Band 65, Heft 1

In this work, application of polyaniline coated onto wood sawdust (PAni/SD) for the removal of methyl orange (MO) as a typical azo dye from aqueous solutions is introduced. The effects of some important parameters such as pH, initial concentration, sorbent dosage, and contact time on the uptake of MO solution were also investigated. In order to get a better comparison, adsorption experiments were also carried out using commercial grade of granulated activated carbon (GAC) and sawdust without coating (SD) at the same time. It was found that PAni/SD can be used to remove azo dyes such as MO from aqueous solutions very efficiently. Experimental data were analyzed by the Langmuir and Freundlich models of adsorption. Kinetic parameters for the adsorption of MO dyes for the selected adsorbents are also reported. In order to study the possibility of desorption for frequent application, chemical regeneration of the used adsorbents was also investigated. Desorption or recovery of dye and regeneration of adsorbent (PAni/SD) was found to be quite possible and of high performance. Application of modified sawdust with polyaniline for the removal of azo dye is very promising for textile wastewater treatment.

Terpene esters of fatty acids have potential applications in food, cosmetic, and pharmaceutical industries. The present study focuses on the synthesis of terpene esters of long chain fatty acids catalyzed by Candida antarctica lipase B. Different parameters like temperature, solvent, and enzyme concentration for the esterification of terpene alcohols (geraniol and citronellol) with oleic acid were studied. Maximum conversion (98 %) was found for both terpene esters at 60°C in 2,2,4-trimethylpentane as well as in dry hexane and around 95–97 % in other tested solvents. The reaction was also carried out using stearic and linoleic acid in hexane to study the effects of unsaturation in the substrate in which stearic acid showed the maximum conversion. The reaction was monitored by 1H nuclear magnetic resonance spectroscopy. Using the peak integration values of methylene protons of terpene and terpene ester of δ = 3.6 and 4.0 for citronellol and δ = 4.2 and 4.6 for geraniol, respectively, percentage conversions of each of the esters were calculated.

Carboxymethyl cellulose (CMC) has been used widely to enhance dry strength of paper and uniformity of sheet in the papermaking industry. Besides these positive effects, it may affect the fines retention and dewatering processes negatively. These negative effects are mainly seen when fiber modifications with high CMC dosages are studied in laboratory scale. In this paper, the effect of fiber modification with CMC on the deposition of precipitated calcium carbonate (PCC) and on the dewatering process in the presence of cationic polyacrylamide (CPAM)/bentonite microparticle flocculation system is examined. It was determined that fiber modification with 10 mg g−1 of CMC decreased PCC deposition at the initial addition of CPAM and gave better PCC deposition at 2 mg g−1 of CPAM. It was also observed that PCC deposition on unmodified fibers is higher at lower CPAM concentration. PCC deposition was found as almost stable after a maximum value obtained at 0.5 mg g−1 of bentonite concentration for fiber modified with 40 mg g−1 of CMC. This indicates that interaction between CPAM and bentonite particles changed due to higher surface charge and CMC conformation on fibers. Results of the dewatering experiments showed that CMC modification increased the drainage time due to a denser and more plugged sheet. This negative effect was compensated with higher concentrations of CPAM and bentonite. On the other hand, dewatering is also affected by the mass ratio of CMC and CPAM, which was not the optimum one in this study at lower of CPAM. Thus, the increase in the drainage time in the presence of CMC on the fiber surface could be also caused by incorrect ratios of chemicals because the effect of CMC on the drainage time was not observed at higher concentrations of CPAM.

A new complex, [Cu2(μ 2-Cl)2(IP)2Cl2] · 4H2O (IP = imidazo[4,5-f]1,10-phenathroline), was synthesised and characterised by elemental analysis, thermal analysis, IR spectra, and X-ray crystallography. The results showed that the complex crystallises in the monoclinic space group P $$ \bar 1 $$; a = 7.880 (2) Å, b = 9.227(2) Å, c = 10.694(2) Å; α = 97.788(4)°, β = 100.637(4)°, γ = 95.841(3)°; V = 750.7(3) Å3, and Z = 1. The complex is further stabilised by H-bonds and a π-π stacking interaction between the pyridine and benzene rings of two neighbouring molecules with the centroid.centroid distance of 3.498(3) Å, leading to a 3D supramolecular architecture. Thermal decomposition procedure of the complex explored by TG-DTG has three stages, and the final product is Cu in residual rate of 16.18 % (calculated to be 16.26 %).

Non-aggregated spherical polystyrene (PS) particles were coated with GdPO4:Tb3+/Ce3+ phosphor layers by a conventional hydrothermal synthesis using poly(vinylpyrrolidone) (PVP) as an additive without further annealing treatment. X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), photoluminescence (PL), as well as luminescence decay experiments were used to characterise the resulting core-shell structured PS@GdPO4:Tb3+/Ce3+ samples. The results of XRD indicated that the PS particles were successfully coated with the GdPO4:Tb3+/Ce3+ phosphor layers, which could be further verified by the images of FESEM. Under ultraviolet excitation, the PS@GdPO4:Tb3+/Ce3+ phosphors show Tb3+ characteristic emission, i.e. 5D4-7FJ (J = {6, 5, 4, 3}) emission lines with green emission 5D4-7F5 (543 nm) as the most prominent group. The core-shell phosphors so obtained have potential applications in field emission display (FED) and plasma display panels (PDP).

We report on an optical characterisation of nanocrystalline diamond films photochemically functionalised with the organosilane-coupling agent, N 1-(3-(trimethoxysilyl)propyl)hexane-1,6-diamine (alternative names: N-(6-aminohexyl)aminopropyl-trimethoxysilane, (3-(6-aminohexylamino)propyl) trimetoxysilane, AHAPS). The presence and homogeneity of the organosilane layers were detected by fluorescence microscopy and infrared reflectance-absorbance spectroscopy. The results indicated that a homogeneous surface coverage with organosilane layers was achieved on diamond surfaces which were modified either by hydrogen or by oxygen plasma treatment. The functionalised nanocrystalline diamonds present a promising solution in future biosensor applications.

The Knoevenagel condensation between aldehydes and substrates with active methylene groups was applied to synthesise a series of 3-(4-substituted phenyl)-2-arylacrylonitriles (aryl = phenyl or pyridyl). Chloro-, fluoro-, or dimethylamino-substituted aryls and a cyano group attached to the double bond of acrylonitrile were studied. Previous studies showed that the condensation products were E isomers. The compounds synthesised were: 3-(4-chlorophenyl)-2-phenylacrylonitrile, 3-(4-chlorophenyl)-2-(pyridin-2-yl)acrylonitrile, 3-(4-chlorophenyl)-2-(pyridin-3-yl)acrylonitrile, 3-(4-chlorophenyl)-2-(pyridin-4-yl)acrylonitrile, 3-(4-fluorophenyl)-2-phenylacrylonitrile, 3-(4-fluorophenyl)-2-(pyridin-2-yl)acrylonitrile, 3-(4-fluorophenyl)-2-(pyridin-3-yl)acrylonitrile, 3-(4-fluorophenyl)-2-(pyridin-4-yl)acrylonitrile, 3-(4-dimethylaminophenyl)-2-phenylacrylonitrile, 3-(4-dimethylaminophenyl)-2-(pyridin-2-yl)acrylonitrile, 3-(4-dimethylaminophenyl)-2-(pyridin-3-yl)acrylonitrile, and 3-(4-dimethylaminophenyl)-2-(pyridin-4-yl)acrylonitrile. Structures were confirmed by IR, MS, and NMR spectral data. Molar absorption coefficient, absorbance, and fluorescence emission spectra were compared in order to evaluate the effects of substituents on phenyl and the position of nitrogen in pyridine moiety on the electronic properties of acrylonitrile derivatives prepared.

As a part of our systematic study of antimycobacterially active derivatives of salicylamides, a series of nineteen derivatives of N-(2-pyridylmethyl)salicylamides and N-(3-pyridylmethyl)salicylamides was synthesised. The compounds exhibited in vitro activity against Mycobacterium tuberculosis and M. avium. Their lipophilicity, R M, was measured by thin layer chromatography on silica gel impregnated with trioctadecylsilane and the logarithm of the partition coefficient (octanol-water), logP, was calculated. Both the parameters of lipophilicity correlated. The quantitative relationship between the structure and antimycobacterial activity was calculated. Antimycobacterial activity increased with an increase in lipophilicity. The N-(2-pyridylmethyl)salicylamide derivatives were more active than the derivatives of isomeric N-(3-pyridylmethyl)salicylamides. The geometry of compounds was calculated and the calculation was verified by measuring the length of the hydrogen bond between hydroxyl and carbonyl groups on the salicylic moiety.

New acylthiourea derivatives, 2-((4-ethylphenoxy)methyl)-N-(phenylcarbamothioyl)benzamides, were tested by qualitative and quantitative methods on various bacterial and fungal strains and proved to be active at low concentrations against Gram-positive and Gram-negative bacteria as well as fungi. These compounds were prepared by the reaction of 2-((4-ethylphenoxy)methyl)benzoyl isothiocyanate with various primary aromatic amines, and were characterised by melting point and solubility. The structures were identified by elemental analysis, 1H and 13C NMR, and IR spectral data. The level of antimicrobial activity of the new 2-((4-ethylphenoxy)methyl)benzoylthiourea derivatives was dependent on the type, number and position of the substituent on the phenyl group attached to thiourea nitrogen. The iodine and nitro substituents favoured the antimicrobial activity against the Gram-negative bacterial strains, while the highest inhibitory effect against Gram-positive and fungal strains was exhibited by compounds with electron-donating substituents such as the methyl and ethyl groups.

Lamotrigine (LTG) is an antiepileptic drug used for the prevention of convulsions. Except several known side effects, hepatic dysfunction is also reported. Hepatotoxic side effects occur due to the dichlorophenyl moiety which develops an abnormally low level of glutathione. Depletion of glutathione causes oxidative stress and hepatic cell damage. The goal of the present study was to test the action and side effects of the three compounds synthesised and compared to LTG. Three amide prodrugs of LTG were synthesised by its reaction with N-acetylamino acids, viz, glycine, glutamic acid, and methionine. Purified synthesised prodrugs were subjected to thin layer chromatography, melting point, solubility and partition coefficients determination and characterised by UV, FTIR, 1H and 13C NMR spectroscopy. The synthesised prodrugs were subjected to in vitro hydrolysis and to anticonvulsant and hepatotoxic activity studies. Significant reduction in hepatotoxicity and comparable anticonvulsant activities were obtained in all synthesised prodrugs as compared to LTG.

Adsorption of cetyltrimethylammonium bromide (CTAB) onto bituminous coal (BC) and a clay mineral, montmorillonite (MMT), was studied. Simultaneous measurements of the CTAB adsorption and zeta potential determination of the adsorption suspensions were carried out. The adsorption isotherms were found to be of the typical Langmuir type; values of the CTAB adsorption capacities were calculated (a m = 0.65 mmol g−1 for coal and a m = 3.24 mmol g−1 for MMT). The shape of the adsorption isotherms was correlated with zeta potential values at the adsorption equilibrium. The adsorption properties of both sorbents were studied by voltammetry on carbon paste electrodes (CPE) modified with coal-CTAB and MMT-CTAB system, respectively. Open circuit sorption with differential pulse voltammetry was performed in order to compare the sorption properties of the systems with the unmodified sorbents. The Cu2+ adsorption on BC and MMT decreased to approximately 50 % and 40 %, respectively. The surface adsorption mechanism of CTAB on coal based on hydrophilic interactions was proposed. In the case of montmorillonite, the CTAB intercalation is expected via ion exchange into the inter-layer space forming a double- or triple-layer arrangement.

The densities of two systems of molten mixtures (NaF/AlF3)—NaVO3 and (NaF/AlF3)—AlPO4 were measured using an Archimedean method. Each molten mixture contained varying amounts of “impurity” constituents. The measurements were performed at various NaF/AlF3 mole ratios (CR, cryolite ratio), equal to 3, 2.5, 2, and 1.5.

In this paper, examination of the aerial parts of seven Senecio species from Serbia and Montenegro is reported. Phytochemical investigation of Senecio erucifolius led to the isolation and characterization of semiquinol butyl 2-(1-hydroxy-4-oxocyclohexa-2,5-dienyl)acetate (I), along with methyl 2-(1-hydroxy-4-oxocyclohexa-2,5-dienyl)acetate (jacaranone, II), and methyl 2-(4-hidroxyphenyl)acetate (III). The structure of I was established based on spectroscopic studies (1H- and 13C-NMR, IR, and CI-MS). Compound II was also isolated from S. carpathicus and S. subalpinus. The presence of jacaranone in the methanol extracts of S. wagneri, S. othonnae, and S. paludosus was confirmed by LC/ESI-TOF MS.

Areas of fusion and crystallization peaks of K3NbO2F4 were measured using the DCS mode of a high-temperature calorimeter (SETARAM 1800 K). On the basis of these quantities, considering the temperature dependence of the calorimeter sensitivity, the value of the fusion enthalpy of K3NbO2F4 of (98 ± 6) kJ mol−1 was determined at the fusion temperature of 1257 K.