X-Ray Diffraction (XRD) provides information concerning crystallographic phases and structure, cell parameters, crystallites preferential orientation, residual stress&strain and dimension.
Philips X’ Pert PW 3710 operates with Bragg-Brentano geometry, using Cu Kα (λ=1.54056Å, 40kV, 30 mA). Samples can be analysed as powder or thin film. In detail, the analysis of thin film is carried out under grazing incidence, thus allowing a lower sampling depth of the X-rays and so maximizing the intensity reflections deriving from the film.
- Philips X’ Pert PW 3710 diffractometer
The Nuclear Magnetic Resonance spectroscopy allows to outline the chemical structure of a molecule, to draw the bonds and arrange the atoms that compose it. This, together with other techniques, is the basis for structural characterization of organic and inorganic molecules and is the principal analysis tool for the chemicals. IENI-CNR lab hosts a high-performance digital spectrometer Bruker Avance III 300 MHz, configured for the analysis of liquids (probe head for liquids) and solids (probe head for solids).
The use is oriented in the following areas:
determination of the molecular structure of various compounds in the field of i) organic, organometallic and inorganic synthetic chemistry, ii) chemistry of materials and natural products.
study of dynamic processes i) reaction kinetics, ii) study of equilibrium (chemical or structural).
Typically, the analyzed samples are solutions at millimolar concentrations in suitable deuterated solvents (liquid probe) or powders as is, to fill a 4mm diameter rotor (solid state probe). 1D and 2D acquisition techniques are commonly used with direct or inverse observation of the nuclei involved (typically 1H, 13C, 31P, 11B, 19Ag, 23Na, 29Si, 27Al etc). The expertise currently available in the field of materials include: the study of raw materials and products in geopolymerization processes; the study of natural clays; the study of high performance cements; the analysis of polymers and composite materials. In the field of synthetic chemistry include: identification of synthesized organic and complexes molecules (with transition metals or not); identification and validation of unknowns; determination qualitative and quantitative of impurities in pharmaceutical preparations; determination of 'fingerprint' in complex mixtures of extracts of natural products.
Bruker Avance III 300 MHz
- Avance III 300MHz spectrometer with Ultra Shield magnet
- 2 indipendent RF channels with 100 Watt for 1H-19F / 300 Watt 31P-15N amplificators
- Digital Temperature Control BSVT -200°C +400°C
- Z field gradient spectroscopy (accessory GRASP II: 10 A amplificator)
- Probehead BBI 5mm with Z grad 1H-13C-15N - 1H high sensitivity
- Probehead BBFO 5mm with Z grad 1H-13C-15N; 1H and13C high sensitivity with automatic tuning and matching.
- Multinuclear probehead CP-MAS 4mm 1H/31P-15N spinning speed up to 15KHz
- Pneumatic unit MAS
Spectroscopic analysis is based on the matter-electromagnetic radiation interaction. UV-Vis spectroscopy operates with ultra-violet and visible radiation, thus allowing electronic transitions in the investigated samples. The matter-radiation interaction result is collected as a spectrum in which the physical quantity (absorbance, transmittance or reflectance) is displayed as a wavelength function. UV-Vis Spectroscopy allows both qualitative and quantitative (detection limit is in the micro-molar range, as a function of the investigated compound) measurements.
The Spectronic Unicam spectrophotometer can operate both on solution and solid samples (thanks to the reflectance mode device).
- Spectronic Unicam UV-Vis spectrophotometer
The laboratory is equipped with a Thermo-Nicolet IS10 spectrophotometer coupled with Continuum microscope. The instrumentation allows the collec-tion of transmission spectra in the 4000-400 cm-1 wavenumber range and the micro-analysis of small samples (after an easy sample adapting). Thanks to the spectrophotometer-microscope cou-pling, reflection and/or transmission analysis can be carried out on sample surface (until 100μm2) be-tween 4000 and 650 cm-1. Two micro-ATR (Attenu-ated Total Reflection) devices (in Silicon or Germa-nium crystals) are also available. These allow the direct analysis of the sample surface with 2-3 μm sampling depth.
The laboratory is also equipped with a Bruker Alpha potable spectrophotometer. This allows in situ, not invasive analysis in external reflecting mode in the range 7000-400 cm-1.
- FT-IR Thermo-Nicolet IS10
- Materials for energetics
- Materials and devices for heat recovery and energy efficiency
- Structural materials and coatings for nuclear and aerospace applications, gas turbines and energy processes
- Materials and technologies for renewable energies, fuel cells and hydrogen
- Electrochemistry of materials for catalysis, electrocatalysis, sensors and energetics
- Modeling and computational methods to study energy systems
- Advanced manufacturing
- Molecular systems and nanomedicine
- Materials for energetics
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