Anodic Stripping Voltammetry of Heavy Metals at Nanocrystalline Boron‐Doped Diamond Electrode

Boron‐doped Diamond (BDD) electrode has become one of the important tools for heavy metal detection. By studying some analytical parameters of DPASV method, like deposition time and potential in different electrolyte concentrations (acetate buffer), the conditions for detecting very low metal ion levels (Zn, Cd, Pb, and Cu) could be chosen. Diluted electrolyte (0.01 M buffer) was one of the factors favoring low detection and quantification limits, but its quantification range is short in comparison to more concentrated media. For ?1.7 V deposition potential, the detection of single metal at ppb levels was reached in 60 s deposition time. Understanding different metal‐metal interactions shows the limits to the simultaneous determination of heavy metals at BDD. Quantification was possible for the simultaneous determination of Zn, Cd and Pb despite the overlapping of Zn and Cd peaks. The performance of the BDD was compared with that of another C‐based solid electrode: the glassy carbon electrode (without mercury plating). A lower base line current, wider potential range, higher sensitivity (3 to 5 times higher than GC) and longevity of the material were noticed for the BDD.     

Ungewöhnliche Bildung und Struktur eines O‐Sulfinato‐Zinkkomplexes

Unusual Formation and Structure of a O‐Sulfinato Zinc Complex Whereas the reaction between hydrotris[(N‐xylyl)‐thioimidazolyl]borato‐zinc perchlorate ([ L· Zn‐OClO₃]) and ethanethiolate under an inert atmosphere leads to the thiolate complex [ L· Zn‐SC₂H₅], the same reaction in air produces the sulfinato complex [ L· Zn‐O‐S(O)‐C₂H₅] ( 1 ). 1 is the first fully characterized sulfinato‐zinc complex. Its structure determination has confirmed the unusual coordination of the sulfinato ligand via one of its oxygen atoms.     

Development of the FTIR properties of nano-structure silica gel doped with different rare earth elements,prepared by sol-gel route

Structural characteristics of pure silica gel (silica-xerogel, SiO₂) and silica gel doped with some rare earth elements (REEs) such as, praseodymium Pr³⁺, and Europium Eu³⁺, Erbium Er³⁺ and Holmium Ho³⁺ ions, with different concentrations ranging from 1 up to 6%, in the form of monolith materials were prepared by sol-gel technique, Using tetra-ethoxysilane as precursor materials, which are of particular interest for sol-gel integrated optics applications. Some structural features of sol-gel derived monolith are analyzed, namely the structure of nano-particle momolith samples, based on X-ray diffraction (XRD) and Fourier Transform Infrared (FTIR). We show that the XRD spectra of α-crystobalite are obtained for the pure samples at 1100°C and even by doping with the four REEs ions.     

Loganin,loganic acid and periclymenoside,a new biosidic ester iridoid glucoside from Lonicera periclymenumL. (Caprifoliaceae)

Loganin ( 1 ), loganic acid ( 2 ), and periclymenoside ( 3 ) have been isolated from Lonicera periclymenum L . The structure of the new compound 3 and the identity of the others have been determined by chemical transformations and interpretation of the spectral data.     

Ylures sans sel,evolution en phosphoranes et equilibre ylure ⇌ phosphorane : I Synthese et structure

Synthesis of new salt-free ylids $\text{9}$,$\text{12}$ to $\text{16}$, $\text{19}$, $\text{20}$, $\text{22}$, $\text{27}$ and $\text{29}$ and phoiphoranes $\text{10}$, $\text{17}$, $\text{18}$, $\text{21}$, $\text{23}$, $\text{30}$ to $\text{33}$ by addition of a trivalent phosphorus compound (phosphites and amino-phosphines ) $\text{1}$ to $\text{7}$ with dimethyl acetylencedicartboxylate in presence of a protic trapping reagent are described. The results are consistent with trapping of carbanionic species. In relation with the. cyclic of acyclic structure of the triivalent phosphorus compound and the protic trapping reagent ie : methanol, phenol, carboxylic acid, etc.., several pathways are involved. Clearly), three phenomena are shown : one can obtain an ylid via a phosphorane or conversely a phosphorane via an ylid or an equilibrium Phoiphorane ? ylid. Results are dealing with thermodynamic or kinetically controlled reactions.     

Heterocycles from carbohydrate precursors. Part XIX. The X-ray crystal structure determination of the reaction product of 4-(2-acetoxyethylidene)-4-hydroxy-2,3-dioxobutyro-1,4-lactone-2-(p-bromophenylhydrazone) with methylhydrazine

X-ray crystallographic data show that the product obtained in the reaction of 4-(2-acetoxy-ethylidene)-4-hydroxy-2,3-dioxobutyro-1,4-lactone-2-(p-bromophenylhydrazone) with methyl-hydrazine is the bicyclic compound 2,6-dimethyl-3,4-dioxo-2,3,4,6,7,8-hexahydropyridazino-[4,3-c]pyridazine 4-(p-bromophenylhydrazone) ( 10 ) and not as originally suggested 1-methyl-3-(1-methylpyrazolin-3-yl)-4,5-pyrazoledione 4-(p-bromophenylhydrazone) ( 8 ).     

Solvation numbers and hydration constant for thorium(IV) in ethanol-water medium

The solvation number and hydration constant of Th⁴⁺ in ethanol-water medium were determined at 25°C using UV-spectral and electrochemical measurements. A solvate formation equilibrium is demonstrated and characterized. Three molecules of ethanol (S) can bond to the metal cation with strengths comparable to that for H₂O to form ThS₃(H₂O) ₃ ⁴⁺ Formation of thorium monochelate with lawsone (2-hydroxy-1,4-naphthoquinone) eliminates bonding with alcohol molecules. The dissociation constant of the chelating agent_sK_a and the formation contant of the monochelated metal ion_sK _f ^* that are essentially independent of the solution composition are evaluated. Hydration titrations involving thorium-lawsone monochelate are performed and the data obtained from the changes of pH with solvent composition are analyzed. The solution independent constant,_sK _f ^* for thorium-lawsone complex formation in mixed aqueous ethanol is given by $$log_s K_f * = vpK_a + log_s K_h - log[LH] - vpH + 3logv$$ where vpK_a is the dissociation constant of the chelating agent LH in the solvent system of ν volume fraction of water and_sK_h is the solution-independent hydration constant of thorium (IV) in the solvent system. Log-values for the constants_sK_h,_sK _f ^* and_sK _a ^* are found to be 7.8±0.02, 11.38±0.04 and ?0.753, respectively.     

Recoil spectrometry: Ion accelerator based elemental characterisation of surface layers

Recoil Spectrometry covers a group of techniques that are very similar to the well known Rutherford backscattering Spectrometry technique, but with the important difference that one measures the recoiling target atom rather than the projectile ion. This makes it possible to determine both the identity of the recoil and its depth of origin from its energy and velocity, using a suitable detector system. The incident ion is typically high-energy (30–100MeV)³⁵C1,⁸¹Br or¹²⁷I. Low concentrations of light elements such as C, O and N can be profiled in a heavy matrix such as Fe or GaAs. Here we present an overview of mass and energy dispersive recoil Spectrometry and illustrate its successful use in some typical applications.     

Fractal analysis of hydroxyapatite from nitrogen isotherms

Samples of calcium hydroxyapatite, CaHap, were prepared via a wet method and subjected to thermal treatment in air in the temperature range 100-900 degrees C. Nitrogen adsorption-desorption isotherms were obtained on different samples, and their data points were used to analyze the fractal properties of the obtained solids. Both FHH and Neimark's equations were used for such purpose, and the agreement or disagreements between obtained results on using both equations are discussed. Considering the appropriate values of the obtained surface fractal dimensions D, it was concluded that an appreciable defractalization of the prepared hydroxyapatite is only noted upon calcinations at 900 degrees C. Below this temperature the loss in surface area and pore volume result from simultaneous bulk and surface mass transport, which conserve the initial surface roughness and average pore radius. Calcination at 900 degrees C caused sintering to proceed via bulk mass transport, with a consequent pore widening and a decrease in surface roughness.