Production of <Emphasis Type="Italic">R</Emphasis>-Mandelic Acid Using Nitrilase from Recombinant <Emphasis Type="Italic">E. coli</Emphasis> Cells Immobilized with Tris(Hydroxymethyl)Phosphine

Recombinant Escherichia coli cells harboring nitrilase from Alcaligenes faecalis were immobilized using tris(hydroxymethyl)phosphine (THP) as the coupling agent. The optimal pH and temperature of the THP-immobilized cells were determined at pH 8.0 and 55 °C. The half-lives of THP-immobilized cells measured at 35, 40, and 50 °C were 1800, 965, and 163 h, respectively. The concentration of R-mandelic acid (R-MA) reached 358 mM after merely 1-h conversion by the immobilized cells with 500 mM R,S-mandelonitrile (R,S-MN), affording the highest productivity of 1307 g L^?1 day^?1 and the space-time productivity of 143.2 mmol L^?1 h^?1 g^?1. The immobilized cells with granular shape were successfully recycled for 60 batches using 100 mM R,S-MN as substrate at 40 °C with 64% of relative activity, suggesting that the immobilized E. coli cells obtained in this study are promising for the production of R-MA.     

Characterization of Truncated <Emphasis Type="Italic">dsz</Emphasis> Operon Responsible for Dibenzothiophene Biodesulfurization in <Emphasis Type="Italic">Rhodococcus</Emphasis> sp. FUM94

Numerous desulfurizing bacteria from the Rhodococcus genus harbor conserved dsz genes responsible for the degradation of sulfur compounds through 4S pathway. This study describes a newly identified desulfurizing bacterium, Rhodococcus sp. FUM94, which unlike previously identified strains encodes a truncated dsz operon. DNA sequencing revealed a frameshift mutation in the dszA gene, which led to an alteration of 66 amino acids and deletion of other C-terminal 66 amino acids. The resulting DszA polypeptide was shorter than DszA in Rhodococcus sp. IGTS8 reference strain. Despite the truncation, desulfurizing activity of the operon was observed and attributed to the removal of an overlap of dszA and dszB genes, and lack of active site in the altered region. Desulfurization experiments resulted in specific production rate of 6.3 mmol 2-hydroxy biphenyl (kgDCW)^?1 h^?1 at 2 g l^?1 biocatalyst concentration and 68.8% biodesulfurization yield at 20 g l^?1 biocatalyst concentration, both at 271 μM dibenzothiophene concentration which is comparable to similar wild-type biocatalysts.     

Screening of <Emphasis Type="Italic">Isochrysis</Emphasis> Strains and Utilization of a Two-Stage Outdoor Cultivation Strategy for Algal Biomass and Lipid Production

Isochrysis is a genus of marine algae without cell wall and capable of accumulating lipids. In this study, the lipid production potential of Isochrysis was assessed by comparing 15 Isochrysis strains with respect to their growth rate, lipid production, and fatty acid profiles. Three best strains were selected (lipid productivity, 103.0~121.7 mg L^?1 day^?1) and their lipid-producing capacities were further examined under different controlled parameters, e.g., growth phase, medium nutrient, and light intensity in laboratory cultures. Furthermore, the three Isochrysis strains were monitored in outdoor panel photobioreactors with various initial cell densities and optical paths, and the strain CS177 demonstrated the superior potential for outdoor cultivation. A two-stage semi-continuous strategy for CS177 was subsequently developed, where high productivities of biomass (1.1 g L^?1 day^?1) and lipid (0.35 g L^?1 day^?1) were achieved. This is a comprehensive study to evaluate the lipid-producing capability of Isochrysis strains under both indoor and outdoor conditions. Results of the present work lay a solid foundation for the physiological and biochemical responses of Isochrysis to various conditions, shedding light on the future utilization of this cell wall-lacking marine alga for biofuel production.     

Synthesis,crystal structure and fungicidal activity of 1-(4-chlorophenyl)-2-(5-((3,5-dimethyl-1H-pyrazol-1-yl)methyl)-4-phenyl-4H-1,2,4-triazol-3-ylthio)ethanone

A novel bis-heterocyclic compound was synthesized and characterized. The crystal structure of the title compound (C₂₂H₂₀ClN₅OS, Mr = 437.94) has been determined by single-crystal X-ray diffraction. The crystal is of triclinic, space group P-1 with a = 8.646 (2), b = 9.148 (3), c = 14.540 (4) Å, α = 94.422 (4), β = 98.500 (4), γ = 102.823 (4)°, V = 1101.8 (5) Å³, Z = 2, F(000) = 312, Dc = 1.320 g/cm³, μ = 0.2900 mm^?1, the final R ₁ = 0.041000 and wR ₂ = 0.1160 for 2675 observed reflections with I > 2σ(I). A total of 5623 reflections were collected, of which 3866 were independent (R _int = 0.019000). The fungicidal activity of title compound was determined, the results showed the title compound displayed moderate fungicidal activity against G. zeae Petch, Phytophthora infestans (Mont.) de Bary, Botryosphaeria berengeriana f. sp. piricola (Nose) koganezawa et Sakuma, Fusarium oxysporum f.sp. cucumerinum, and Cercospora arachidicola.     

Enzymatic Hydrolysis of Black Liquor Xylan by a Novel Xylose-Tolerant,Thermostable β-Xylosidase from a Tropical Strain of <Emphasis Type="Italic">Aureobasidium pullulans</Emphasis> CBS 135684

From three cell-associated β-xylosidases produced by Aureobasidium pullulans CBS 135684, the principal enzyme was enriched to apparent homogeneity and found to be active at high temperatures (60–70 °C) over a pH range of 5–9 with a specific activity of 163.3 units (U) mg^?1. The enzyme was thermostable, retaining over 80% of its initial activity after a 12-h incubation at 60 °C, with half-lives of 38, 22, and 10 h at 60, 65, and 70 °C, respectively. Moreover, it was tolerant to xylose inhibition with a K _i value of 18 mM. The K _m and V _max values against p-nitrophenyl-β-d-xylopyranoside were 5.57 ± 0.27 mM and 137.0 ± 4.8 μmol min^?1 mg^?1 protein, respectively. When combining this β-xylosidase with xylanase from the same A. pullulans strain, the rate of black liquor xylan hydrolysis was significantly improved by up to 1.6-fold. The maximum xylose yield (0.812 ± 0.015 g g^?1 dry weight) was obtained from a reaction mixture containing 10% (w/v) black liquor xylan, 6 U g^?1 β-xylosidase and 16 U g^?1 xylanase after incubation for 4 h at 70 °C and pH 6.0.     

Harvesting Microalgae with Different Sources of Starch-Based Cationic Flocculants

In this study, starches obtained from wheat, potato, and corn were used to synthesize cationic starches (CS), and the flocculation efficiency of these materials was tested with Chlorella pyrenoidosa and Botryococcus braunii cultures under different conditions. Our results indicated that these three CS had differing degrees of substitution following identical synthesis conditions. The various CS functioned similarly in this study, and the desired harmless flocculation efficiency was obtained at low dosages, with CS to microalgal biomass ratios of approximately 89 and 119 mg g^?1 for C. pyrenoidosa and B. braunii, respectively. Impressive harmless harvesting efficiencies were obtained at lower dosages with respect to appropriate stirring time before the settling, with ratios ranging from 58 to 78 mg g^?1 for C. pyrenoidosa cultures. The cost of microalgae harvesting can be cut dramatically by choosing cheaper starches prior to the synthetic CS and by applying suitable flocculation procedures.     

Temperature-dependent AC electrical conductivity,thermal stability and different DC conductivity modelling of novel poly(vinyl cinnamate)/zinc oxide nanocomposites

Thermal analysis on organically modified Ca²⁺-montmorillonite (OMON) and its source materials—octadecylamine (ODA) and Ca²⁺-montmorillonite (Ca²⁺-Mon)—was studied using thermally stimulated current (TSC) technique. The appearance of ρ _MON peak with the T _max = 75 °C shows the ability of the developed TSC system to demonstrate the relaxation effects of dehydration in Ca²⁺-Mon. It appeared within the temperature range of DSC endothermic peak (30–100 °C) where the T _mMON = 58 °C. Segmental motions of ODA chains and structural disruptions in the modifier agent compound produced TSC α _ODA, ρ _ODA and ρ _1ODA peaks that are comparable to thermal transition and endothermic peaks in DSC profile (T _gODA, T _m1ODA and T _m2ODA). The effect of localized motion in ODA chains as revealed by the TSC β_OMON peak (T _max = ?23 °C), however, is absent in the DSC profile of OMON. It shows TSC technique has high sensitivity in detecting various relaxation behaviors at molecular level. More evidences are demonstrated by the ρ _OMON (T _max = 86 °C) and ρ _1OMON (T _max = 105 °C) peak originated from the ODA chains structures. These peaks also confirm the intercalation of the modifier cations inside the Ca²⁺-Mon gallery.     

Structure,bioactivity and theoretical study of 1-cyano-<Emphasis Type="Italic">N</Emphasis>-p-tolylcyclo-propanecarboxamide

A novel cyclopropane derivative, 1-cyano-N-p-tolylcyclopropanecarboxamide (C₁₂H₁₂N₂O, Mr = 200.24) was synthesized and its structure was studied by X-ray diffraction, FTIR, ¹H and ¹³C NMR spectrum and MS. The crystals are monoclinic, space group P2_1/c with a = 7.109 (4), b = 13.758 (7), c = 11.505 (6) Å, α = 90.00, β = 102.731 (8), γ = 90.00 °, V = 1097.6 (9) ų, Z = 4, F(000) = 312, D _c  = 1.212 g/cm³, μ = 0.0800 mm^?1, the final R = 0.0490 and wR = 0.1480 for 1,375 observed reflections with I > 2σ(I). A total of 6,109 reflections were collected, of which 2,290 were independent (R _int = 0.0290). Theoretical calculation of the title compound was carried out with HF/6-31G (d,p), B3LYP/6-31G (d,p), MP2/6-31G (d,p). The full geometry optimization was carried out using 6-31G(d,p) basis set, and the frontier orbital energy. Atomic net charges were discussed, and the structure-activity relationship was also studied. The preliminary biological test showed that the synthesized compound is bioactive against the KARI of Escherichia coli.     

Molecular structure and conformation of nitrobenzene reinvestigated by combined analysis of gas-phase electron diffraction,rotational constants,and theoretical calculations

The molecular structure and conformation of nitrobenzene has been reinvestigated by gas-phase electron diffraction (GED), combined analysis of GED and microwave (MW) spectroscopic data, and quantum chemical calculations. The equilibrium r _e structure of nitrobenzene was determined by a joint analysis of the GED data and rotational constants taken from the literature. The necessary anharmonic vibrational corrections to the internuclear distances (r _e ? r _a) and to rotational constants (B _e ⁽ⁱ⁾  ? B ₀ ⁽ⁱ⁾ ) were calculated from the B3LYP/cc-pVTZ quadratic and cubic force fields. A combined analysis of GED and MW data led to following structural parameters (r _e) of planar nitrobenzene (the total estimated uncertainties are in parentheses): r(C–C)_av = 1.391(3) Å, r(C–N) = 1.468(4) Å, r(N–O) = 1.223(2) Å, r(C–H)_av = 1.071(3) Å, \({\angle}\)C2–C1–C6 = 123.5(6)°, \({\angle}\)C1–C2–C3 = 117.8(3)°, \({\angle}\)C2–C3–C4 = 120.3(3)°, \({\angle}\)C3–C4–C5 = 120.5(6)°, \({\angle}\)C–C–N = 118.2(3)°, \({\angle}\)C–N–O = 117.9(2)°, \({\angle}\)O–N–O = 124.2(4)°, \({\angle}\)(C–C–H)_av = 120.6(20)°. These structural parameters reproduce the experimental B ₀ ⁽ⁱ⁾ values within 0.05 MHz. The experimental results are in good agreement with the theoretical calculations. The barrier height to internal rotation of nitro group, 4.1±1.0 kcal/mol, was estimated from the GED analysis using a dynamic model. The equilibrium structure was also calculated using the experimental rotational constants for nitrobenzene isotopomers and theoretical rotation–vibration interaction constants.     

Synthesis,crystal structure,and thermodynamics of a high-nitrogen copper complex with <Emphasis Type="Italic">N</Emphasis>, <Emphasis Type="Italic">N</Emphasis>-bis-(1(2)H-tetrazol-5-yl) amine

A new high-nitrogen complex [Cu(Hbta)₂]·4H₂O (H₂bta = N,N-bis-(1(2)H-tetrazol-5-yl) amine) was synthesized and characterized by elemental analysis, single crystal X-ray diffraction and thermogravimetric analyses. X-ray structural analyses revealed that the crystal was monoclinic, space group P2(1)/c with lattice parameters a = 14.695(3) Å, b = 6.975(2) Å, c = 18.807(3) Å, β = 126.603(1)°, Z = 4, D _c = 1.888 g cm^?3, and F(000) = 892. The complex exhibits a 3D supermolecular structure which is built up from 1D zigzag chains. The enthalpy change of the reaction of formation for the complex was determined by an RD496–III microcalorimeter at 25 °C with the value of ?47.905 ± 0.021 kJ mol^?1. In addition, the thermodynamics of the reaction of formation of the complex was investigated and the fundamental parameters k, E, n, \( \Updelta S_{ \ne }^{{{\uptheta}}} \), \( \Updelta H_{ \ne }^{{{\uptheta}}} \), and \( \Updelta G_{ \ne }^{{{\uptheta}}} \) were obtained. The effects of the complex on the thermal decomposition behaviors of the main component of solid propellant (HMX and RDX) indicated that the complex possessed good performance for HMX and RDX.     

Growth of Cyanobacteria: Optimization for Increased Carbohydrate Content

Growths of Lyngbya limnetica and Oscillatoria obscura were investigated at varying pH, light intensity, temperature, and trace element concentration with a view to optimize these parameters for obtaining the maximum carbohydrate content. The maximum growth for both strains was obtained at pH 9.0 and temperature 20 ± 3 °C using a light intensity of 68.0 μmol m^?2 s^?1 with continuous shaking. Growth under the nitrogen starvation condition affected the carbohydrate content more compared to the phosphorus starvation, and maximum concentrations were found as 0.660 and 0.621 g/g of dry biomass for L. limnetica and O. obscura, respectively. Under the optimized nitrogen-rich conditions, the specific growth rates for the two strains were found to be 0.187 and 0.215 day^?1, respectively. The two-stage growth studies under nitrogen-rich (stage I) followed by nitrogen starvation (stage II) conditions were performed, and maximum biomass and carbohydrate productivity were found as 0.088 and 0.423 g L^?1 day^?1 for L. limnetica. This is the first ever attempt to evaluate and optimize various parameters affecting the growth of cyanobacterial biomass of L. limnetica and O. obscura as well as their carbohydrate contents.     

New hybrids of clozapine and haloperidol and their isosteric analogues: synthesis,X-ray crystallography,conformational analysis and preliminary pharmacological evaluation

Schizophrenia is a debilitating mental disorder which affects approximately 1% of the world’s population. Clozapine is an atypical antipsychotic showing unmatched effectiveness in the control of treatment-resistant schizophrenia. Unlike typical antipsychotics, clozapine does not induce extrapyramidal side effects (EPS), tardive dyskinesia or elevate prolactin levels. However, clozapine can induce a potentially fatal blood disorder, agranulocytosis, in 1–2% of patients, severely limiting its clinical use. The model for antipsychotic activity under investigation is based on obtaining a clozapine-like profile with preferential dopamine D₄ and serotonin 5-HT_2A receptor affinity. Profiled herein are three unique members of a series of prospective antipsychotic agents. Compound (I) originated from the structural hybridization of the commercial therapeutics, clozapine and haloperidol, whilst compounds (II) and (III) possess an alternative tricyclic nucleus derived from JL13; a clozapine-like atypical antipsychotic developed by Liégeois et al. These compounds have been synthesized and characterized by means of elemental analysis, IR, ¹H and ¹³C-NMR spectroscopy, MS and X-ray diffraction. Compound (I) crystallizes in space group P(?1) with a = 10.5032(1), b = 10.6261(2), c = 12.6214(3) Å, α = 81.432(1)°, β = 83.292(1)°, γ = 61.604(1)°, Z = 2, V = 1223.62(4) Å³, C₂₈H₂₉ClN₄O, M _r = 473.00, D _c = 1.284 Mg/m³, μ = 0.185 mm^?1, F(000) = 500, R = 0.0506 and wR = 0.1304. Compound (II) crystallizes in the monoclinic space group P2₁/c with a = 10.8212(2), b = 9.3592(2), c = 22.9494(5) Å, β = 106.471(1)°, Z = 4, V = 2228.88(8) Å³, C₂₅H₂₅ClN₄O₂, M _r = 448.94, D _c = 1.338 Mg/m³, μ = 0.202 mm^?1, F(000) = 944, R = 0.0529 and wR = 0.1129. Compound (III) crystallizes in the monoclinic space group P2₁/c with a = 10.5174(2), b = 9.3112(2), c = 24.2949(5) Å, β = 98.666(1)°, Z = 4, V = 2352.03(8) Å³, C₂₅H₂₄Cl₂N₄O₂, M _r = 483.38, D _c = 1.365 Mg/m³, μ = 0.306 mm^?1, F(000) = 1008, R = 0.0478 and wR = 0.1067. The solid state conformations of (I), (II) and (III) exhibit the characteristic V-shaped buckled nature of the respective dibenzodiazepine and pyridobenzoxazepine nuclei with the central seven-membered heterocycle in a boat conformation. The molecules of (I) form a head-to-tail dimeric motif stabilized by hydrogen bonding. The results of a conformational analysis of compounds (I)–(III) investigating the effect of environment (in vacuo and aqueous solution) are presented. These analogues were tested for in vitro affinity for the dopamine D₄ and serotonin 5-HT_2A receptors and their comparative receptor binding profiles to clozapine and JL13 are reported.     

<Emphasis Type="Italic">cis</Emphasis>-Dioxomolybdenum(VI) complexes of sterically encumbered phenol-based tetradentate N<Subscript>2</Subscript>O<Subscript>2</Subscript> ligands: Structural,spectroscopic, and electrochemical studies

Two cis-dioxomolybdenum(VI) complexes [MoO₂L] (L: L ¹, 2 and L: L ², 3) in a phenol-based sterically encumbered N₂O₂ ligand environment have been synthesized, and their crystallographic characterizations are reported. The orange crystals of 2 are monoclinic, space group P2₁/a with unit cell dimensions as a=16.2407(17) Å, b=7.2857(8) Å, c=18.400(2) Å, β=98.002(9)°, Z=4, and d _cal=1.486 g cm^?3. The light orange crystals of 3, however, are orthorhombic, space group, Pbcn, with unit cell dimensions a=8.3110(12) Å, b=12.637(3) Å, c=34.673(5) Å, Z=4, and d _cal=1.187 g cm^?3. The structures were refined by a full-matrix least-squares procedure on F ² to a final R=0.046 (0.055 for 3) using 4944 (3677) all independent data. In both the cases, the Mo atom exists in a distorted octahedral geometry defined by a N₂O₄ donor set, which features a cis-Mo(–O)₂ and a trans-Mo(OPh)₂ arrangement. Compound 2 undergoes a quasireversible one-electron reduction at ?1.3 V vs Ag/AgCl reference due to Mo^VIO₂/Mo^VO₂ electron transfer and thus providing a rare example of steric solution to the comproportionation–dimerization problem encountered frequently in the development of valid biomimetic models for the active sites of oxomolybdenum enzymes.     

Kinetics of Na|CF<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript> and Li|CF<Subscript><Emphasis Type="Italic">x</Emphasis></Subscript> systems

Properties of CF _x /Li and CF _x /Na cells were examined while using galvanostatic charging/discharging, electrochemical impedance spectroscopy and scanning electron microscopy (SEM). The capacity during the first cycle was as high as ca. 1000 mAh g^?1. Such an electrode is suitable for primary CF _x /Li and CF _x /Na batteries. SEM images of CF _x cathode showed that during discharging it was transformed into amorphous carbon and LiF or NaF crystals (of diameter of ca. 5–20 μm). These systems (C?+?LiF or C?+?NaF) cannot be reversibly converted back into CF _x /Li or CF _x /Na, respectively. Exchange current densities are between 10^?7 Acm^?2 and 10^?9 Acm^?2 when working with LiPF₆ and NaPF₆ electrolytes (1.12?×?10^?7 Acm^?2 and 6.82?×?10^?9 Acm^?2, respectively). Those values are low and indicate that the charge transfer process may be the rate-determining step. Activation energies for the charge transfer process were 57 and 72 kJ mol^?1 for CF _x /LiPF₆ and CF _x /NaPF₆ systems, respectively. Higher activation energy barrier for the CF/Na⁺?+?e^??→?C?+?NaF reaction results in lower observed exchange current density in comparison to the system with lithium ions.     

Crystal structure,DFT study,antimicrobial properties and DNA cleavage potential and thermal behavior of some new mercury complexes

In this study, a new bidentate Schiff base ligand (L) entitled as N,N’-bis(dimethylaminocinnamaldehyde)-2,2-dimethyl-1,3-propanediamine and its mercury complexes were synthesized. The Schiff base ligand and its complexes were characterized using FT-IR, ¹H-, ¹³C-NMR spectroscopy, molar conductivity and electronic spectral study. Regarding physical and spectral data, the general formula for the complexes was suggested as HgLX₂ (L = Schiff base ligand and X = Cl^?, Br^?, I^?, SCN^?, N₃ ^?). For structural identification of these complexes, crystal structure of mercury iodide complex was analyzed as typical one. In the structure of this complex, Hg ion is surrounded by 2 iodide ions and 2 N atoms from the Schiff base ligand to form a four-coordinated mercury complex in triclinic system with space group of P ₁. Angular index (τ ₄) value was evaluated equal to 0.85, so the geometry around the mercury ion in this complex can be described as trigonal pyramid. A layered supramolecular structure for HgLI₂ complex is stabilized by C–H···I and C–H···π interactions in solid state. DFT study on the ligand and its complexes was also carried out, and then some calculated and experimental structural parameters of HgLI₂ were compared. Thermal behaviors of the titled compounds were investigated by thermogravimetric analyses. Furthermore, biological properties of the ligand and its complexes were examined against some Gram-negative and Gram-positive bacteria and also against 2 fungi. Finally, the interaction of the ligand and its complexes with DNA was investigated by electrophoresis method.     

Preparation,characterization and crystal structures of metal(II) tetraza macrocyclic complexes with organic co-ligands

The complexes [Ni(L1)(pyc)₂]·2H₂O (1) (L1 = C-meso-5,5,7,12,12,14-hexamethyl-1,4,8,11-tetraazacyclotetradecane; Hpyc = pyrazinecarboxylic acid) and [Cu(L2)(H-cpdc)] (2) (L2 = 3,14-dimethyl-2,6,13,17-tetraazatricyclo[14,4,0^1.18,0^7.12]docosane; H₂-cpdc = cyclopropanedicarboxylic acid) have been synthesized and structurally characterized. The crystal structure of complex 1 shows a distorted octahedral coordination geometry around the nickel(II) center, with four secondary amines in the equatorial positions and two nitrogen atoms of the pyc^? ligands in the trans positions. In complex 2, the coordination environment around the copper(II) center is a Jahn–Teller distorted octahedron with four Cu–N bonds and two axial Cu–O bonds. The electronic spectra, electrochemical and TGA behavior of the complexes are significantly affected by the nature of the axial pyc^? and H-cpdc^? ligands.     

Pomegranate rind-derived activated carbon as electrode material for high-performance supercapacitors

In this paper, activated carbon materials were synthesized from pomegranate rind through carbonization and alkaline activation processes. The effects of pyrolytic temperature on the textual properties and electrochemical performance were investigated. The surface area of the activated carbon can reach at least 2200 m² g^?1 at different pyrolytic temperatures. It was found that, at the range of 600–900 °C, decreasing the carbonization temperature leads to the increase of t-plot micropore area, t-plot micropore volume, and capacitance. Further decreasing the carbonization temperature to 500 °C also leads to the increase of t-plot micropore area and t-plot micropore volume, but the capacitance is slightly poorer. The activated carbon carbonized at 600 °C and activated at 800 °C possesses very high specific area (2931 m² g^?1) and exhibits very high capacitance (～268 F g^?1 at 0.1 A g^?1 and ～242 F g^?1 at 1 A g^?1). There is no capacitance fading after 2000th cycle.     

Thermal analysis of a white calcium bentonite

A white calcium bentonite (CaB) taken from Çaml?dere (Ankara, Turkey) region was heated at various temperatures between 100 and 1100 °C for 2 h. The mineralogy of the CaB was determined as calcium smectite (CaS), metahalloysite (MH), opal-A (OA), opal-CT (OCT), quartz (Q), feldspar (F), and calcite (C) using the X-ray diffraction patterns of the natural CaB and its heated samples. Besides the XRD patterns, the thermogravimetry, differential thermal analysis, and low-temperature nitrogen adsorption (N₂-AD) data show that the CaS lose adsorbed and hydration water up to 300 °C, dehydroxylation takes place between 300 and 750 °C, and then the 2:1 layer structure completely collapses above 900 °C. The activation energies for the dehydration and dehydroxylation were calculated as 7636 and 48838 J mol^?1, respectively, from the TG data using Coats and Redfern method. The specific surface area (S) and specific micro–mesopore volume (V) obtained from N₂-AD data were 44 m² g^?1 and 0.100 cm³ g^?1 for the natural CaB. S and V reach their maxima of 105 m² g^?1 and 0.155 cm³ g^?1, respectively, at 300 °C, remain approximately constant as the temperature increases up to 700 °C and then decrease almost in parallel with each other, reaching their minima at 900 °C. This indicates that the S and V values increase gradually during dehydration and dehydroxylation of the CaS.     

Dissolved air flotation for treating wastewater of the nuclear industry: preliminary results

Preliminary testing of dissolved air flotation (DAF) for wastewater treatment is presented. A combined coagulation-flocculation/DAF column system is used to remove oil and ⁶⁰Co from nuclear industry wastewater. In this work, operational conditions and coagulant/flocculant concentrations are optimized by varying pH. Determinations of air-solids ratio (G/S), retention time (θ), pressure (P), volume of depressurized air–water mixture (V), turbidity and ⁶⁰Co concentrations are reported. The effect of the treatment on the efficiency of separation of oily residues is also discussed. The results establish that the coagulant/flocculant system, formed by a modified polyamine (25 mgL^?1) and a slightly cationic polyacrylamide (1.5 mgL^?1), under specific operational conditions (pH = 7, mixing intensity Im₁ = 300 s^?1 and Im₂ = 30 s^?1), allowed the destabilization of colloidal matter, resulting in resistant flocs. It was concluded that by using G/S = 0.3, θ = 15 min, P = 620 kPa and V = 0.0012 m³, the greatest percentage removals of oil, turbidity, total cobalt and ⁶⁰Co were obtained. These preliminary results then show that dissolved air flotation represents a good alternative for treatment of nuclear industry wastewater contaminated with radionuclides.     

Synthesis,characterization, and crystal structure of modified benzophenone UV-absorber containing reactive group

A modified benzophenone UV-absorber containing reactive group (4-(4,6-dichloro-1,3,5-triazin-2-yloxy)-2-hydroxyphenyl)phenyl)methanone (UV-DTHM) has been prepared in good yield from the nucleophilic substitution reaction of 2,4-dihydroxy benzophenone with 2,4,6-trichlorotriazine, catalyzed by 1.3 equiv. NaOH. The most favorable reaction conditions (the catalyst dosage, the mole ratio of the reactants, and reactive time) were selected. The compound was characterized by IR spectroscopy, ¹H NMR, ¹³C NMR, mass spectrometry, elemental analysis, and single crystal X-ray diffraction. The crystal monoclinic, space group C c with the unit cell parameters a = 3.987(2), b = 30.688(16), c = 12.423(6) Å and α = 90.00, β = 92.117(15), γ = 90.00º, Z = 4, R = 0.0620. wR(F ²) = 0.1589. The crystal structure reveals that 2,4,6-trichlorotriazine is boned to 4-seat hydroxyl of 2,4-dihydroxy benzophenone and a intramolecular hydrogen bond is formed with hydrogen of 2-hydroxyl and oxygen of carbonyl group. Moreover, thermogravimetric analysis (TGA) of UV-DTHM was studied, showing two distinct endothermic peaks at temperatures of 281.5 and 358.5 °C. The molar absorption coefficient of UV-DTHM is 1.6 × 10⁴ and 6.3 × 10³ at 268 and 330 nm, respectively, and shows excellent ultraviolet absorption property.