the destruction time of coal and silica sediment column structures formed in to two homologous series of liquids i.e. alkane and alcohol. On the basis of the results the manner of the calculation of the detachment and attachment forces in the system solid particle/liquid (alkane or alcohol) /solid particles is also presented. Some unpublished results were advantageous to explanation of the changes of the attachment and detachment forces.
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Article 25EN: Water on solid surfaces
359-375

Erich Robens


Institut für Anorganische Chemie und Analytische Chemie Johannes Gutenberg Universität, Mainz Duesbergweg 10-14, D-55099 Mainz, Germany, erich.robens@t-online.de

Earth and water are two of the four antique elements. Of special interest however is the space between the interface water/solid. In the macro-area economic and cultural developments are concentrated on the coastal region. In the micro-area a great number of chemical and physical processes take place, many of which are important for the existence and development of life. Increasingly interface processes are applied in techniques and methods are used based on interface effects. On the other hand, the omnipresence of water at surfaces which are exposed to the atmosphere often disturbs remarkably.
In comparison with other liquids water has anomalous features. In the free water volume the molecules form variable structures. Also vizinal water is structured and shows strange effects. Different types of binding at the surface or in the interior of a solid can be observed. The water molecule is angled, its shape determining its polarity. This facilitates its analytical detection. Very different methods can be applied in the determination of water uptake, humidity, water content or dry mass of solids. These parameters, however, are not well defined and cannot be determined exactly. Usually results from different measuring methods are not comparable. A short survey on the large variety of measuring methods is given and results of gravimetric sorption measurements with water vapour and nitrogen, quasi-isothermal thermogravimetry and Karl Fischer method are compared.
Future European and American missions to Mars will be focussed on the search for life or traces of it. A precondition for the existence of complex organisms is liquid water which may appear only temporarily at the surface of that dry planet. We assume that in some depth water adsorbed on soil exists as a permafrost structure. Therefore we intend to investigate the adsorptive features of Martian soil. It is reported on the project of a gravimetric experiment on Mars.
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Volume 59 - 2004

Article 01EN: The adsorbed solution theory with Wilson's activity. Adsorption equilibria and calorimetry
3-18

Krzysztof Nieszporek


Maria Curie-Sklodowska University, Faculty of Chemistry Department of Theoretical Chemistry pi M. Curie-Sklodowskiej 3, 20-031 Lublin, Poland e-mail: krzysn@hektor. umcs. lublin.pl

The modified Adsorbed Solution theory is used to describe the calorimetric effects accompanying mixed-gas adsorption equilibria. As the model of non-ideality of adsorbed phase the Wilson's parameters are used. The obtained results were compared with the regular adsorbed solutions theory and the Flory-Huggins activity. The simple way to minimize the number of best-fit parameters in the Wilson's model is presented. Theoretical expressions for phase diagrams and isosteric heats of adsorption are compared with the experimental data.
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Article 02EN: Micellar medium structure of the cetyltrimethylammonium - oxyethylated polyethylenimine - water system
19-24

R. Bakeeva 1, A. Rajewska 2, G. Zakirova 1, T. Gorbunova 1, Yu. Kovalev 3, A.h. Islamov 3, A. Kuklin 3, V. Sopin 1


1 Kazan State Technological University, Kazan, Russia
2 Institute of Atomic Energy, Swierk, 05-400 Otwock, Poland
3 Joint Institute for Nuclear Research, LNP, Dubna, Russia

We have used several experimental methods including viscosity and surface tension measurements as well as small angle neutron scattering method for the investigation of the associations in the cetyltrimethylammonium bromide - oxyethylated polyethylenimine - water ternary system. It is shown that in this system cetyltrimethylammonium bromide micelles coexist with molecular or polymer-colloidal complexes formed by cetyltrimethylammonium bromide monomers adsorbed on the polymer.
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Article 03EN: The influence of sample treatment on SPME extracts from conifers. I. Comparison of terpene composition in Engelmann Spruce (Picea engelmanii) using hydrodistillation, SPME and PLE
25-42

M. Mardarowicz 1, D. Wianowska 1, A. L. Dawidowicz 1, R. Sawicki 2


1 Faculty of Chemistry, Maria Curie-Sklodowska University, 20-031 Lublin, pi Marii Curie-Sklodowskiej 3, Poland
2 Botanical Garden of Maria Curie-Sklodowska University in Lublin 20-830 Lublin, ul. Slawinkowska 3, Poland

Terpenes emitted by conifer trees are generally determined by analysing plant extracts or essential oils, prepared from foliage and cones using steam distillation. The application of these procedures limits experiments to cut plant materials. Recently headspace techniques have been adopted to examine terpene emission by live plants. This paper deals with the application of Solid Phase Micro-Extraction (SPME) for the analysis of terpenes emitted by conifers foliage of Engelmann spruce (Picea engelmanii), including its seedlings. The compositions of SPME extracts obtained for destroyed and non-destroyed old and juvenile spruce needles are compared with the compositions of essential oils and PLE extracts corresponding to the same plant materials. No substantial differences have been found in the qualitative terpene composition estimated by analysing essential oil and PLE and SPME extracts from non-destroyed old and juvenile foliage. The disintegration of spruce needles results in the formation of a significant amount of myrcene in the case of the old conifer foliage and non-terpenoic compounds in the case of juvenile conifer foliage. This phenomenon can be attributed to enzymatic reactions occurring in the destroyed plant cells.
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Article 04EN: Voltammetric determination of malathion
43-49

M. K. Pawlak


Institute of Chemistry, Poznan University of Technology, 60-965 Poznan, Poland

The cathodic adsorptive stripping differential pulse voltammetric method was proposed for the determination of malathion {S-bis (etoxycarbonyl) ethyl O,O-dimetyl phosphorodithioate}. The voltammetric response was evaluated in 0,04 mol 1-1 Britton-Robinson buffer with respect to the accumulation time and potential, and concentration dependence. The relationship between peak current and malathion concentration was linear within the range of 1x10-7 - 8x10-7 mol 1-1. Interferences from some other organophosphorus insecticides on the determination of malathion were studied.
voltammetry, malathion, organophosphorus insecticides.
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Article 05EN: Investigation on dyes oxidation by Fenton's reagent in aqueous medium
50-57

A. Jóźwiak, S. Wiktorowski, A. Dębicka


Institute of General and Ecological Chemistry, Technical University of Łódź, 90-924 Łódź, ul. Żwirki 36

Investigations on oxidation of two dyes: Acid Violet 1 and Direct Blue 74 were carried out with application of Fenton's reagent (hydrogen peroxide in the presence of Fe2+ ions). These dyes are representatives of acid and reactive dyes. The effect of hydrogen peroxide dose and concentration of Fe2+ ions on efficiency of colour removal in model solutions of dyes at concentration of 100 mg/L in the pH range from 2 to 4 was determined. The efficiency of the oxidation process was controlled by measurements of changes in TOC (total organic carbon) and absorbance values (spectrophotometric method) vs. time. Under optimum conditions of the reaction, colour removal was relatively high (90-95%) in the case of both dyes. However, their susceptibility to oxidation was found to be different.
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Article 06EN: Application of oxidation process with the use of H2O2 and NaCIO to dyes aqueous solutions
58-66

R. Tosik, A. Jóźwiak, M. Mitros


Institute of General and Ecological Chemistry, Technical University of Łódź, Żeromskiego 116, 90-924 Łódź, Poland tel (48-42) 6313118, fax (48-42) 6313103

Hydrogen peroxide and sodium hypochlorite were applied to discoloration of dyes Reactive Orange 20 and Reactive Blue 13 in water solution concentration 100 mg L-l. Influence of ferrous ions concentration ranging from 0 to 30 mg L-l, different doses of oxidants at varied pH and at ambient temperature was investigated. Both dyes were oxidized by hydrogen peroxide at pH below 4 at 5 mg L-l Fe2+ ions as catalyst. Oxidation by sodium hypochlorite of Reactive Orange 20 was effective at pH below 4 with the presence of 5 mg L-l of ferrous ions. Reactive Blue 13 was sufficiently discolored by sodium hypochlorite both at values of pH below 4 and at pH 8. High removal of color (95-100 %) was obtained for dyes used.
discoloration, dyes, hydrogen peroxide, sodium hypochlorite
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Article 07EN: Spectrophotometric determination of Fe (II) in pharmaceutical preparations using heterodiazophenoles
67-73

S. Zaręba, M. M. Zaręba-Giezek


Department and Chair of Bromatology of the Department of Pharmacy, Skubiszewski Medical University of Lublin, Staszica 4, 20-081 Lublin

3 -mercapto-5 -(2' ,4' -dihydroxyphenyloazo-1')-1,2,4-triazol (METRIAP) and 5-(5'-mercapto-1,3,4-tiadiazolo-2'-azo)-2,4-dihydroxybenzoic acid (METIDAREZ-p) were used for determination of milligram quantities of Fe (II) in pharmaceutical preparations as Ferrum, Ferrum 4mg +Vit. C, Pan Vitan for women and TardyferonR. The stability of the complexes with Fe (II) was expressed as log K at the pH of 10.3 and with METRIAP it was 16.46, while with METIDAREZ-p at the pH of 7.4 it was 14.25. Iron ions (II) after mineralisation and reduction of Fe III to Fe II were determined spectrophotometrically.
2-mercapto-l,2,4-triazole and2-mercapto-l,3,4-thiadiazole azo dyes, iron determination, spectrophotometry, AAS, pharmaceutical preparations
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Article 08EN: Studies on syntheses and biological activities of novel 3,5-dimethylpyrazole compounds containing [monohalogeno-(methyl)phenoxy] acyl group
77-88

B. Tarasiuk


Maria Curie-Skłodowska University, Faculty of Chemistry Department of Organic Chemistry and Technology Gliniana 33, 20-614 Lublin, Poland

The results of the study on the syntheses and properties of new 3,5-dimethylpyrazole derivatives of 2-[methyl-, aryl-, monochloro-(bromo)phenoxy]alkane acids are presented. The compounds were synthesised during the reaction of 2-(aryloxy)alkanoic chlorides with an on 3,5-dimethylpyrazole and diethylaniline. The chemical structure of the newly obtained derivatives was confirmed through elementary and spectrophotometer FTIR analysis and spectroscopy of ^-NMR. Their physico-chemical properties were examined, along with their fungicidal, insecticidal, acaricidal and herbicidal activity. It was found that he highest herbicidal activity characterised the derivatives of l-(4-chloro-2-methylphenoxyacetyl)-3,5-dimethylpyrazole and 1 -[2-(4-chloro-3,5-di-methylphenoxy)propio-nyl] -3,5 -dimethylpyrazole.
derivatives of the 3,5-dimethylpyrazole of the 2-[methyl-, aryl-, monochloro-(bromo)phenoxy]alkane acids; synthesis, structure, properties, herbicidal activity
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Article 09EN: Synthesis of 5-(3-amino-2-hydroxypropoxy)-2,3-diphenyl--1,2,4-triazol derivatives
89-97

J. Kossakowski, M. Struga


The Medical University, Department of Medical Chemistry, Oczki 3, 02-007 Warsaw

This paper presents the preparation of a number of new derivatives of 2,3-diphenyl-l,2,4-triazol-5-ol with an expected p-adrenolytic activity.
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Article 10EN: Synthesis of new N-substituted isoindoles with an expected anxiolytic and/or (3-adrenolytic activity. Derivatives of 4-isobutoxy-497-ethano-3a949797a-etrahydro-lH-isoindole-l,3,6(2H)trione
98-107

J. Kossakowski, A. Wojciechowska


The Medical University, Department of Medical Chemistry, 3 Oczki Str., 02-007 Warsaw

This paper presents the synthesis of a number of new derivatives of 4-isobutoxy-4,7-ethano-3a,4,7,7a-tetrahydro-lH-isoindole-l,3,6(2H)trione with an expected anxiolytic and/or p-adrenolytic activity.
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Article 11EN: Thioether glycidyl resins II. Synthesis, structure and properties of the addition products bis[p-(293-epoxypropyl)thiophenyl]methane with acrylic acid
108-121

J. Nowak, W. Majewski, W. Charmas


Maria Curie-Skłodowska University, Faculty of Chemistry Department of Organic Chemistry and Technology, MCS University, ul. Gliniana 33, 20-614 Lublin, Poland

The synthesis of bisthiophenol-F glycidyl acrylate (BIS-GATF) was described in the addition reaction between epoxide resin and acrylic acid. The reaction was carried out without a solvent (in the alloy) and in the solvent (xylene). The reaction kinetics between the epoxide and carboxyl groups during the BIS-GATF reaction was observed using chemical analytical methods and in the infrared radiation (IR). It was found that the esterification reaction is of II order at a the temperatures over 45°C in the alloy and 70°C in the solvent. The spectroscopic characteristics of unsaturated resin BIS-GATF was determined from IR spectra, 13-NMR and 13C-NMR. Epoxyacrylate was subjected to photocuring, with the addition of IRGACURE 651, with a high-pressure mercury lamp in an oxygen-free atmosphere. The cured foil was subjected to thermal, thermo-mechanical, and mechanical investigations.
epoxyakrylate; bis(thiophenol-F)glycidyl acrylate resin; structure; kinetic parameters; curing
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Article 12EN: Synthesis of l,2,4-triazoline-5-thione derivatives
122-143

M. Pitucha, M. Wujec, M. Dobosz


Department of Organic Chemistry, Faculty of Pharmacy, Medical University, Staszica 6, 20-081 Lublin, Poland

This paper is a review of the methods used for preparation of 1,2,4--triazoline-5-thione derivatives. The initial products were thiosemicarbazide, thiosemicarbazone, amidrazones salts, aminoguanidine salts and their derivatives.
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Article 13EN: Synthesis of new derivatives of 3-(l-methylpyrrole-2-ylmethyl)-4-substituted-1,2,4-triazolin-5-thione
144-153

M. Pitucha, M. Wujec, M. Dobosz


Departament of Organic Chemistry, Faculty of Pharmacy, Medical University, Staszica 6, 20-081 Lublin, Poland

In the reaction of hydrazide of l-methylpyrrole-2-acetic acid (I) with isothiocyanates the thiosemicarbazide derivatives of l-methylpyrrole-2--acetic acid (II-IX) were obtained. Cyclization of these compounds in the presence of 2% NaOH led to formation of derivatives of l,2,4-triazolin-5--thione (X-XVII).
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Article 14EN: Electro-oxidative reactions of naphthalene and alkyl-derivatives
154-165

R. E. Sioda, B. Frankowska


Department of Analytical Chemistry and Electrochemistry, Institute of Chemistry, University ofPodlasie, 3 Maja 54, 08-110 Siedlce, Poland

Naphthalene, methyl-, ethyl-, and several dimethylnaphthalenes were electro-oxidized galvanostatically at Pt-net electrode in 1:1 v/v acetone-water solution, containing 0.1 M Na2SO4 as supporting electrolyte and 20 mM CoSO4 as mediator; the average electric charge passed was c. 7 F/mole of substrate per reaction. The products were analyzed by TLC and GC-MS, and separated by column chromatography. Alkyl-substituted quinones were the main products, apart from detected binaphthyls, hydroxy- and carboxyaldehyde derivatives. The mechanism of the oxidation is discussed, which begins with unstable radical cations formed initially at the electrode.
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Article 15EN: The electron configuration of the exocyclic nitrogen atom of allyl (5(2'-pyridyl)-[l,3,4]thiadiazol-2-yl) amine
166-177

L. Strzemecka


Department and Chair of Organic Chemistry, Department of Pharmacy, Medical University, Staszica 6, 20-081 Lublin, Poland e-mail: strzem@panaceum. am. lublin.pl

The electron configuration of the exocyclic nitrogen atom of allyl- (5-(2?--pyridyl)-[l,3,4] thiadiazol-2-yl)-amine has been determined on the basis of the 1H 13C 15N NMR spectra and B3LYP/6-31G(d, p) computations.
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Volume 58 - 2003

Article 01EN: Dynamic theory of adsorption on surfaces undergoing self-similar reconstruction
3-36

G. F. Cerofolini


ST Microelectronics, Stradale Primosole 50, 95100 Catania CT, Italy

A rate equation, which takes explicitly into account the surface reconstruction phenomena occurring (reversibly or irreversibly) while adsorption or desorption proceeds, is proposed. The equation contains a few free parameters which specify the adsorption and desorption rate constants, and the reconstruction and irreversibility degrees of the process. A complete qualitative study of the solutions of the rate equation for two kinds of reversible and self-similar reconstruction is given.
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Article 02EN: Wetting and capillary condensation in self-assembling systems
37-55

A. Ciach


Institute of Physical Chemistry and College of Science, Polish Academy of Sciences Kasprzaka 44/52, 01-224 Warsaw, Poland

Results obtained within Ciach-H0ye-Stell model of oil-water-surfactant mixtures in restricted geometry are reviewed. Special attention is paid to phase transitions in semiinfinte and in slit geometries. Similarities and differences between simple fluids and self-assembling systems are higlighted.
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Article 03EN: Aggregation behavior of nonionic lactobionylamide-type gemini surfactants: steady-state and time-resolved fluorescence studies
56-68

U. Komorek, K. A. Wilk


Institute of Organic and Polymer Technology Wrocław University of Technology Wybrzeże Wyspiańskiego 27, 50-370 Wroclaw, Poland

Nonionic gemini surfactants, N,Nv-bisalkyl-N,Nv-bis[(3-lactobionyl-amide)propyl]-a,co-diaminoalkanes, have been synthesised with a great variety of structures differing by the length of the hydrophobic alkyl chains as well as the spacer group. Steady-state fluorescence quenching (SSFQ) and time-resolved fluorescence quenching (TRFQ) methods were employed in order to describe their aggregation phenomena on the basis of obtained micellar aggregation numbers (ND) over the concentration range up to seventy-fold above the critical micelle concentration (cmc). The results suggest forming spherical micelles upon micellization and a slowly micelle growth with the surfactant concentration. The micelles formed by these structures have been also characterized in terms of the cmc and micropolarity due to the information provided by micelle-solubilized fluorescent probe.
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Article 04EN: Adsorption of asphaltenes from toluene on quartz and silica-rich soils
69-79

A. W. Marczewski, M. Szymula


Maria Curie-Skłodowska University, Faculty of Chemistry Department of Radio chemistry and Colloid Chemistry pi. M. Curie-Skłodowskiej 3, 20-031 Lublin, Poland

Adsorption of asphaltenes from tolune on quartz and silica-rich soil fractions is investigated. Such process mimics the phenomena occurring during oil spills and in natural oil reservoirs. In order to simulate natural conditions we used pentane-precipitated asphaltenes obtained from local crude oil (drills at Swidnik, near Lublin), toluene as solvent and natural Brazilian quartz as model adsorbent. The results obtained for model system are compared with asphaltene adsorption on silica-rich soil fractions from the Lublin region. The isotherm features are typical for asphaltene adsorption. Characteristic "steps" - often masked by heterogeneity of adsorbent and complex composition of natural asphaltenes - indicate changes in the state of asphaltene molecules in the solution and at the mineral surface and may be related to the asphaltene association and formation of hemimicelles and micelles.
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Article 05EN: Determination of diffusion coefficient of zinc (II) ions in polymeric membrane by absorption spectroscopy
83-93

J. Chmiel, B. Marczewska, C. Wardak


Maria Curie-Skłodowska University, Faculty of Chemistry pi M. Curie-Skłodowskiej 3, 20-031 Lublin, 20-031 Poland

The paper presents the new determination method of ions diffusion coefficients in polymer membranes. The investigations were performed in a specially constructed cell. The method is based on membrane absorbance measurement in time function. The membrane included chelating l-(2-pyridylazo)-2-naphtol (PAN) component which forms colorful complex with Zn(II) ions. On the basis of performed measurements and interpretation of second Fick' s law zinc ions diffusion coefficient in investigated membranes was calculated to be 3.28 10~8 cm /s.
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Article 06EN: Spectrophotometric determination of Zn in pharmaceutical preparations: Antioxidant and Zincuprin Forte by azo-dyes derivatives of thriazolodiazophenols
94-101

Stanistaw Zaręba 1, Arkadiusz Pomykalski 2


1 Department of Food and Nutrition, Faculty of Pharmacy, Medical University of Lublin, Staszica4, 20-016 Lublin, Poland
2 Department of Medicinal Chemistry, Faculty of Pharmacy, Medical University of Lublin, Chodzki 6, 20-093 Lublin, Poland Tel : +81 740 58 71, Fax : +81 742 51 65, E-mail: kzchl@asklepios.am.lublin.pl

To determine the miligram amounts of Zn(II) in phamaceutical multimineral (Zincuprin Forte) and multivitamin containing microelements (Antioxidant) preparations there have been used 3-(2/-hydroxynaftylazo-l0-5-mercapto-l,2,4-triazol (Metrian) and 3-(5'-mercapto-l/,2/,4/-triazolo-3/-azo)-2,6-dihydroxybenzoas acid (Matriarez-y). Durability of Zn(II) complexes expressed with lg K with pH 9.23 with Metrian is 10.311 and with Metriarez-y with pH 7.35 it is 11.224. Zinc ions of the preparations, after mineralisation (30% H2O2 with the use of condenced H2SO4 with d = 1,84 g • cm"1) were put into a soluble compound ion [Zn(NH3)4] + by adding 5 ml of 25 % of ammonia solution ,at the same time eliminating, which was achieved by filtrating, hydroxide sediments of other microelements. Spectrophotometric determination was performed in the water-methanol solution (1:1) with permanent ion power |n=0.1, pH 7.35 (Metriarez-y) and ^anaL 480 nm; pH 9.23, ^anaL 530 nm (Metrian). The outcomes were executed statistically and compared with the outcomes of AAS marking method. The main features of the proposed method are selectivity,precision and the possibility to repeat it. The outcomes of markings show lesser defect than the markings achieved with the use of AAS method.The marking method is simple and its feature is high level of sensitivness.
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Article 07EN: Synthesis of pyrimido[4,5-d]pyrimidine derivatives
105-111

J. Cieplik


Department of Organic Chemistry, Medical Academy, Grodzka 9, 50-137 Wrocław, Poland

The paper presents synthesis of pyrimido[4,5-d]pyrimidine derivatives where identical structures have been obtained by different methods
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Article 08EN: Synthesis of pyrimido[4,5-d]pyrimidinesulfon derivatives
112-117

J. Cieplik


Department of Organic Chemistry, Medical Academy, Grodzka 9, 50-137 Wroclaw, Poland

The paper presents synthesis of pyrimido[4,5-d]pyrimidine sulfonamidoderivatives using various methods to reach the final product.
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Article 09EN: The synthesis and properties of N-substituted amides of l-(5-methylthio-l,2,4-triazol-3-yl)-cyclohexane-2-carboxylic acid
118-125

K. Galewicz-Walesa, A. Pachuta-Stec


Medical Academy in Lublin, Staszica 6, 20-081 Lublin

The synthesis of S-methyl-N1-(cyclohexane-l,2-dicarbonyl)-isothiosemi-carbazide and its reactions with primary aliphatic and aromatic amines were performed. The direction and conditions of these reactions were examined.
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Article 10EN: Synthesis of new derivatives of 1-hydroxymethyl and l-methoxymethyl-dibenzo[e.h]bicyclo[2.2.2]-octane-2,3-dicarboximide with an expected (3-adrenolytic activity
126-134

J. Kossakowski, M. Jarocka-Wierzba


Department of Medical Chemistry, Medical University of Warsaw, Oczki 3, 02-007 Warsaw, Poland

This paper presents the preparation of a number of new derivatives of 1-hydroxymethyl-dibenzo[e.h]bicyclo[2.2.2]-octane-2,3-dicarboximide and l-methoxymethyldibenzo[e.h]-bicyclo [2.2.2]-octane-2,3-dicarboximide with an expected p-adrenolytic activity.
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Article 11EN: Synthesis of new N-substituted cyclic imides with an expected anxiolytic activity. XXVIL Derivatives of l-chloromethyl-dibenzo[e.h]bicyclo [2.2.2] octane-2,3-dicarboximide
135-146

J. Kossakowski, M. Perlinski


Department of Medical Chemistry, Medical University of Warsaw, Oczki 3, 02-007 Warsaw, Poland

This paper presents the preparation of a number of new derivatives of l-chloromethyl-dibenzo[e.h]bicyclo[2.2.2]-octane-2,3-dicarboximide with an expected anxiolytic activity.
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Article 12EN: Synthesis of new N-substituted cyclic imides with an expected anxiolytic activity.xxvi.derivatives of N-hydroxy-7-diphenylmethylenebicyclo [2.2.1 ]hept- -2-ene-5,6-dicarboximide
147-153

J. Kossakowski, A. Prędka


Department of Medical Chemistry, Medical University of Warsaw, Oczki 3, 02-007 Warsaw, Poland

This paper presents the methods used for preparation of new N-substituted derivatives of N-hydroksy-7- diphenylmethylenebicyclo[2.2.1]hept-2-ene-5,6-dicarboximide. The starting material was N-hydroxy-7-diphenyl-methylenebicyclo[2.2.1]hept-2-ene-5,6-dicarboximide
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Article 13EN: Synthesis of 3-R-4-substituted-A2-l,2,4-triazoline-5-thione
154-163

M. Wujec, M. Dobosz


Zaklad Chemii Organicznej, Wydzial Farmacji, Akademia Medyczna, Staszica 6, 20-081 Lublin, wujec@panaceum.am.lublin.pl

In the reaction of hydroiodide of methyl ester of S-methylthiosemi-carbazide with secondary amines hydroiodides of 2-amino-l-substitute-dguanidine were obtained (1). These compounds were then converted to respective 3-R-4-substituted A2-l,2,4-triazoline-5-thione and (2) in the reactions with isothiocyanates.
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Volume 57 - 2002

Article 01EN: The real space renormalization group and lattice gas model
3-45

A. Tarasenko, L. Jastrabik


Institute of Physics, Academy of Sciences of the Czech Republic, Na Slovance 2, 182 21, Prague 8, Czech Republic

The article presents a brief survey of application of the real space renormalization group to investigation of the thermodynamic properties of Ising-like and lattice-gas two dimensional systems. A number of RSRG transformations for a square lattice and their properties have been compiled together. It is shown that the precision of the RSRG method strongly depends not only on the size of the blocks used in the RSRG transformations, but also on its symmetry and composition. In general, the accuracy of the RSRG method increases with the number of sites in the block. But the most accurate results have been obtained for blocks of average sizes having all symmetry elements and optimal composition. We present results of the RSRG calculations of many thermodynamic quantities: phase diagrams, adsorption isotherms, spontaneous magnetization, coverage dependencies of the pair correlation function for the nearest neighbor particles, the isothermal susceptibility, tracer, jump and chemical diffusion coefficients. The RSRG data are compared with the well-known exact expressions and results obtained by Monte Carlo simulations. The coincidence between the exact, numerical and RSRG data is surprisingly good.
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Article 02EN: Characterising porous carbonaceous materials using the new methods. An attempt for estimation of micropore size distribution function from adsorption isotherm of nitrogen and benzene
46-74

P. Kowalczyk 1, P. A. Gauden 2, A. P. Terzyk 2, D. D. Do 3, G. Rychlicki 2


1 Military Institute of Chemistry and Radiometry, Department of Respiratory Protection, Al. Gen. Chrusciela 105, 00-910 Warszawa, Poland
1 N. Copernicus University, Department of Chemistry, Physicochemistry of Carbon Materials Research Group, ul. Gagarina 7, 87-100 Torun, Poland
1 Department of Chemical Engineering, University of Queensland, St. Lucia, Qld4072, Australia

The study presents the analysis of adsorption data of nitrogen and benzene adsorption onto four microporous carbons. The most advanced methods of porosity characterisation, namely: the method of Do and co-workers (called Do), DFT, CONTIN, HK, and the methods basing on Dubinin's potential theory of adsorption are put to use. It is shown, that the similarity between obtained results depends on the dispersion of microporosity of carbonaceous material, and if this dispersion is relatively high, all methods lead to very similar pore size distribution curves.
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Article 03EN: Description of the structural and energetic heterogeneities of solid surfaces in terms of fractal geometry. A comparative analysis of the methods of estimation of fractal dimension from a single gas adsorption isotherm and some suggestions for the future research
75-100

A. P. Terzyk 1, P. Kowalczyk 2, A. Gauden 1


1 N. Copernicus University, Department of Chemistry, Physicochemistry of Carbon, Materials Research Group ul Gagarina 7, 87-100 Torun, Poland
2 Military Institute of Chemistry and Radiometry, Department of Respiratory Protection, Al. Gen. Chrusciela 105, 00-910 Waszawa, Poland

Different methods of the calculation of fractal dimension (D) of adsorbents are shortly reviewed. Freshly projected algorithms are applied to calculate D for two systems previously studied by Ehrburger-Dolle, and Rudzinski et al., and the results are compared. Further a modification of the recently derived fractal analogue of the Dubinin - Astakhov adsorption isotherm equation is proposed to take into account the effect of multilayer adsorption. Numerical analysis of obtained "hybrid" isotherms is presented for some arbitrarily chosen parameters.
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Article 04EN: Time separation of surface heterogeneity through experimental measurement of adsorption energies, local monolayer capacities, local isotherms, and energy distribution functions by inverse gas chromatography
101-118

N. A. Katsanos 1, F. Roubani-Kalantzopoulou 2


1 Physical Chemistry Laboratory, University ofPatras, 26504 Patras, Greece
2 Department of Chemical Engineering, National Technical University, 15780 Zografou, Greece

The inverse gas chromatography version of Reversed-Flow is described for experimental determination of local adsorption energies, local monolayer capacities, local isotherms, energy distribution functions, and lateral molecular interactions of gaseous adsorbates on heterogeneous solid surfaces. This method circumvents altogether the traditional integral equation of the three functions ®(p, 7), 6(p, T, s) andX^) used in various approximations for finding energy distribution functions. Based on some explicit functions of time derived from the solution of a simple mathematical model, all physicochemical quantities mentioned above can be determined as functions of experimental time by means of simple PC programmes. This creates a domain of time-resolved chemistry of surfaces, used to reach important conclusions regarding adsorption sites. Some representative results are explicitly given.
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Article 05EN: The methods of preparation and modification of surface properties of synthetic carbon adsorbents
119-139

A. Gierak, M. Seredych


Maria Curie-Sklodowska University, Faculty of Chemistry pi M.Curie-Sklodowskiej 3, 20-031 Lublin, Poland e-mail: gierak@hermes. umcs. lublin.pl European Collegia! Polish and Ukrainian University, Lublin

ur concern in this paper is to review the methods of preparation and modification the surface properties of synthetic carbon adsorbents, obtained by carbonization different porous organic polymers. The first section are devoted to the methods of carbonization polymers, application catalysts and the influence of some important factors such as carbonization temperature, heating rate and soak time of salt solutions on the resulting char properties In our paper we pay special attention to application this carbon adsorbents to trace analysis of organic pollutants in environmental samples. The physico-chemical properties of synthetic carbon adsorbents are superior compared to those of the "traditional" active carbon materials.
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Article 06EN: Characterization of surface properties of carbon black and graphite
140-157

M. Gotzinger, C. Mehler, W. Peukert


Institute of Particle Technology, Technische Universitdt Munchen Boltzmannstr. 15, 85748 Garching, Germany

Carbon black is used in several technical applications. Fillers in tires, black pigments in printing technology or synthetic cloth fibers are only a few examples. Because of the small particle size of carbon blacks, the surface properties have a great influence on the product property. We studied two different carbon black that show a large difference up to 20% in rolling drag when used as filler in tires. Different roughness or diverse polar groups on the surfaces are possible reasons for this. Morphology, surface structure and chemical surface composition of carbon black are not well defined. For such systems, TGA-MS and gas adsorption are powerful tools to analyze surface properties. We use adsorption equilibria in the Henry-region that reflect the interaction of molecules with the particle surfaces. From measured Henry-coefficients and known atomic surface structure, dispersive interaction parameters of the solid, e.g. a Hamaker-constant, can be determined by inversely solving the applied adsorption model. This method can be used to characterize carbon black if the interactions of different molecules with carbon atoms are calibrated on a defined surface like graphite. From known interaction potentials of various probe molecules, structural information like surface roughness of carbon black can be determined.
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Article 07EN: Packing transitions of Lennard Jones fluids in carbon slit pores
159-177

T.x. Nguyen, S.k. Bhatia, D. Nicholson


Department of Chemical Engineering The University of Queensland Brisbane, Qld. 4072, Australia

In this article we apply a recently developed density functional theory approach to the prediction of the temperature dependent variation in capacity with pore size of methane and carbon tetraflouride, and the associated packing transitions. The latter is an important compound as a member of the halocarbon family that are established greenhouse gas contributors. The capacities predicted by the proposed model are in good agreement with those obtained from grand canonical Monte Carlo simulation. Pair distributions reveal characteristic features that correspond to the sequence of buckling and rhombic transitions that occur as the slit pore width is increased.
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Article 08EN: Synthesis and characterization of modified methacrylate polymeric packing based on bisphenol-s for chromatography
178-193

T. Jabloriska-Pikus 1, W. Majewski 1, W. Charmas 1, B. Gawdzik 1, F. Villieras 2


1 Maria Curie-Sklodowska University, Faculty of Chemistry, Department of Organic Chemistry pi M. Curie-Sklodowskiej 3, 20-031 Lublin, Poland
2 LEM, UMR 7569 CNRS-INPL, Ecole Nat. Sup. Geologic 15 avenue du Charmois, PB 40, Vandoeuvre les Nancy, 54501 France

Synthesis and properties of modified porous polymeric packings for high performance liquid chromatography (HPLC) are presented. As modifiers of the OH groups present in the polymeric matrix, Ti-donor (2-naphthoic acid chloride), Ti-acceptor (3,5-dinitrobenzoic acid chloride), and cyclo-hexyl isocyanate which indicates any polar interactions, are used. Chemical structure of these packings are confirmed by elemental analysis, FTIR and rentgenography. Additionally, porous structure, thermal resistance, and swelling propensities of polymers are presented.
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Article 09EN: From metal ions, organic molecules and their complexes to nanostructures in amorphous and vitreous matrices
194-214

A. M. Klonkowski


Department of Chemical Technology,Faculty of Chemistry, University of Gdansk ul Sobieskiego 18, 80-952 Gdansk, Poland e-mail: aklonk@chemik chem. univ.gda.pl

This review attempts to present some aspects of glasses and other amorphous materials such as xerogels both from the fundamental and applied viewpoints. Are given three examples of how doped xerogel materials prepared by sol-gel method are emerging as an important means of producing new materials. Moreover, there is present brief description of nanostructural materials. The first part of this review is devoted to general characteristics of glasses, gels and nanostructures. The second part contains description of such functional materials as oxide glasses, catalyst precursors, chemical recognition phases and luminescent materials. Thus, firstly oxide glasses are classified by the proximity to the onset of metallization and simultaneously discribed by their ionic-covalent bond. Secondly, ligand protected metal nanoclusters as immobilized catalysts in oxide xerogels are the point of interest. This type of heterogeneous catalysts are much less investigated than the bare metal particles on supports. The main interest is focused on the function of the ligands. Then, silica xerogel samples with entrapped series of three fluorescent chemosensors of the Ant-R-Ant type, where Ant is an anthryl group and R is a receptor (spacer) with donor atoms, were prepared as chemical recognition phases. The recognition phase with fluorosensor of the type Ant-N-O-O-N-Ant, where N and O are donor atoms, can be regenerated many times and seems to be most promising system for the fluorescent chemical sensor. Finally, luminescent materials which are based on the antenna effect and are composed of Eu(III) complex (luminescence centre) entrapped in xerogel matrix. In this case results of the experiments concerning the coordination sphere composition show that a cryptand ligand with aromatic groups and an aromatic co-ligand, settle efficient action the antenna effect and isolate the central ion from each efficient quenchers, as e.g. water molecules. In this section is presented influence of nanoparticles of semiconductors of the II-VI type on luminescence properties.
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Article 10EN: Studies of the mechanism of polyethylene oxide (PEO) adsorption on the surface of A12O3 in the presence of sodium dodecylsulfate (SDS) S. Chibowski and M. Paszkiewicz
215-225

S. Chibowski, M. Paszkiewicz


Maria Curie-SModowska University, Faculty of Chemistry Department of Radiochemistry and Colloid Chemistry pi M. Curie-Sklodowskiej 3, 20-031 Lublin, 031 Poland, fax: +48 (81) 533-28-11; e-mail: schibows@hermes.umcs.lublin.pl

An influence of polyethylene oxide (PEO) with sodium dodecylsulfate (SDS) interaction on the adsorption behavior of the polymer at Al2O3/solution interface was examined. Observed increase of the PEO adsorption in the presence of SDS resulted from a polymer-surfactant complex formation. The presence of the surfactant influences also on the structure of the adsorbed polymer layers. This effect was proved by viscometry measurements that allow calculate thickness of the adsorbed layer of the polymer on the surface of AI2O3 in the presence and the absence of SDS.
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Article 11EN: Electrical interfacial layer at solid/liquid interface*
226-248

N. Kallay, A. Cop, D. Kovacevic, K. Majorinc, T. Preocanin, S. Zalac


Laboratory of Physical Chemistry, Department of Chemistry, Faculty of Science, University of Zagreb, Marulicev trg 19, P.O. BOX 163, 10 001 Zagreb, Croatia

Some problems related to the theoretical concepts applied in studying interfacial equilibria at solid/liquid interfaces are discussed. It was shown that assumptions related to the mechanism of surface reactions and the structure of interfacial layer need to be reconsidered. The commonly used 3-layer models were considered as simplification of the general 4-layer model. The concept of the capacitors of constant capacitances was discussed. The equilibrium at the electrical interfacial layer was used to discuss the colloid stability phenomenon. The Schulze-Hardy rule, i.e. the effect of the lyotropic series was explained on the basis of equilibrium constants of counterion association with charged surface groups. It was concluded that new experimental methods are necessary for further progress in this area. The second route is to apply all existing experimental methods to one sample and to interpret the data simultaneously.
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Article 12EN: The electrokinetic potentials of oxides in mixed water-1-propanol solvent
249-258

M. Kosmulski 1, J. B. Rosenholm 2


1 Department of Electrochemistry, Technical University of Lublin, ul Nadbystrzycka 38A, 20-618 Lublin, Poland
2 Department of Physical Chemistry, Abo Akademi University, Porthansgatan 3-5, 20500 Turku, Finland

The effect of the solvent (water versus mixed solvent 70% water + 30% 1-propanol, mass fraction) on the electrokinetic potential of oxides was studied at NaNO3 concentrations of 0.1 and 0.01 mol dm"3. Only with anatase and indium oxide the IEP was shifted to high pH in the mixed solvent at high ionic strength. The IEP of rutile, and of niobium and tantalum oxides was rather insensitive to the solvent composition. The negative £ potentials of all oxides were depressed in the presence of 1-propanol, but for silica and tantalum oxide, this effect was substantial only at NaNO3 concentration of 0.1 mol dm"3. The positive branch of electrokinetic curves was less sensitive to the admixture of 1-propanol.
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Article 13EN: Agglomerate flotation of fine MgO and ZnO particles at the presence of polymer and surfactant
259-270

Z. Sadowski


Department of Chemical Engineering and Heating Equipment Wroclaw University of Technology Wybrzeze Wyspianskiego 27, 50-370 Wroclaw, Poland Sadowski@iic.pwr. wroc.pl

The paper presents the experimental data with using both flocculants and surfactants for flotation and aggregation of fine particles. The work has been performed with two oxides ZnO and MgO. The conventional flotation collectors such as sodium oleate, sodium dodecyl sulphate and cetyltrimethylammonium bromide were used. The surfactant adsorbed layers were characterized by both the surfactant adsorption data and zeta potential measurements. The sedimentation experiments showed that the addition of anionic surfactant and cationic flocculant induces strong flocculation as a result of electrostatic interaction. The hydrophobic floes and satisfied flotation conditions were created by addition of sodium dodecyl sulphate and nonionic flocculants
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Article 14EN: Antioxidants activity in oil-in-water microemulsion stabilized by anionic surfactant
271-280

M. Szymula


Maria Curie-Sklodowska University, Faculty of Chemistry Department of Radiochemistry and Colloid Chemistry pi M. Curie-Sklodowskiej 3, 20-031 Lublin, Poland fax: (48) 81 53 32 811, e-mail: szymu@hermes.umcs.lublin.pl

Investigations of oxidation kinetics of some antioxidants like: vitamin C, propyl gallate, vitamin E and P-carotene solubilized in the O/W microemulsion formed by SDS, pentanol and water were carried out. The present results as well as the literature data allow to compare the resistance to oxidation of antioxidants acting separately and together with vitamin C. Vitamin C (water-soluble species) turned out to be the best of them, contrary to the C (totally non-polar, fat-soluble species), which appeared to be the poorest one. When observing vitamin C, occurring in O/W microemulsion together with vitamin E and P-carotene, we discovered stimulating (not protective) action of vitamin C towards vitamin E oxidation. Vitamin C does not influence the p-carotene behaviour; in the absence and presence of vitamin C its action is similar.
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Article 15EN: FT-IR/PAS applications in surface science and catalysis 1
281-316

J. Ryczkowski, S. Pasieczna


Maria Curie-Sklodowska University, Faculty of Chemistry, Department of Chemical Technology pi M. Curie-Sklodowskiej 3, 20-031 Lublin, Poland tel +48-81 537-55-96; fax: +48-81 537-55-65; e-mail: ryczkows@hermes. umcs. lublin.pl

Our concern in this paper is to present basis and the selected examples of the modern spectroscopic technique - FT-IR/PAS (Fourier transform infrared photoacoustic spectroscopy) applications in the surface science and catalytical investigations. Vibrational spectroscopies are among most widely used methods for the surface characterization. This is because very detailed structural information can be obtained from vibrational spectra. FT-IR/PAS is one of the basic spectroscopic techniques belonging to the conventional optical spectroscopy, and it is an important complimentary method to the other spectroscopic methods applied.
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Article 16EN: Effect of diaminotoluene isomers on Zn(II) ions electroreduction in the perchlorate solutions at varied water activities
319-331

G. Dalmata, J. Saba, J. Szaran


Maria Curie-SModowska University, Faculty of Chemistry Department of Analytical Chemistry and Instrumental Analysis pi M. Curie-Sklodowskiej 3, 20-031 Lublin, Poland

The reduction of Zn(II) ions in the presence of the diaminotoluene isomers has been studied in the perchlorate solutions at varied water activity. The hydration number of the Zn(II) ions in the solutions was obtained from the shift of Ey2 r with water activity. The results obtained allow to isolate the following stages in the mechanism of catalytic action of the diaminotoluene isomers on the Zn(II) ions electroreduction in sodium perchlorate: - fast dehydration of Zn(II) ions and formation of the active complex Zn(II) - diaminotoluene, - slow transfer of the first electron, - fast loss of the remaining water molecules and formation of the active complex Zn(I) - diaminotoluene, - slow transfer of the second electron.
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Article 17EN: Water-soluble porphyrins and their metal complexes
332-363

M. Makarska, S. Radzki


Maria Curie-Sklodowska University, Department of Inorganic Chemistry, pi. M. Curie-SModowskiej 2, 20-031 Lublin, Poland e-mail: madzia@hermes. umcs. lublin.pl

Nowadays the chemistry of porphyrins and related compounds are one of the most interesting and promising subjects of supramolecular chemistry, because of their unique photoactive properties and the ability to electron transfer. The possibility of synthesis of porphyrin complexes with almost all metal ions and easy to modify the molecular structure of such obtained compounds give a chance of using the porphyrins in many different areas of life. In this paper we present the most significant problems concerning water-soluble porphyrins and their metal complexes, such as the molecular structures, different manners of synthesis, physicochemical properties, as well as the origin and classification of porphyrins and metalloporphyrins UV-VIS spectra. We also show the most interesting applications, including the role of porphyrins as molecular conductors and photosensitizers in photolysis of water and in photodynamic therapy of cancer (PDT).
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Article 18EN: Synthesis, structure and properties of 2-(acenaphthen-5-yl)--3-methylbutanoic acid and its derivatives
367-376

W. Kowalewska, W. Podkoscielny


Department of Organic Chemisty and Technology, Maria Curie-Sklodowska University, ul Gliniana33, 20-614 Lublin, Poland

Synthesis, structure and fundamental chemical and physical properties as well as biological activity of 2-(acenaphthen-5-yl)-3-methylbutanoic acid and its some derivatives were described. The chemical structure of the newly obtained compounds was confirmed by elementary analysis and FTIR and ^-NMR spectroscopies. 2-(Acenaphthen-5-yl)-3-methylbuta-noic acid and its amide and ester derivatives were investigated at the Institute of Organic Chemistry in Warsaw in view their biological activity. It was found that the high fungicidal activity characterized the acid chloride and amide of 2-(acenaphthen-5-yl)-3-methylbutanoic acid.
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Article 19EN: Reactions of terpene tosylates with sodium ethyl carbonate
377-383

Z. Rykowski, E. Drozd-Szczygieł


The Chair of Organic Chemistry, Medical Academy, pl. Nankiera 1, Wroclaw, Poland

For a long time [1] terpene compounds have been arousing a continuously growing interest of chemists, pharmacologists and pharmacists. This interest was only enhanced by their prevalence and frequent ample occurrence in easily accessible vegetable material. They are widely applied mainly in perfume, cosmetic food and pharmaceutic industries. Chemical reactivity research of these combinations has contributed to theoretical knowledge and what is more important it facilitated the exploration of a number of stereochemistry principles. P-toluenosulfonyl acid terpene alcohols esters, called tosylates, were of particular interest among terpenes derivatives. From the theoretical point of view they constitute an interesting group of combinations. Terpene tosylates reduced with lithium-aluminium hydride, unlike other esters which produce alcohols, afford hydrocarbons [2]. While reduced with lithium in ethyl amine [3] terpenes tosylates afford to obtain free alcohols both in the case of mono- and polyhydroxide alcohols. Unlike other esters, terpene tosylates are not hydrolysed under the influence of alkalies. Strong bases in non-aqueous solutions result in eliminations. This is an easy way to obtain unsaturated hydrocarbons [4] with good efficiency. Polyhydroxide alcohol tosylates depending on their structure may form aldehydes [5], ketones [6] or epoxides [7]. The introduction of aprotic solvents terpenes to chemistry created new opportunities. In these conditions monohydroxide alcohols tosylates easily reacted in nucleophilic substitution producing azides or nitriles [8] with good effectiveness. The latter form useful substrates for the synthesis of new derivatives.
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