Combining Coagulation and Electrocoagulation with UVA-LED Photo-Fenton to Improve the Efficiency and Reduce the Cost of Mature Landfill Leachate Treatment

This study focused on the reduction of the treatment cost of mature landfill leachate (LL) by enhancing the coagulation pre-treatment before a UVA-LED photo-Fenton process. A more efficient advanced coagulation pretreatment was designed by combining conventional coagulation (CC) and electro-coagulation (EC). Regardless of the order in which the two coagulations were applied, the combination achieved more than 73% color removal, 80% COD removal, and 27% SUVA removal. However, the coagulation order had a great influence on both final pH and total dissolved iron, which were key parameters for the UVA-LED photo-Fenton post-treatment. CC (pH = 5; 2 g L⁻¹ of FeCl₃6H₂O) followed by EC (pH = 5; 10 mA cm⁻²) resulted in a pH of 6.4 and 100 mg L⁻¹ of dissolved iron, whereas EC (pH = 4; 10 mA cm⁻²) followed by CC (pH = 6; 1 g L⁻¹ FeCl₃6H₂O) led to a final pH of 3.4 and 210 mg L⁻¹ dissolved iron. This last combination was therefore considered better for the posterior photo-Fenton treatment. Results at the best cost-efficient [H₂O₂]:COD ratio of 1.063 showed a high treatment efficiency, namely the removal of 99% of the color, 89% of the COD, and 60% of the SUVA. Conductivity was reduced by 17%, and biodegradability increased to BOD₅:COD = 0.40. With this proposed treatment, a final COD of only 453 mg O₂ L⁻¹ was obtained at a treatment cost of EUR 3.42 kg COD⁻¹.     

Carbocyclic analogues of nucleosides from bis-(Hydroxymethyl)-cyclopentane: synthesis,antiviral and cytostatic activities of adenosine,inosine and uridine analogues

Six new carbocyclic nucleosides were prepared by constructing a purine base (in compounds 9-11) or pyrimidine base (in 6-8) on the amino groups of (+/-)-(1 beta,2 alpha,4 beta)-4-amino-1,2-cyclopentanedimethanol (4) and (+/-)-(1 beta,3 alpha,4 beta)-4-amino-1,3-cyclopentanedimethanol (5), and their activities against a variety of viruses and tumour cell lines were determined.     

Application of micellar electrokinetic chromatography to the quality control of a pharmaceutical preparation containing three bronchodilators

Theophylline(1,3-dimethylxanthine), dyphylline [7-(2,3-dihydroxypropyl)theophylline] and proxyphylline [7-(beta-hydroxypropyl)theophylline] are three bronchodilators administered jointly in a single pharmaceutical preparation used against asthma. A micellar electrokinetic chromatography (MEKC) method for their resolution using a background electrolyte consisting of 20 mM tetraborate at pH 8.5 and 100 mM sodium dodecyl sulfate is proposed. The method was used to determine the three active principles in a pharmaceutical preparation. The small amount of sample required and the expeditiousness of the procedure allow content uniformity to be determined in individual tablets. The values of the validation parameters for the method (viz. selectivity, linearity, accuracy, precision, limit of detection, limit of quantitation and robustness) are reported. A complete factor design (2(3)x2) including pH, the surfactant concentration and the ionic strength of the background electrolyte as factors was used to estimate robustness. Based on the results, the method is robust enough for quantitation purposes.     

Study of the action of flavonoids on xanthine-oxidase by molecular topology

A study was performed on xanthine-oxidase inhibition by 22 flavonoids, including flavones, flavonols, flavanones, and chalcones, using UV spectroscopy for experimental data and molecular topology to establish the structure-activity relationship (SAR) model. The flavonoids were classified into four groups according to their activity on xanthine-oxidase (inactive, low, significant, or high), and linear discriminant analysis was used to classify each compound within a group. The results led to a very good model, which was able to classify correctly as xanthine oxidase inhibitors, along with a test set of molecules including a variety of different compounds such as allopurinol, caffeic acid, esculetin, and alloxantin.     

Simple and rapid micellar electrokinetic capillary chromatographic method for simultaneous determination of four antiepileptics in human serum

A very rapid and simple MEKC method was developed for the simultaneous determination of four antiepileptic drugs, ethosuximide (Etho), primidone (Pri), phenytoin (Pht) and carbamazepine (Cbz) in human serum. Sample analysis required only 100 microL of human serum which only needed to be centrifuged, decanted and combined with the running buffer [5.3 mM Na(2)HPO(4)/3.2 mM borax buffer (pH 9.5) containing 55 mM SDS and 3.5% (v/v) acetone]. The analysis was performed in only 10 min into fused-silica capillaries (57 cm total length with 50 microm i.d. and 50 cm to the detector) using the MEKC methodology with diode-array detection at 220 nm. The calibration graphs were established for ethoximide, primidone, phenytoin and carbamazepine between 0 and 20 mg/L. Recoveries were between 85 and 87%. The simplicity of the proposed methodology makes it suitable for routine clinical use, especially for epileptic patients on polytherapy.     

Alkoxide-induced reactions of N-substituted saccharins. Synthesis of 1,2-benzothiazocine 1,1-dioxide and 2,3-dihydropyrrolo[1,2-b]-[1,2]benzisothiazole 5,5-dioxide derivatives

The reactions of saccharin derivatives 1 with sodium alkoxides were studied. Under mild conditions, compounds 1a-f gave the corresponding open sulfonamides 5a-f . Under drastic conditions, β-(saccharin-2)propionic acid derivatives 1a,b reacted with sodium ethoxide affording saccharin and β-ethoxypropionic acid derivatives 4a,b . γ-(Saccharin-2)butyric acid derivatives 1c,d and γ-(saccharin-2)-butyrophenone 1f reacted with sodium t-butoxide in dimethyl sulfoxide affording 5-substituted 6-hydroxy-3,4-dihydro-2H-1,2-benzothiazocine 1,1-dioxides 9 . From mother liquors, 1-substituted 2,3-dihydro-pyrrolo[1,2-b][1,2]benzisothiazole 5,5-dioxides 10 were isolated several hours later, though not detected immediately after completing the reaction. When the reactions were carried out in t-butyl alcohol, the yields of 9 diminished and those of 10 increased with product ratio inversion. Different experimental observations on the possible pathway generating 9 and 10 are discussed.     

Derivative spectrophotometric resolution of mixtures of the food colourants Tartrazine, Amaranth and Curcumin in a micellar medium

A study of the absorption spectra of the food colourants Tartrazine (E-102), Amaranth (E-123) and Curcumin (E-100) in various organic solvents and pH media, have been carried out. In addition, the spectral behaviour in aqueous micellar systems of anionic, cationic and non-ionic surfactants, as well as beta-cyclodextrin, was investigated. Analytical methods are proposed for the determination of the three dyes in mixtures without any prior separation step, by the application of the derivative technique to the normal absorption spectra, based on the use of cetyltrimethylammonium bromide (CTAB) in 0.1 M NaOH, over the concentration range 2-50 mug ml(-1). The methods are applied for determining the three dyes in commercial food products.     

How Aromatic Fluorination Exchanges the Interaction Role of Pyridine with Carbonyl Compounds: The Formaldehyde Adduct

The rotational spectrum of the weakly bound complex pentafluoropyridine⋅⋅⋅formaldehyde has been investigated using Fourier transform microwave spectroscopy. From the analysis of the rotational parameters of the parent species and of the ¹³C and ¹⁵N isotopologues, the structural arrangement of the adduct has been unambiguously established. The full ring fluorination of pyridine has a dramatic effect on its binding properties: It alters the electron density distribution at the π-cloud of pyridine creating a π-hole and changing its electron donor-acceptor capabilities. In the complex, formaldehyde lies above the aromatic ring with one of the oxygen lone pairs, as conventionally envisaged, pointing toward its centre. This lone pair⋅⋅⋅π-hole interaction, reinforced by a weak C−H⋅⋅⋅N interaction, indicates an exchange of the electron-acceptor roles of both molecules when compared to the pyridine⋅⋅⋅formaldehyde adduct. Tunnelling doublets due to the internal rotation of formaldehyde have also been observed and analysed leading to a discussion on the competition between lone pair⋅⋅⋅π-hole and π⋅⋅⋅π stacking interactions.     

Kinetic study of the thermal and thermo-oxidative degradations of polylactide-modified films for food packaging

In this study, the thermal degradations of some commercial polylactide (PLA) films, pure and subjected to various superficial treatments, were investigated in both inert (flowing nitrogen) and oxidative (static air) atmospheres. Degradations were carried out in a thermobalance, in the scanning mode, at various heating rates, and the obtained thermogravimetric curves were discussed and interpreted. Experiments, performed in the temperature range of 35–700 °C, showed similar behavior in both the atmospheres used. The initial decomposition temperature (T _i) and the apparent activation energy (E _a) of degradation of the differently treated PLA films were determined and compared with each other and with those of untreated PLA. The E _a of degradation was obtained by Kissinger’s method, and the values were found increased linearly as a function of crystallinity percentage (%c) as well as the T _i values. The glass transition temperature (T _g) was also determined by differential scanning calorimetry. All the investigated parameters showed dependence on different treatments made to the films. The results obtained for the degradations of PLA films were compared with each other, and a classification of thermal stability in the studied environments were made.     

Dimensional Matching of Polycyclic Aromatics with Rectangular Metallacycles: Insertion Modes Determined by [C?H⋅⋅⋅π] Interactions

A family of Pd^II/Pt^II dinuclear receptors, designed to give a smooth increase in their cavity lengths (from 7.46–13.78 Å), is presented. Their inclusion complexes with a representative set of polycyclic aromatic substrates (naphthalene, carbazol, pyrene, and benzo[a]pyrene), were characterized and studied in aqueous solution and the solid state. By taking into account the dimensions of both receptors and substrates, an excellent complementarity was found between the size of the receptors and their ability to complex a given substrate. Furthermore, this dimensional matching results in specific binding modes depending on the ability of the guest to establish stabilizing [C? H???π] interactions with the host.