This unit gives scientific support to the institute’s research groups in spectroscopic techniques and methods related to the testing and characterization of solid materials, regarding their structure and chemical reactivity
The Spectroscopy and Material Characterisation Unit gives scientific support to the institute’s research groups in spectroscopic techniques (UV-Vis, FTIR, FT-Raman, Circular Dichroism and Fluorescence spectra as well as polarimetric measurements) and methods related to the testing and characterisation of solid materials (textural properties, paramagnetism, surface chemistry, DLS, pycnometry, viscosity, gases online analysis), regarding their structure and chemical reactivity.
Among other devices, the Unit has a Stopped Flow system to measure fast reaction rates in the millisecond range at different temperatures (from -90 to +100 ºC).
Moreover, the Unit trains the users in order to achieve optimal use of the instruments.
Microplate reader FLUOstar Omega. System composed by a xenon flash-lamp, wheels with 8 excitation and 8 emission filters, temperature control from ambient +5ºC to 45ºC, a reagent injector and a PMT detector. The instrument allows fluorescence and absorbance intensity measurements in the UV/Vis in microplates up to 1536-wells. Wavelength range for fluorescence: 240-740 nm. Wavelength range for absorbance: 220-850 nm.
UV-Vis-NIR spectrophotometer Lambda 1050 from Perkin Elmer. This high performance instrument has double beam optics, double monocromator and three detectors system (PMT, InGaAs and PbS) covering 175 to 3300 nm range.
Double beam UV-Vis Shimadzu spectrophotometer model UV-1800. Spectral range from 190 to 1100 nm, 1 nm fixed slit.
Double beam UV-Vis Agilent Technologies spectrophotometer model Cary 60 UV-Vis. Spectral range from 190 to 1100nm, 1.5nm fixed slit and room light immunity.
Double beam UV-Vis Shimadzu spectrophotometer model UV-2401PC with a Peltier thermostated (7-60 ºC) sample holder. Optical range from 190 to 1100 nm, variable slit.
LifeSpec II from Edinburgh Instruments. This is a compact, high performance, computer controlled spectrometer for the rapid measurement of fluorescence lifetimes based on the technique of Time Correlated Single Photon Counting. The LifeSpec II has two detectors, one standard PMT in the UV-vis range and another PMT nitrogen cooled with spectral response in the vis-NIR region from 300 to 1700nm.
Fast mixing stopped flow module Bio-Logic SFM300, with three syringes controlled independently, that allow simple or double mixing, different mixing ratios and submilisecond mixing time. The system is completed with a cryostat Huber CC3-905 VPCw (-90 ºC to +100 ºC) and a fast UV-Vis Diode Array spectrophotometer TIDAS capable of recording one spectrum in 0.8 ms.
Luminescence Spectrofluorimeter Aminco-Bowman Series 2. System composed by a continuum and a pulsed xenon lamps, four temperature-controlled cuvettes holder (20-60ºC) and a solid sample holder. Wavelength range: 250-850 nm.
Spectrofluorimeter Horiba Jobin Yvon. System composed by a continuum 450W Xenon lamp, double monochromator for excitation, a solid sample holder, detection in Right Angle or Front Face mode and absorbance measurements. The instrument allows fluorescence measurements in the wavelengths range of the UV/Vis and NIR from 250 to 1600 nm.
Dispersive Raman Spectrometer model i-Raman from BWTEK. This instrument has an excitation laser at 785nm and a fiber optic probe with a TE Cooled Linear Array detector. The resolution is 3cm-1 and the spectral range goes from 75 to 3200cm-1.
Dispersive Raman Spectrometer model i-Raman from BWTEK. This instrument has an excitation laser at 532nm and a fiber optic probe with a TE Cooled Linear Array detector. The resolution is 3cm-1 and the spectral range goes from 75 to 4000cm-1.
Polarimeter Jasco model P-1030 with simmetrical angular oscilation for the Sodium line and photomultiplier tube detector. Angular range: ± 90 º, speed better than 6 º s-1.
FTIR spectrometer Nicolet is50 from Thermo Scientific, with DLaTGS and MCT detectors, and FTRaman module with the capability of Raman mapping and well plates screening. The instrument also includes a built in ATR module with diamond crystal that allows measuring samples in the Far Infrared (up to 150 cm-1) and Middle Infra-red regions (4000-400cm-1). Spectral range in main sample compartment: 4000–400 cm-1.
FTIR Bruker spectrometer model Alpha with an ATR accessory. Spectral range from 4000 to 400 cm-1.
FTIR React IR 15 from Mettler Toledo. The instrument allows in situ reaction monitoring in the mid-infrared. Spectral range: 3000 to 650 cm-1.
FTIR spectrometer Cary 630 from Agilent technologies equipped a DLaTGs detector (4 cm-1 resolution) and a single bounce diamond ATR accessory (spectral range 650-4000cm-1). There is also a DialPath accessory for measuring liquid samples in transmission mode with selectable 30, 50 and 100 μm pathlength.
Microcalorimeter Super CRC 20-250-2.4 from Omnical Technologies to follow heat flow in chemical reactions. Temperature range from -100C to +200C, 1 microwatt sensitivity.
Porous structure of solids by gas physisorption (BET area and pore volume, pore size distribution) typically by nitrogen. Surface characterization by chemisorption.
Chemical characterisation of solids by gas flow temperature ramp experiments (TPD, TPR, TPO) and pulse chemisorption. Active sites: types, reactivity and amount. Affinity for representative probe molecules (typically NH3 and CO2).
Online analysis of gases. Up to 100 AMU. Analysis of gas streams and atmospheres. Support of other apparatus (TPDRO 1100, setups of the researchers).
Allows measuring the true or skeletal density of solids (without considering the volume occupied by pores) by gas displacement, normally helium. Precision increases with the amount of sample (ideally 0.5-2 cm3).
Malvern Light scattering (DLS) analyzer for nanoparticles and macromolecules in suspension. Hydrodynamic diameter by DLS (0.6 to 6000 nm). Zeta potential of particles between 5 and 10000 nm by DLS. Molecular weight (1 to 20000 kDa) by SLS. Effect of pH or additives on zeta potential and particle size by a titration accessory.
Allows determining the absolute viscosity and the flow behavior under different conditions of speed or shear stress and temperature.
Fluid viscosity at given shear rates.
Automated and computer-controlled laboratory reactor for catalytic testing. Up to 1000 ºC and 100 bar. Flow with up to five gases and a vapor. Programmable to work 24h/day. Exhaust gases analyzed by GC (optionally by MS).
EMX Micro spectrometer with an X-band bridge of 9.1 – 9.9 GHz. Allows acquiring spectra of both solution and powder samples for studying metal complexes or organic radicals at ambient conditions (298 K) or low temperature like 4 K (He) or 77 K (N2), in perpendicular or parallel mode. Additionally, paramagnetic compounds can be generated in situ via UV-Vis irradiation (Hg lamp 200 – 2000 nm) or external devices (LEDs).
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