Average and local magnetic moments on Fe atoms in microcrystalline and amorphous Fe100−xPx alloys

We have measured the concentration dependence of the average magnetic moment per Fe atom _Fe(x) in microcrystalline and amorphous Fe-P alloys obtained over a wide concentration range using electrochemical deposition. The model of local magnetic moments has been used to described _Fe(x). On the basis of this model the effects of phosphorus on the value _Fe are explained in terms of the parameters of the local environment of the Fe atom.     

Déformations des algèbres de Lie locales et analogue du théorème d'algébricité de Carles

Sans résumé

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The influence of synthetic conditions on the stability of methotrexate-monoclonal antibody conjugates determined by reversed phase high performance liquid chromatography.

Methotrexate (MTX) has been convalently attached to an IgG-type monoclonal antibody (791T/36) directed to tumour-associated antigen gp72. Conjugates were synthesized by the active ester method using MTX N-succinimidyl ester at various pH values (7.5-10.5). Following purification by gel filtration, high performance liquid chromatography was used to assess the free drug or its derivatives in samples of MTX-791T/36 conjugates previously treated (or not) with hydroxylamine. Quantitative analysis, performed on a reversed phase column (pore size 300 A) with isocratic acetonitrile-sodium acetate buffer (pH 4.8) as mobile phase, indicated no detectable amount of free methotrexate in hydroxylamine-treated conjugates even six months after their preparation. Similar observations were made with conjugates, whose synthesis were performed at pH greater than or equal to 10. In contrast, the presence of increasing amounts of drug/metabolite could be demonstrated in samples produced at lower pH values. Based on these findings, the pH-dependent kinetics of MTX release has been determined and used to design conditions under which stable MTX-791T/36 conjugates could be prepared without hydroxylamine reaction.     

Crystallographic report: Bis[bis(N,N‐dibenzyldithiocarbamato)cadmium(II)]

The centrosymmetric structure of {Cd[S₂CN(CH₂Ph)₂]₂}₂ features both bridging and chelating dithiocarbamate ligands so that a square pyramidal S₅ coordination geometry results. Copyright © 2004 John Wiley & Sons, Ltd.     

An estimation of the measurement uncertainty for an optical emission spectrometric method

 A validation procedure based on the ISO/IEC 17025 standard was used to demonstrate the long-term stability of a calibration process and to assess the measurement uncertainty of a standard test method for optical emission vacuum spectrometric analysis of carbon and low-alloy steel (ASTM E 415–99a). The validation was used to provide documented evidence that the selected method fulfils the requirements and that the method is ”fit for purpose”. A test for drift was applied to determine statistically whether the analytical results vary systematically with time. The accuracy and traceability of the optimised method were tested by an analysis of closely matched matrix certified reference materials (CRMs). The measurement uncertainty estimations took account of the precision study, the bias and its uncertainty, and the qualification of uncertainties not considered in the overall performance studies. Received: 2 November 2002 Accepted: 2 January 2003 Acknowledgement The author expresses gratitude to Dr. Aleš Fajgelj for helpful discussions during the 3rd Central European Conference on Reference Materials and Measurements. Presented at CERMM-3, Central European Reference Materials and Measurements Conference: The function of reference materials in the measurement process, May 30–June 1, 2002, Rogaška Slatina, Slovenia Correspondence to T. Drglin     

Dynamics of the surface layer in cyanobiphenyl-aerosil nanocomposites with a high silica density

Composites were prepared from an aerosil and 4-n-alkyl-4'cyanobiphenyls with five to eight carbon atoms in the alkyl chain. Their high silica density of ∼7 g aerosil in 1 cm³ of liquid crystal (LC) allows the observation of the behaviour of a thin cyanobiphenyl layer (having nearly a monolayer structure) on the silica particles. The systems are investigated by dielectric spectroscopy (10^-2-10⁹ Hz) in a large temperature range (220-370 K). All the composites show a (main) relaxation process at frequencies much lower than the processes observed for the bulk LC that was assigned to the dynamics of the molecules in the surface layer. The temperature dependence of its characteristic frequencies obeys the Vogel-Fulcher-Tammann law, which is found to be typical for glass-forming liquids. The quasi two-dimensional character of the glass transition in the surface layer is discussed for the first time. At the nematic-to-isotropic transition temperature of the bulk, the composites show a continuous decrease of the characteristic frequencies as a function of the alkyl chain length, while the bulk LCs show the well known odd-even behaviour. The magnitude and temperature dependence of the slow relaxation process in the composites (molecules on an outer surface) agree with those of the same molecules confined to the nanopores of molecular sieves (internal surface).     

Determination of formic and acetic acids in air by piezoelectric microweighing

The quantitative and kinetic parameters of sorption of formic and acetic acids on thin films of various modifiers of piezoelectric quartz resonator electrodes are determined. Parameters of film formation on the electrodes (application procedure and thickness) are optimized. Methods for joint and separate determination of formic and acetic acids in air by piezoelectric microweighing with single- and double-sensor devices are developed.     

Thickness dependence of free‐standing thin films

Below a critical thickness, of about 60 nm, the glass transition temperature of polystyrene (PS) films decreases with film thickness, as demonstrated using free‐standing films. A geometrical model is developed here describing this phenomenon in the case of ideal (Gaussian) chains. This model, which can be considered as an application of the free volume model, assumes that the decrease of the glass transition temperature from thick to ultrathin films is due to the modification of the interpenetration between neighboring chains. The theoretical curve deduced from the model is in excellent agreement with the PS experimental results, without using any adjustable parameters. From these results, it can be concluded that new chain motions, usually buried in bulk samples, are expressed by the presence of the surface. © 2006 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 45: 10–17, 2007     

High pressure elastic and plastic deformations of silica: In situ diamond anvil cell Raman experiments

Normal silica glass is usually referred to as low density amorphous silica as it can be converted to high density amorphous silica by a hydrostatic pressure (polyamorphic transition). In this work in situ Raman experiments are performed in a diamond anvil cell up to 18 GPa. The pressure effects on the structure of silica after successive compression decompression experiments are analyzed. The mode Grüneisen parameters corresponding to the elastic compression of high density amorphous silica are obtained and compared with those of normal silica. A reorganization of the high density amorphous silica below 3 GPa is evidenced.