Sequential Voltammetric Determination of Uranium,Cadmium and Lead by Using the ex situ Bismuth Film Electrode: Application to Phosphate Fertilizers

A sequential voltammetric procedure for the determination of uranium, cadmium and lead was investigated at an ex situ bismuth film electrode (BiFE). First, the adsorptive stripping voltammetry was applied to assay the U(VI)‐cupferron complex in the differential pulse mode (detection limit of 1.0 µg L^?1, 200 s accumulation time). Through the manipulation of the same aliquot of the sample, efforts were made to quantify cadmium and lead by square wave anodic stripping voltammetry. Detection limits of 2.03 µg L^?1 for Cd (II) and 2.43 µg L^?1 for Pb (II) were calculated (100 s accumulation time). The methodology was successfully applied to phosphate fertilizer samples after open vessel wet decomposition (HNO₃/H₂O₂). The following value ranges were evaluated: U (VI) 37.2–150 mg kg^?1, Pb (II) 78.3–204 mg kg^?1 and Cd (II) 44.1–71.6 mg kg^?1. Validation was performed by using the standard reference materials SRM‐695 – phosphate fertilizer – and SRM‐1643e – water.     

Revealing Phosphorus Nitrides up to the Megabar Regime: Synthesis of α′-P3N5, δ-P3N5 and PN2

Non-metal nitrides are an exciting field of chemistry, featuring a significant number of compounds that can possess outstanding material properties. These properties mainly rely on maximizing the number of strong covalent bonds, with crosslinked XN₆ octahedra frameworks being particularly attractive. In this study, the phosphorus–nitrogen system was studied up to 137 GPa in laser-heated diamond anvil cells, and three previously unobserved phases were synthesized and characterized by single-crystal X-ray diffraction, Raman spectroscopy measurements and density functional theory calculations. δ-P₃N₅ and PN₂ were found to form at 72 and 134 GPa, respectively, and both feature dense 3D networks of the so far elusive PN₆ units. The two compounds are ultra-incompressible, having a bulk modulus of K₀=322 GPa for δ-P₃N₅ and 339 GPa for PN₂. Upon decompression below 7 GPa, δ-P₃N₅ undergoes a transformation into a novel α′-P₃N₅ solid, stable at ambient conditions, that has a unique structure type based on PN₄ tetrahedra. The formation of α′-P₃N₅ underlines that a phase space otherwise inaccessible can be explored through materials formed under high pressure.     

Side-chain chlorination of methylquinolines

Methylquinolines 1–4 were chlorinated by heating with phosphorus pentachloride in chlorobenzenes to side-chain halogen derivatives 5–14 . Methyl groups of compounds 1–4 can be chlorinated to chloromethyl, dichloromethyl or trichloromethyl groups depending on their positions and the reaction conditions.     

Fused 1,2,4-triazole heterocycles. IV. Synthesis of four new heterocyclic ring systems of [1,2,4]triazolo[1,3]thiazinoquinolines

Syntheses of 5H-[1,2,4]triazolo[5′,1′:2,3][1,3]thiazino[5,4-c]quinolines 8, 5H-[1,2,4]triazolo[3′,4′:2)3][1,3]thiazino[5,4-c]quinolines 9, 5H-[1,2,4]triazolo[5′,1′:2,3][1,3]thiazino[5,6-c]quinolines 14 and 5H-[1,2,4]triazolo[3′,4′:2,3][1,3]thiazino[5,6-c]quinolines 15 are described starting from 4-chloro-3-chloromethylquinaldine (4) and 1,2,4-triazole-5-thiols 5 taking advantage of different reactivity of the chlorine atoms of 4 under different reaction conditions. The structures of products 8, 9, 14 and 15 and the intermediates leading to them were confirmed by desulfurization, unequivocal syntheses and nmr spectroscopy as well.     

Torsional Line Splittings in the (ν4+ν8)−ν4 Hot Transitions of C2H6 between 1400 and 1510 cm

A detailed investigation of the high-resolution infrared spectrum of ethane revealed the occurrence of features belonging to the hot perpendicular system (ν₄+ν₈)−ν₄ between 1400 and 1510 cm⁻¹. Transition lines of the subbranches with K″ΔK from −7 to 4, exhibiting torsional splittings of several tenths of a cm⁻¹, were observed and measured in this region. The observed line splittings are strongly influenced by the interaction between the ν₄+ν₈ and 2ν₄+ν₁₂ states and change with the values of K″ΔK, depending on the zero-order energy separation of the interacting levels. We found by numerical extrapolation that splittings still occur far from resonance, showing that the intrinsic torsional splittings of the combining states ν₄+ν₈ and ν₄ are quite different. We determined the intrinsic torsional splitting of ν₄+ν₈ to be less than 0.083 cm⁻¹, compared with 0.236 cm⁻¹ estimated for the ν₄ state. This result is in agreement with the expected effects of torsional Coriolis and head-tail coupling and is consistent with previous observations on vibrationally degenerate states of ethane-like molecules.     

Influence of attenuation on the behavior of refracted elastic waves at the interface between anisotropic media

During the ultrasonic non-destructive evaluation of complex materials, like multilayer or composite materials, the behavior of the ultrasonic waves at the interface of samples is strongly dependent upon the anisotropy as well as the attenuation characteristics of the propagation media. In the generally arbitrary case, the incident wave is assumed to be inhomogeneous. Therefore the application of the Snell-Descartes laws requires to consider the real as well as the imaginary parts of all the quantities encountered during the study. In that aim, we use a representation of the complex slowness curves so-called slowness interface curves which point out the evolution of the interaction of the waves at the interface with the inhomogeneity factors, i.e. the imaginary part of the slowness vectors. The continuous distortion of the curves with the inhomogeneity factor increasing is an interesting approach of these complicated phenomena.     

一种交互式自动挖掘知识的模型

提出一种交互式自动挖掘知识的模型,论述了该模型的原理、实现机制,并讨论了模型中数据宝藏和影响域及其相互关系．该模型同时具有在线性与深入挖掘的优点,能灵活有效地满足实际应用的需求．     

k—Very Ample Line Bundles on Del Pezzo Surfaces

A k-very ample line bundle L on a Del Pezzo Surface is numerically characterized, improving the results of Biancofiore— Ceresa in [7].     

Bestimmung geringer Mengen Phenol-2,4-disulfons?ure neben Phenol-4-sulfons?ure

Ohne Zusammenfassung

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Determination of minute amounts of phenol-2,4-disulphonic acid in the presence of phenol-4-sulphonic acid