TLC and HPLC Analysis of the Phenolic Acids in Silphium perfoliatum L. Leaves,Inflorescences and Rhizomes

JPC – Journal of Planar Chromatography – Modern TLC - TLC and HPLC have been used for preliminary evaluation of the phenolic acids occurring in the leaves, inflorescences, and rhizomes...     

Thioacetylacetone: structural and vibrational assignments.

Thioacetylacetone and its variously deuterated isotopomers have been investigated using electronic and vibrational spectroscopy combined with quantum chemical calculations. Thioacetylacetone is known for its photochromic properties, but the structures of the initial and final forms have been the subject of a long debate. Analysis of the IR spectra recorded in low-temperature argon and xenon matrices, room-temperature solutions, and in the gas phase has allowed us to establish the nature of the photochromic species and of its precursor. Similar to the case of another beta-thioxoketone, monothiodibenzoylmethane, the photo-product has been assigned to the nonchelated SH exo-rotamer of the (Z)-enethiol tautomeric form, whereas the dominant ground-state species corresponds to the chelated (Z)-enol tautomeric form. Detailed vibrational assignments have been proposed for both forms based on quantum chemical calculations and polarization experiments. In the case of the chelated (Z)-enol species prevailing in the ground state, a second-order perturbative anharmonic analysis at the B3LYP/cc-pVTZ level indicated strong anharmonic effects associated with the intramolecular hydrogen bond, leading to a shift of more than 600 cm-1 of the wavenumber of the OH-stretching vibration. A small fraction of the SH endo-rotameric chelated (Z)-enethiol form was also detected under unperturbed conditions. The (Z)-enethiol form can be converted into the (Z)-enol form by irradiation at 290 nm.     

A polymorphic pocket at the P10 position contributes to peptide binding specificity in class II MHC proteins

Peptides bind to class II major histocompatibility complex (MHC) proteins in an extended conformation. Pockets in the peptide binding site spaced to accommodate peptide side chains at the P1, P4, P6, and P9 positions have been previously characterized and help to explain the obtained peptide binding specificity. However, two peptides differing only at P10 have significantly different binding affinities for HLA-DR1. The structure of HLA-DR1 in complex with the tighter binding peptide shows that the peptide binds in the usual polyproline type II conformation, but with the P10 residue accommodated in a shallow pocket at the end of the binding groove. HLA-DR1 variants with polymorphic residues at these positions were produced and found to exhibit different side chain specificity at the P10 position. These results define a new specificity position in HLA-DR proteins.     

Microviscosity of ions and salting-out in the extraction of rare-earth and transplutonium elements

A chemical procedure has been developed for the separation of U, Th, Fe, Sc, Na, Ta and Mo, which interfere in neutron activation analysis of the lanthanide elements in rocks. This methods in based on the extraction of interferents, before irradiation of the samples, using a solution of tetracycline in benzyl alcohol. The lanthanide elements remain in the aqueous phase and are coprecipitated with calcium oxlate or ferric hydroxide for irradiation and subsequent determination by gamma-ray spectrometry. Conditions for the separation of these interferences are examined determining the extraction curves. The chemical separation procedure was applied in the analysis of lanthanides in geological materials and the results showing the accuracy and the reproducibility of the method are presented. The sensitivity for all the lanthanides was determined.     

Mathematical model of aerobic stabilization of old landfills

A short-term aerobic stabilization of digested waste in the final methane phase was studied. The effect of aeration rate on the reduction of leachate parameters and on the rate of CO₂ production and O₂ assimilation was investigated. Experimental simulation of aerobic landfill stabilization was carried out using lysimeters. When testing the effect of aeration rate on the reduction of leachate indices (BOD₅, COD, N-NH₄⁺), it was reported that the most significant reduction was obtained at the highest rate of aeration and the smallest reduction of leachate indices was attained not at the lowest but at medium aeration rates. Both the rate of CO₂ production and the O₂ assimilation reached their highest values in the lysimeters aerated at a high rate of aeration. The proposed mathematical model which consists of a system of five differential equations describing CO₂ production, O₂ assimilation and the changes of organic carbon content in the leachate correspond well with the experimental data.     

Der Einsatz von Sorbentien räumlich-globulrer Struktur zur Abtrennung radioaktiver Verunreinigungen aus Wasser

Abstract

Possibilities of using a new generation of sorbents have been investigated. Polymers of spatial-globular (spherulitic) structure (RGS polymers) have been tested to separate Cs, Sr and rare earth elements – which can also be radioactive contaminants – from different waters.

RGS polymers are both, solids and highly-disperse systems being extremely permeable to fluids and gases with low pressure decline. They were currently used to clean industrial waste-water.

It is shown that these polymers can be used successfully to separate radionuclides. Polymers RGS-81 and RGS-112 have high distribution coefficients for CS, Sr, Sc, the lanthanide series and Hf in weakly acid solutions. In HF solutions, Sc and Hf can be separated from Cs, Sr and the lanthanides.     

Reaction of Phenolic Mannich Base with Trialkyl Phosphite

Dialkyl [2-hydroxy-5-(phenylazo)benzyl]phosphonates were prepared by a convenient procedure in good yield from Mannich base and trialkyl phosphite in benzene with the elimination of ammonium or morpholinium cation. 2-[(Dialkylamino)methyl]-4-(phenylazo)phenol methiodide is a new reagent in the Michaelis-Arbuzov reaction.     

A New Phosphonium Calix[4]arene for Selective Anion Recognition: Synthesis and Studies in Solution and in Ion Selective Electrodes

The synthesis and characterization of a new tetra (triphenylphosphonium) p-tert-butylcalix[4]arene 2 is presented. Its interactions with anions were studied by ¹H and ³¹P NMR and UV absorption spectrophotometry, showing the biggest interaction with ClO₄ ^? , I^?  and SCN^? . Anion selectivity in ion-selective PVC-membrane electrodes (ISEs) plasticized with o-NPOE containing ionophore 2 was also investigated. Compound 2 shows a potentiometric response for various anions with the following selectivity pattern: ClO₄ ^?  > SCN^?  > I^?  > Cr₂O₇ ^2 ?  > NO₃ ^?  > Br^?  > Cl^? .