Thermodynamic statistical evaluation ofS andF from ESR experimental order parameters.

Summary A statistical analytical procedure for calculating entropy (S) and Helmholtz free energy (F) from the order parameters obtained from ESR spectra of spin-labelled membranes is described. The method is here applied to some literature data. A brief discussion on the results is also reported.

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Riassunto Si descrive un metodo statistico per calcolare l'entropia (S) e l'energia libera di Helmholtz (F) dai parametri d'ordine ottenuti da spettri ESR di membrane spin-marcate. Il metodo è applicato da alcuni dati di letteratura e sono brevemente discussi i risultati ottenuti.

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Резюме Описывается статистическая аналитическая процедура вычисления энтропии (S) и свободной энергии Гельмгольца (F) из параметров порядка , полученных из ESR спектров для мембран со спиновыми метками. Развитый мэтод применяется к некоторым данным, имеюшимися в литературе. Проводится обсуждение полученных результатов.

     

Trace enrichment of polar pollutants from water and the influence of humic substances

Summary A practical liquid chromatographic early-warning system for polar pollutants in water ought to have detection limits at a level below a microgram per litre. Using ultraviolet absorbance detection this normally necessitates trace enrichment of the samples. In this study ten different sorbents have been tested with respect to their enrichment capacity. The hydrophobic polymeric PLRP-S material, in combination with a C-18 modified analytical column, proved to be the best choice. The influence of humic substances, present in surface water, was also studied. Lowering of the sample pH, resulted in a significant increase in the interferences due to the humic substances.     

Spectroscopic Analysis of a Pulsed-Laser Deposition System for Fullerene-like Cn x Film Production

Plasma produced by a (1064 nm) Nd:YAG laser focused onto a graphite target at different nitrogen pressures in the range of 1–90 mTorr, was studied spectroscopically. In the spectral range of 350–600 nm, emission lines of CI neutral carbon (501.12, and 505.21 nm), NI neutral nitrogen (493.5 nm), CII (426.72, 463.7, 515.11 nm), and CIII ions (465.02 and 569.59 nm), and NII ions (501.06, and 500.73 nm), were dominating. Bands of C₂ Swan (d³Π_g → a³Π_u, Δ ν=2, 1, 0, −1), and CN Violet (B²Σ ⁺→ X²Σ⁺, Δ ν=1, 0, −1) systems, and ionic emissions from the First Negative system N2⁺ (band head at 391.44 nm), were faintly observed under our specific experimental conditions. From the band intensities, vibrational temperature for CN and C₂ was calculated to be 1.25 and 0.31 eV at 90 mTorr, respectively. The electron density and temperature, measured by Stark broadening, assuming a local thermodynamic equilibrium (LTE), were found to be 2.1× 10¹⁷ cm⁻³ and 0.33 eV at 1mTorr, respectively. The validity of the LTE is discussed according to the results discussed. Pressure dependence shows a decrease in the vibrational temperature when nitrogen pressure increases, while the electron density and temperature increase.     

基于认识视角与认识思路的化学课堂教学*——物质的分类及转化

以解决“保存NaOH溶液的试剂瓶为什么不用玻璃塞”这一真实问题为情境,设计3个教学板块:运用分类方法认识物质、对物质进行分类、合成物质,从物质组成和物质变化的认识视角,对物质进行分类,建构分类观。依据物质分类研究同一类别物质的性质及应用,在完成知识结构化的同时,重在凝练基于物质分类及转化的认识视角和认识思路,寻找并体验陌生情境下解决复杂化学问题的突破口和思维框架,发展学生的化学学科核心素养。     

Synthesis and Characterization of Related Substances of Deferasirox,an Iron (Fe3+) Chelating Agent

Deferasirox is an orally active iron chelating agent, and during process development for deferasirox, we observed six related substances (impurities), namely deferasirox methyl ester, deferasirox salicylyl derivative, deferasirox ethyl ester, deferasirox methoxy carbonyl derivative, bis(salicyl)imide, and deferasirox-2-isomer. The present work describes the detection, origin, synthesis, and characterization of these related substances.     

Bioanalysis of pentoxifylline and related metabolites in plasma samples through LC‐MS/MS

Analytical aspects related to the assay of pentoxifylline (PTX), lisofylline (M1) and carboxypropyl dimethylxanthine (M5) metabolites are discussed through comparison of two alternative analytical methods based on liquid chromatography separation and atmospheric pressure electrospray ionization tandem mass spectrometry detection. One method is based on a ‘pure’ reversed‐phase liquid chromatography mechanism, while the second one uses the additional polar interactions with embedded amide spacers linking octadecyl moieties to the silicagel surface (C‐18 Aqua stationary phase). In both cases, elution is isocratic. Both methods are equally selective and allows separation of unknowns (four species associated to PTX, two species associated to M1) detected through specific mass transitions of the parent compounds and owning respective structural confirmation. Plasma concentration–time patterns of these compounds follow typical metabolic profiles. It has been advanced that in‐vivo formation of conjugates of PTX and M1 is possible, such compounds being cleaved back to the parent ones within the ion source. The first method was associated with a sample preparation procedure based on plasma protein precipitation by strong organic acid addition. The second method used protein precipitation by addition of a water miscible organic solvent. Both analytical methods were fully validated and used to assess bioequivalence between a prolonged release generic formulation and the reference product, under multidose and single dose approaches. Copyright © 2009 John Wiley & Sons, Ltd.     

Hydrolysis of some imidazole, benzimidazole, and 1,2,3-benzotriazole derivatives according to HPLC and NMR diffusimetry data

Hydrolysis of 1-mesylimidazole, 1-mesylbenzotriazole, and 1-tosylbenzimidazole was studied by reversed-phase HPLC and pulsed field gradient NMR diffusimetry. The hydrolysis rate constants and half reaction times were determined. The self-diffusion coefficients of the substances in aqueous solutions were measured. The reversed-phase HPLC data agree well with those of NMR diffusimetry.     

Validation of stir bar sorptive extraction for the determination of 24 priority substances from the European Water Framework Directive in estuarine and sea water

This paper describes the validation of a method for the determination of 24 priority substances from the European Framework Directive in estuarine and sea water using the new extraction technique known as stir bar sorptive extraction (SBSE), followed by thermal desorption using capillary gas chromatography-mass spectrometry. We studied linearity, detection and quantitation limits and accuracy (which includes determination of trueness and precision). Using the lack-of-fit method we tested linearity in the 0-200 ng L⁻¹ range for all the priority substances. The detection and quantification limits were less than 5 and 10 ng L⁻¹, respectively, for most of the compounds studied. Precision was assessed by variance analysis (ANOVA) and relative standard values of less than 10% were obtained for repeatability and less than 15% for intermediate precision. The recovery percentages in spiked estuarine and sea water were close to 100%. Finally, for quality control of the method (stability of precision and accuracy through time), we developed a method for calculating Shewhart control charts based on the information obtained in the validation process.     

New evidence of earthquake precursory phenomena in the 17 January 1995 Kobe earthquake, Japan

Significant advances, both in the theoretical understanding of rupture processes in heterogeneous media and in the methodology for characterizing critical behavior, allows us to reanalyze the evidence for criticality and especially log-periodicity in the previously reported chemical anomalies that preceded the Kobe earthquake. The ion (Cl^-, K⁺, Mg⁺⁺, NO₃ ^- and SO₄ ^-) concentrations of ground-water issued from deep wells located near the epicenter of the 1995 Kobe earthquake are taken as proxies for the cumulative damage preceding the earthquake. Using both a parametric and non-parametric analysis, the five data sets are compared extensively to synthetic time series. The null-hypothesis that the patterns documented on these times series result from noise decorating a simple power law is rejected with a very high confidence level. Received 21 January 2000     

无机物对淀粉塑料力学性能影响的研究进展

淀粉以其来源广、成本低、可完全降解的特点已成为制备生物可降解塑料的重要来源。近年来,淀粉塑料的研究和应用发展迅速,其核心是不断提高其各项使用性能(如力学、耐水性能等)。当前,无机或矿物填料被广泛应用于复合材料中来提高材料的性能,本文主要根据无机物的种类不同,综述了典型的氧化物、氢氧化物,以及碳酸盐、硅酸盐、磷酸盐等盐类对淀粉塑料力学性能的影响,归纳了近期的研究成果,分析了该领域研究的热点和难点,并对今后的发展趋势提出了展望。