Size Determination of Porosity Inclusions in an Organic Solid Material by (1)H NMR Diffusion and SEM-FIB Experiments: The TATB Case.

An original approach has been presented to characterize the local geometry of pores containing protonated small molecule impurities in organic materials. It was here applied in TATB (1,3,5-triamino-2,4,6-trinitrobenzene) powder material to investigate the porosity able to enclose water molecules. The presence of such defects may have a significant impact on TATB-based compositions mechanical properties, efficiency, and shock sensitivity.

Electrochemical detection of nitromethane vapors combined with a solubilization device.

During the past decade, the number of terrorism acts has increased and the need for efficient explosive detectors has become an urgent worldwide necessity. A prototype, Nebulex™, was recently developed in our laboratory. Basically, it couples the solubilization of an analyte from the atmosphere by a nebulization process and in-situ detection.

Sensitivity improvement of 1H-15N cross-polarization at high MAS frequency applied to NMR structural characterization of organic solids.

(15)N CP/MAS solid state NMR should be a method of choice to obtain essential structural information on organic materials containing nitrogen atoms. However, the technique is generally not selected for the characterization of non-labelled chemical compounds, which represents the most common situation encountered by chemists. Actually, due to the poor sensitivity of (15)N the method is time-consuming and a very fine calibration is often a prerequisite to reach a sufficient signal/noise.

Design of interpenetrated networks of mesostructured hybrid silica and nonconductive poly(vinylidene fluoride)-cohexafluoropropylene (PVdF-HFP) polymer for proton exchange membrane fuel cell applications.

Organic-inorganic hybrid membranes of poly(vinylidene fluoride)-cohexafluoropropylene (PVdF-HFP) and mesostructured silica containing sulfonic acid groups were synthesized by using the sol-gel process. These hybrid membranes were prepared by in situ co-condensation of tetraethoxysilane and an organically modified silane (ormosil) by a self-assembly route using organic surfactants as templates for tuning the architecture of the hybrid organosilica component. In this paper, we describe the elaboration and characterization of hybrid membranes all the way from the precursor solution to the evaluation of the fuel cell performances.

(1)H, (13)C and (15)N NMR spectral assignments for new triazapentalene derivatives.

Mesomeric heteropentalene betaines are conjugated fused polyheterocyclic structures that represent interesting intermediates for organic synthesis. Five such structures, containing at least four nitrogen atoms and various substituents, have been characterized by (1)H, (13)C and (15)N NMR. We report, apparently for the first time, nitrogen NMR data and coupling information on such systems.

Restricted diffusion and exchange of water in porous media: average structure determination and size distribution resolved from the effect of local field gradients on the proton NMR spectrum.

NMR Pulsed field gradient measurements of the restrained diffusion of confined fluids constitute an efficient method to probe the local geometry in porous media. In most practical cases, the diffusion decay, when limited to its principal part, can be considered as Gaussian leading to an apparent diffusion coefficient. The evolution of the latter as a function of the diffusion interval yields average information on the surface/volume ratio of porosities and on the tortuosity of the network.

Diffusive diffraction measurements in porous media: effect of structural disorder and internal magnetic field gradients.

Pulsed Field Gradient NMR (PFG-NMR) method used to measure the self-diffusion coefficient of liquids can also be exploited to probe the local geometry of porous media. In most practical cases, the measured diffusion attenuation is generally Gaussian and can be interpreted in terms of an apparent diffusion coefficient. Using well chosen experimental conditions, a so called "diffusive diffraction" phenomenon can be observed in the diffusion curve with a specific shape and maxima location characteristic of the system local dimensions.

Spectral assignments for 1H, 13C and 15N solution and solid-state NMR spectra of s-tetrazine and dihydro-s-tetrazine derivatives.

Tetrazine-based organic species are interesting intermediates for organic synthesis and represent a source of new materials bearing specific properties with potential applications in biology and material science. 1H, 13C, 15N NMR measurements carried out in solution and in the solid-state have been used to characterize a series of 3,6-disubstituted 1,2,4,5-tetrazine/dihydrotetrazine new derivatives. Experimental results presented here provide data for the assignment of 15N chemical shifts including new organic small molecules; two polymers having the tetrazine ring in the main chain and several previously published compounds.

Tautomerism and 1H, 13C and 15N NMR spectral assignments of some nitro derivatives of malonic acid diamide.

Because of its reactivity, malonic acid diamide (1) was initially identified as an alternative precursor for the development of a new class of high-density insensitive energetic materials possessing low sensitivity to thermal decomposition and detonation by impact. Nitration of 1 was studied under different conditions and led to three different tautomeric forms (2-4) of nitromalonic acid diamine. Using stronger oxidation conditions the oxadiazole 5 was generated in one step.