Simultaneous determination of Cd,Cr, Cu,Ni, Pb and Zn in sewage sludge by slurry introduction ICP-OES method

In order to evaluate the slurry nebulisation method as an alternative method for analysis of sewage sludge, the metal content of sludge samples of different origins was determined. The concentrations of six elements: Cd, Cr, Cu, Ni, Pb, and Zn were determined by introducing the sludge as a slurry into an inductively coupled plasma optical emission spectrometer (ICP-OES). Calibration was performed by using aqueous standard solutions. For comparison, the sewage sludge was also digested by microwave digestion and introduced into the plasma as an aqueous solution. The accuracy of the method was checked by analysing a sewage sludge certified reference material (CRM 007-040 Sewage Sludge). The Student's t-test showed that values obtained using slurry nebulisation were close to the certified values at a 95% confidence level. The values of elements Cd 11.1?±?0.8; Cr 37.7?±?3.3; Cu 563.3?±?38.4; Pb 119.2?±?10.1; Zn 729?±?68.2?mg?kg^?1 obtained using this method were comparable with those obtained using the conventional method. The slurry method can, therefore, be successfully applied to the determination of content of each element in sewage sludge with RSD less than 3%, without the need to predissolve them. This could avoid the use of hazardous chemicals, incomplete dissolution and loss of volatile analytes.     

Molecular organization in two-dimensional films of liquid II. Langmuir and Langmuir-Blodgett films of a perylene-like dye mixed with liquid crystals having a terminal cyano group crystalline mixtures

Langmuir and Langmuir-Blodgett (LB) films of a perylene-like compound and its binary mixtures with 4-octyl-4'-cyanobiphenyl (8CB) and 4-pentyl-4"-cyano-p-terphenyl (5CT) have been studied. On the basis of the surface pressure-area isotherms, the molecular organization on the air-water interface has been estimated. Information about the miscibility or the phase separation of components in the binary mixtures has been obtained. The spectroscopic study of the LB films has allowed conclusions to be drawn about the arrangement of the molecules on the quartz slides. The fluorescence spectra of the LB films of the perylene-like compound have revealed the formation of self-aggregates.     

Diaquadichloridobis(1H‐imidazole)manganese(II) at 100 K

The mononuclear title complex, [MnCl₂(C₃H₄N₂)₂(H₂O)₂], is located on a crystallographic inversion center. The Mn^II ion is coordinated by two imidazole ligands [Mn—N = 2.2080 (9) Å], two Cl atoms [Mn—Cl = 2.5747 (3) Å] and two water molecules [Mn—O = 2.2064 (8) Å]. These six monodentate ligands define an octahedron with almost ideal angles: the adjacent N—Mn—O, N—Mn—Cl and O—Mn—Cl angles are 90.56 (3), 92.04 (2) and 90.21 (2)°, respectively. Hydrogen bonds between the coordinated water molecules and Cl atoms form a two‐dimensional network parallel to (100) involving R₄²(8) rings. The two‐dimensional networks link into a three‐dimensional framework through weaker N—H...Cl interactions. Thermogravimetric analysis results are in accordance with the water‐coordinated character of the substance and its dehydration in two successive steps.     

Chemoselective Removal of Protecting Groups from O-Glycosyl Amino Acid and Peptide (Methoxyethoxy)ethyl Esters Using Lipases and Papain

The selective C-terminal deprotection of O-glycopeptide (methoxyethoxy)ethyl esters is achieved under mild conditions (pH 6.6, 37 degrees C) by enzymatic hydrolysis using papain or lipase M from Mucor javanicus to give building blocks useful for chain-extending glycopeptide synthesis. On the other hand, the selective removal of acetyl protecting groups from the saccharide portion of glycopeptides is accomplished by alternative enzymatic hydrolysis with lipase WG from wheat germ to furnish model substrates for enzymatic glycosyl transfer reactions in order to extend the carbohydrate side chain of these conjugates.     

Alignment of liquid crystal and dichroic dye molecules in mixed Langmuir and Langmuir-Blodgett films

A study of dichroic dye-liquid crystal mixtures (guest-host systems) in monolayers formed at a gas-liquid interface (Langmuir films) and at a solid surface (Langmuir-Blodgett films) has been made. As a host 4- n -octyl-4'-cyanobiphenyl (8CB) or 4- n -pentyl-4"-cyano- p -terphenyl (5CT) were chosen, while three dichroic azo dyes with various molecular structures were used as guest species. The dyes were added to the liquid crystal matrices at a concentration corresponding to the whole range of molar fractions and the surface pressure-mean molecular area isotherms for Langmuir films were recorded. On the basis of the isotherms, conclusions about the molecular organization and the miscibility of the components in the ultrathin films were drawn. The Langmuir films were transferred onto the quartz plates at surface pressures below the collapse point. The polarized absorption spectra of the Langmuir-Blodgett films were recorded and information about the alignment and intermolecular interactions in the mixtures of the non-amphiphilic dichroic dyes and the liquid crystals with strongly polar terminal groups were obtained.     

Application of carbon nanotubes as solid-phase extraction sorbent for analysis of chlorophenols in water samples

The aim of this work was to investigate the efficiency of various MWCNTs as SPE materials for the preconcentration of chlorophenols. The COOH-functionalized MWCNTs and MWCNTs were used as SPE sorbents. To evaluate the capability of MWCNTs for the preconcentration of chlorophenols from water samples, 2,4-chlorophenol, 4-chlorophenol, 2,4,6-chlorophenol, 2,6-chlorophenol, 3,4-chlorophenol, and 2-chlorophenol were used as model compounds. Chlorophenols were extracted with acetone, methanol, ethanol, and dichloromethane, and determined by gas chromatography–mass spectrometry. COOH-functionalized MWCNTs <8 nm were found to be the best sorbent for the tested chlorophenols. For COOH-functionalized MWCNTs <8 nm, the recovery rates for all chlorophenols were higher than 50% when acetone or ethanol was used as eluents. In the case of dichloromethane elution, recovery rates for chlorophenols were from 62.0% for 2,6-DCP to 116.8% for 2,4-DCP; only for 2,4,6-TCP was the recovery rate 30.6%. Similar percentage recoveries were achieved with methanol as the eluent.     

Synthesis and Sm/Sm doping effects on photoluminescence properties of Sr4Al14O25

Complete and partial samarium reduction was achieved under strong reducing atmosphere by solid-state and combustion synthesis of Sr_3.96Sm_0.04Al₁₄O₂₅. Dependence of different fluxing agents on the formation of various strontium aluminates was examined. The samples were investigated by X-ray powder diffraction, temperature dependent luminescence decay and photoluminescence measurements. Excitation with UV radiation resulted in sharp and well resolved emission lines of samarium ions. Distinct temperature behavior for Sm²⁺ and Sm³⁺ were detected in the range of 100-500 K. Estimated emission thermal quenching values (TQ_1/2) for divalent samarium were approximately 270 K while for trivalent state around 660 K. Measured luminescence decay values of Sm²⁺ are substantially lower than for Sm³⁺,≈1.7 and ≈2.7 ms, respectively. The spectral feature of Sm²⁺ emission spectrum indicates that dopant occupies low symmetry site in Sr₄Al₁₄O₂₅ compound.     

Synthesis, spectroscopic characterization, X-ray structure and DFT calculations of [Re(CO)3L2Cl] (L = 1,2,4-triazolo-[1,5-a]pyrimidine)

The paper presents a combined experimental and computational study of novel tricarbonyl complex – fac-[Re(CO)₃(tp)₂Cl] (tp = 1,2,4-triazolo-[1,5-a]pyrimidine). The compound has been characterized spectroscopically and structurally (by single-crystal X-ray diffraction). The absorption and emission spectra of the complex have been discussed on the basis of DFT and time-dependent (TD)DFT calculations.     

Reliability in reconstruction of the axisymmetric refractive index profiles from transverse interferograms. Accurate versus approximate methods: A comparative study

A mathematical formalism related to the approximate as well as the accurate interferometric data reduction schemes is briefly outlined and subsequently applied in the reconstruction of the assumed (Luneburg) axisymmetric refractive index distribution. The presented comparative analysis confirms the generally held opinion that the approximate methods (“straight-line” and Kokubun-Iga approaches) may provide quite reasonable results in the examination of refractively inhomogeneous disturbances characterized by weak gradient and moderate index variation. On the other hand, the accurate scheme for transverse interferometric data interpretation and reduction, based on the close-form correlation between the fringe shift and the deflection function, [1] remains the only method for reliable reconstruction of strongly refracting index profiles, independently of magnitude of refraction and ambiguity of the fringes. This fact is of considerable importance for transverse interferometry of fibers (preform rods) and/or GRIN-rod lenses characterized by high numerical apertures.