Cloud point extraction procedure for flame atomic absorption spectrometric determination of lead(II) in sediment and water samples

The conditions for cloud point extraction of lead(II) from aqueous solutions were investigated and optimized. The procedure is based on the separation of Pb(II) – brillant cresyl blue (BCB) complexes into the micellar media by adding the surfactant Triton X-114. After phase separation, the surfactant-rich phase was dissolved with 1 mol L⁻¹ HNO₃ in ethanol and diluted with 1 mol L⁻¹ HNO₃ solution before lead was determined by flame atomic absorption spectrometry. Optimization of the pH, ligand and surfactant quantities, incubation time, temperature, viscosity, sample volume, and interfering ions was performed. The effects of the matrix ions were also examined. The detection limits for three times the standard deviations of the blank for lead were 7.5 μg L⁻¹ for water samples and 0.33 μg g⁻¹ for sediment samples. The validity of cloud point extraction was checked by employing certified reference samples of Lake Sediment IAEA-SL-1 and Sewage Sludge BCR-CRM 144R. The procedure was applied to natural waters and sediment samples with satisfactory results (recoveries >95%, relative standard deviations <6.4%).     

Determination of the local inhomogeneity of a crystal lattice using a two-frequency nuclear quadrupole resonance method

Nonuniform line broadening in quadrupole spin systems is analyzed. It is shown theoretically that this broadening is of the tensor type. This forms the basis of the method for analyzing the distribution of local inhomogeneities in the crystal lattice, which is verified experimentally on a sodium nitride sample.     

Synthesis and investigation of antibacterial activities and carbonic anhydrase and acetyl cholinesterase inhibition profiles of novel 4,5-dihydropyrazol and pyrazolyl-thiazole derivatives containing methanoisoindol-1,3-dion unit

Novel 4,5-dihydropyrazole derivatives (3a–i), 3-(4-((3aR,4S,7R,7aS)-1,3-dioxo-3a,4,7,7a-tetrahydro-1H-4,7-methanoisoindol-2(3H)-yl)phenyl)-5-phenyl-4,5-dihydro-1H-pyrazole-1-carbothio amide, were obtained by the addition of thiosemicarbazide (2) to the chalcones (1a–i). The addition–cyclization of 2,4′-dibromoacetophenone (4) to pyrazole derivatives (3a–i) gave the new pyrazolyl-thiazole derivatives (5a–i), (3aR,4S,7R,7aS)-2-(4-(1-(4-(4-bromophenyl)thiazol-2-yl)-5-phenyl-4,5-dihydro-1H-pyrazol-3-yl)phenyl)-3a,4,7,7a-tetrahydro-1H-4,7-methanoisoindole-1,3(2H)-dione. Antibacterial and acetylcholinesterase (AChE) enzyme and human carbonic anhydrase (hCA) I, and II isoform inhibitory activities of the compounds 3a–i and 5a–i were investigated. Some of the compounds showed promising antibacterial activity. In addition, the hCA II and I were effectively inhibited by the lately synthesized derivatives, with K_i values in the range of 18.90?±?2.37 ?58.25?±?13.62?nM for hCA II and 5.72?±?0.98 ?37.67?±?5.54?nM for hCA I. Also, the K_i parameters of these compounds for AChE were obtained in the range of 25.47?±?11.11???255.74?±?82.20?nM. Also, acetazolamide, clinical molecule, was used as a CA standard inhibitor that showed K_i value of 70.55?±?12.30?nM against hCA II, and 67.17?±?9.1?nM against hCA I, and tacrine inhibited AChE showed K_i value of 263.67?±?91.95.     

Efficient one-pot three-component method for the synthesis of highly fluorescent coumarin-containing 3,5-disubstituted-2,6-dicyanoaniline derivatives under microwave irradiation

A simple and concise approach to the synthesis of coumarin-containing highly fluorescent asymmetric/symmetric 3,5-diaryl/heteroaryl-2,6-dicyanoaniline derivatives are reported. The compounds were synthesized through base catalyzed three-component one-pot synthesis reaction of 2-(1-(7-(diethylamino)-2-oxo-2H-chromen-3-yl)ethylidene)malononitrile, aliphatic, aromatic/heteroaromatic aldehydes, and malononitrile in solvent-free reaction medium, catalyzed by piperidine under microwave irradiation method. The reaction gave the novel, highly fluorescent coumarin-containing 3,5-disubstituted-2,6-dicyanoaniline derivatives in good yields at 300?W, 80?°C in 2?min. This method provides several advantages; such as shorter reaction time, environmental friendliness, simple workup procedure, lower energy consumption and, generally, good yields with high purity. In addition, the synthesized compounds are fluorescently active dyes even in day light, except for compounds including nitro substituent, and show maximum absorption wavelengths (λ_abs.max) in the visible region in DMSO at room temperature. Thermal properties of all the synthesized compounds were also evaluated with thermal gravimetric analysis for usability as optic dye. Optical and thermal screening studies of the compounds showed that the dyes have excellent photophysical and thermal stability properties.     

Investigation of clinoptilolite rich natural zeolites from Turkey: a combined XRF,TG/DTG,DTA and DSC study

Turkey clinoptilolite-rich tuffs from Gördes and Bigadiç regions of western of Anatolia and their exchanged forms (K⁺, Na⁺, Mg²⁺ and Ca²⁺) were characterized by TG/DTG-DTA, DSC and XRF methods and the surface areas were also determined for both tuffs. TG-DTG and DTA curves of all clinoptilolite samples were measured in the temperature range 30–1000 °C. All clinoptilolite samples had major, rapid mass losses between 30 and 200 °C, with slower and less significant mass losses at higher temperatures. The mass loss of the Natural-G is 9.54% while that of the Natural-B sample is 10.50%. Water content increases in the order of K < Na < Ca < Mg for Bigadiç clinoptilolite samples and in the following sequence K < Na < Mg < Ca for Gördes clinoptilolite samples. One mass loss step for all clinoptilolite samples was observed using differential scanning calorimeter (DSC) in the range of 30–550 °C.     

Dipolar and quadrupolar detection using an FT-ICR MS setup at the MPIK Heidelberg

Dipolar and single-phase two-electrode quadrupolar detection schemes have been investigated at a Fourier transform ion cyclotron resonance mass spectrometry (FT-ICR MS) setup built for the KATRIN experiment at the Max-Planck-Institute for Nuclear Physics (MPIK) in Heidelberg. We present first experimental results of ⁷Li^?+? signals from a cylindrical Penning trap configuration for both detection schemes. While the prominent signal of the conventional dipolar detection scheme marks the reduced cyclotron frequency, the main signal for the quadrupolar detection appears at the sum of the reduced cyclotron frequency and the magnetron frequency. For ideal trapping fields, this sum frequency equals the ion cyclotron frequency ?? _c ?=?qB/(2??m). Sidebands due to the combined motions of the cyclotron mode and magnetron mode are observed by quadrupolar detection which allows the determination of the respective combinations of eigenfrequencies.     

Chloro-Bridged Dimeric Cadmium(II)-Isothiocyanate Complex with a Tridentate NNN Type Ligand: Synthesis,X-ray Structure,Thermal Analysis

Abstract  

The dinuclear cadmium(II) complex with 2,6-bis(3,4,5-trimethyl-N-pyrazolyl)pyridine (btmpp) has been synthesized, and characterized by single crystal X-ray diffraction, IR, UV–Vis and TGA–DTA methods. Cd atoms are located in a distorted octahedral environment in the complex. The complex crystalizes in monoclinic space group C 2/c, with unit cell dimensions a = 20.5636(12) Å, b = 14.0167(13) Å, c = 15.6598(11) Å, β = 113.425(5)o, V = 4141.7(5) Å³. There are two intermolecular and a intramolecular hydrogen bonds interactions in crystal.     

On the Pure-injectivity Profile of a Ring

An analog of the injective profile of a ring, with relative injectivity replaced by relative pure-injectivity, is investigated. Emphasis is placed on comparing and contrasting the properties of both profiles. In particular, the analog in this context of the notion of poor modules is considered and properties of pure-injectively poor modules are determined. While we do not know of any ring that does not have pure-injectively poor modules, their existence has not been determined in general. Rings having pure-injectively poor modules of various types are characterized.     

Phase diagram for stripes in YBa2Cu3O6+x superconductors

Neutron scattering has been used to measure the charge and spin structure in the YBa₂Cu₃O_6+x superconductors. Incommensurate static charge ordering is found at low doping levels while only charge fluctuations are found at higher doping. The spin structure is complex with both a commensurate resonance and incommensurate structure observed at low temperatures. The scattering results are used to construct a phase diagram for stripes in the YBa₂Cu₃O_6+x system.