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Infrared Spectroscopy Laboratory

Laboratorio n.

25

Infrared Spectroscopy Laboratory

Topic

FV6A8507

The laboratory is equipped with measurement systems based on optical spectroscopy, such as infrared absorption spectroscopy (FTIR) and Raman spectroscopy for the characterisation of materials of different natures, both solid (catalysts, polymers, membranes, organic films, foils, sensors) and liquid (solutions, reaction mixtures). In particular, the IR spectrometer is able to work in different modes being equipped with dedicated modules and measuring cells including ATR (attenuated total reflectance) multi-reflection, DRIFT (diffuse reflectance in Fourier transform), SMART ARK Flat Plate.

  • In situ/operando spectroscopic investigations are a fundamental tool for the qualitative and quantitative determination of the active sites of catalytic systems and transient species taking part in chemical reactions. Such measurements are possible through the use of the TPR cell Praying MantisTM Diffuse Reflection accessory, equipped with an environmental chamber operating in DRIFT to study the reaction kinetics of catalytic reactions in operando, over a wide range of temperature (25-900 °C) and pressure (1-30 bar).
  • In situ measurements are carried out to investigate surface properties and identify active sites functional to the catalytic pathway using quartz cells for adsorption of probe molecules (pyridine, ammonia, methanol, …).
  • Transmission quartz cells also allow the study of moisture on polymeric samples.

The potential of the laboratory is amplified by the possibility of conducting measurements with hyphenated techniques, such as IR-MS, IR-TGA or TGA-MS. The IR reaction cell is directly connected to a gas management system for the use of pure gases and mixtures supplied with different volumetric flow rates and variable reaction pressures. The mass spectrometer connected with the IR cell also makes it possible to monitor the evolution of the gaseous reaction products and to carry out their qualitative-quantitative analysis. The purpose of thermo-gravimetric analysis combined with infrared spectroscopy (TGA/IR) is to determine the variation of the mass of a sample as a function of temperature under controlled atmosphere conditions (inert, reducing or oxidising) and to analyse the physical changes undergone by the sample during heat treatment. Simultaneous measurement of heat flux (DSC) and mass change (TGA) is possible by using modulated techniques for determining heat capacity and increased productivity, while also evaluating the activation energy of chemical steps using models associated with high-resolution TGA measurements. Thermodynamic transitions, thermal stability or decomposition paths can be detected and quantified as a function of heat treatment. Finally, the availability of a state-of-the-art confocal Raman microscope makes it possible to obtain information on both the chemical nature of materials and the structure and interactions between chemical species. Raman observation enables the identification, mapping, imaging and chemical analysis of polymeric, organic and inorganic materials, being fundamental for the characterisation of carbon-based materials such as graphite, nanotubes and fullerenes.

Apparecchiature presenti

  • 1 IS50 IR spectrometer (ThermoFisher Scientific) equipped with an MCT-A detector and various accessories:
  1. ATR multibounce module for measurements on solids, liquids, pastes and gels, integrated with dedicated detector for extension in the FAR-IR
  2. DRIFT module (diffuse reflectance)
  3. Smart ARK Flat Plate with a 45° flat crystal
  4. Transmission Cells
  5. TPR cell module Praying MantisTM Diffuse Reflection Accessory (HR-DRP-BR3) equipped with Praying MantisTM High Temperature Reaction Chamber (HR-HVC-DRM-5) with interchangeable dome for pressures from 1.33mPa to 3.44MPa and temperatures up to 910 °C.
  • 1 DX3 confocal Raman microscope with spatial resolution down to 0.5 microns for non-destructive, non-invasive analysis of a sample on a single point or in confocal mode. Equipped with laser source with different excitation wavelengths (532 nm and 785 nm) and 4 objectives (100x-50x, 20x, 10x) that can be coupled with cells for measurements under controlled temperature and conditions.
  • 1 HPR-20 (Hiden) RD Research bench-top grade mass spectrometer for gas phase analysis equipped with triple filter and Faraday/Multiplier detector. It is also equipped with a corrosion-resistant system for applications requiring the analysis of corrosive gas mixtures.
  • 1 TGA-DSC thermobalance (Discovery SDT 650 – Simultaneous DSC-TGA Instrument) for thermal analysis in air or inert gas flow in the range 40-1040 °C. The horizontal double-arm design can use the following measurement modes:
    1. Double mass signal to analyse two samples at the same time (dual sample TGA) or double the sample quantity in order to improve the sensitivity of FTIR and MS measurements;
    2. Heat flow (DSC measurement) with reference and measuring crucible;
    3. Single TGA mode with high dynamic resolution and continuous scan rate control;
    4. Modulated TGA mode for kinetics, activation energy, increased separation of superimposed phenomena in both TGA and DSC.

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