Synthesis and structural characterization of a fully conjugated macrocyclic tetraaza(14)-membered Schiff base and its bivalent metal complexes

A novel 14-membered macrocyclic Schiff base derived from 3-cinnamalideneacetoacetanilide and o-phenylenediamine acts as a tetradentate and strongly conjugated ligand to form a cationic solid complex with CuCl₂/NiCl₂/CoCl₂/ZnCl₂. The ligand and the complexes were characterized by the usual spectral and analytical techniques. The main i.r. band of the macrocyclic Schiff base was compared to that of its metal complexes. The C=N bands are shifted to the lower wave number. The cyclic voltammogram of the copper complex shows that the macrocyclic ligand is able to stabilize the copper(III) oxidation state. The e.s.r. spectra of the copper complex in DMSO solution at room temperature and liquid N₂ temperature were recorded and their salient features thoroughly discussed. The antimicrobial screening tests were also recorded and gave good results in the presence of metal ions in the ligand system.     

On the mechanism of electroluminescence emission by porous silicon layers

The analytical treatment of a model considering the electrooxidation of p-porous silicon layers under galvanostatic conditions is able to give account of experimental facts such as the shape and location of the electroluminescence peak as well as of the spectral shift of the electroluminescence peak produced by oxidation. The proposed model considers electroluminescence to be the result of electron injection into the conduction band by an adsorbed intermediate produced by electrooxidation of the surface coverage with hydrogen or siloxene of the silicon nanocrystallites. The access of holes to the surface is made possible by low accumulation layer conditions and is the rate determining step in the electroluminescence mechanism. In this way it is possible to give a satisfactory explanation to the shift towards the blue experimented by the electroluminiscence emission maximum as a consequence of electrooxidation.     

Poly[3-(3,4-dihydroxyphenyl)glyceric acid] from Stems of <Emphasis Type="Italic">Symphytum asperum</Emphasis> and <Emphasis Type="Italic">S. caucasicum</Emphasis>

Two high-molecular-weight (>1000 kDa) water-soluble preparations were isolated from stems of Symphytum asperum and S. caucasicum. Their basic component was established as poly[hydroxy-1-carboxy-2-(3,4-dihydroxyphenyl)ethylene], analogous to that of high-molecular-weight (>1000 kDa) preparations from roots of these same plants, using IR and NMR spectral data. __________ Translated from Khimiya Prirodnykh Soedinenii, No. 4, pp. 303–305, July–August, 2005. An erratum to this article is available at .     

High-productivity continuous biofilm reactor for butanol production

Corn steep liquor (CSL), a byproduct of the corn wet-milling process, was used in an immobilized cell continuous biofilm reactor to replace the expensive P2 medium ingredients. The use of CSL resulted in the production of 6.29 g/L of total acetone-butanol-ethanol (ABE) as compared with 6.86 g/L in a control experiment. These studies were performed at a dilution rate of 0.32 h⁻¹. The productivities in the control and CSL experiment were 2.19 and 2.01 g/(L·h), respectively. Although the use of CSL resulted in a 10% decrease in productivity, it is viewed that its application would be economical compared to P2 medium. Hence, CSL may be used to replace the P2 medium. It was also demonstrated that inclusion of butyrate into the feed was beneficial to the butanol fermentation. A control experiment produced 4.77 g/L of total ABE, and the experiment with supplemented sodium butyrate produced 5.70 g/L of total ABE. The butanol concentration increased from 3.14 to 4.04 g/L. Inclusion of acetate in the feed medium of the immobilized cell biofilm reactor was not found to be beneficial for the ABE fermentation, as reported for the batch ABE fermentation. Names are necessary to report factually on available data. However, the USDA neither guarantees nor warrants the standard of the product, and the use of the names by USDA implies no approval of the product to the exclusion of others that may also be suitable.     

Ultraviolet emission spectra of sunbeds

It is well known that UV radiation contributes to the development of skin cancer. Exposure to solar radiation is predominantly responsible for the high incidence rate of skin cancer, but there are also indications that sunbeds are involved. The aim of the present investigation was to determine the UV emission spectra of sunbeds. It included the most common sunbed models, which cover more than 50% of the Swiss market. The UV emission spectra of sunbeds have special characteristics and are different from the sun spectrum, which can be seen in high-resolution spectral measurements. Sunbed emission spectra are similar to the sun spectrum in the UVB (280-320 nm) range but reach values 10 to 15 times higher in the UVA (320-400 nm) range. An average erythema-effective irradiance of 0.33 W/m2 was determined for sunbeds. This corresponds to a UV index of 13, which is significantly higher than the UV index of 8.5 of the high summer sun at noon at intermediate latitudes. The measurements were spread over the whole effective area of the sunbeds, and an inhomogeneous distribution of the irradiances with variations of up to 30% from the average value was found.     

An overview of laboratory performance studies conducted by the IAEA for marine pollution studies of metals and organic contaminants

Aspects of the International Atomic Energy Agency (IAEA) Analytical Quality Control Services (AQCS) for marine environmental studies are discussed, focusing on recent laboratory performance studies (LPS) and the production of reference materials for trace metals and organic compounds in various marine matrices. The IAEA has organized seventeen global interlaboratory studies for a range of organic contaminants. Of note has been the inclusion of numerous polychlorinated biphenyl congeners (PCBs) and some sterols of anthropogenic origin. Concurrently, there have been eleven worldwide intercomparison exercises for trace metals in the marine environment, most of which included methylmercury. Although such interlaboratory studies can help improve performance in individual laboratories and regional laboratory networks, the results reveal that problems remain in the determination of some metals and many organic contaminants.     

CuSO<Subscript>4</Subscript> as a Mild,Green, and Efficient Catalyst for the One-pot Conversion of <Emphasis Type="Italic">THP</Emphasis> Ethers to Acetates

Summary. An efficient direct conversion of THP ethers into the corresponding acetates was achieved with acetic anhydride in the presence of CuSO₄ · 5H₂O as an available and green catalyst in high yields.     

Fenugreek mucilage as a flocculating agent for sewage treatment

The use of fenugreek mucilage, a natural polysaccharide and a direct food additive, as a flocculating agent for removal of suspended and dissolved solids from sewage effluent has been reported. A flocculation study has been done by the standard jar test method. The percent removal of suspended solid (SS) and dissolved solid (TDS) was determined by varying the polymer dose, pH and contact time. X-ray diffraction patterns of the solid waste material of mucilage and flocs (so obtained after treatment) were used to suggest the incorporation of the crystalline waste material in the mucilage. The optimal mucilage concentration was found to be 0.16 mg/l. The suitable pH range for maximum solid removal (SS and TDS) was alkaline and the time required for treatment was 1-3 h.     

Evaluation of measurement uncertainty for analytical procedures using a linear calibration function

In the EURACHEM/CITAC draft ”Quantifying uncertainty in analytical measurement” estimations of measurement uncertainty in analytical results for linear calibration are given. In this work these estimations are compared, i.e. the uncertainty deduced from repeated observations of the sample vs. the uncertainty deduced from the standard residual deviation of the regression. As a result of this study it is shown that an uncertainty estimation based on repeated observations can give more realistic values if the condition of variance homogeneity is not correctly fulfilled in the calibration range. The complete calculation of measurement uncertainty including assessment of trueness is represented by an example concerning the determination of zinc in sediment samples using ICP-atomic emission spectrometry. Received: 9 February 2002 Accepted: 17 April 2002