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Electron diffraction

The XtaLAB Synergy-ED electron diffractometer, facilitates a smooth transition from data collection to the determination of three-dimensional molecular structures. It is the fruit of innovative collaboration aimed at amalgamating our fundamental technologies: Rigaku’s rapid and highly sensitive electron detector (HyPix-ED), and a cutting-edge instrument management and single crystal analysis software platform (CrysAlisPro for ED), with JEOL’s extensive expertise and market leadership in the design and manufacturing of transmission electron microscopes. The integrated electron diffractometer ensures an uninterrupted workflow from data gathering to the interpretation of 3D molecular structures. This equipment has the capability to examine nano-crystalline samples, thanks to the electron diffraction’s prowess in measuring crystals that are just hundreds of nanometers or less in size. This scale is thousands of times smaller than what can be analyzed using a synchrotron. This apparatus has the capacity to function over a broad temperature spectrum, from 100 K to 1000 K. The technique offers numerous features, including the ability to perform in situ crystallization, absolute structure elucidation, and powder diffraction, among others.

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Energy Lab

The ICIQ's Energy Laboratory aims to analyze the products derived from CO2 reduction. The gaseous products of this reaction can be analyzed online or offline using gas chromatography. On the other hand, the products of the reaction in the liquid phase of the reaction can be analyzed by means of ion chromatography. The laboratory also makes available to users potentiostats for use in electrochemical reactions and the supply of the necessary gases.

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Glass blowing workshop

The ICIQ Glass Blowing Workshop is dedicated to the design, manufacture and repair of glass pieces, with the ability to work with borosilicate glass.

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Mechanical workshop

The ICIQ Mechanical Workshop works on the design and manufacture of a wide range of pieces, with the ability to work with different materials such as plastics, resins, metals or ceramics. Likewise, it also offers designs and assemblies of setups for specific purposes.

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Chemical reaction technologies

The Chemical Reaction Technologies Unit makes available to the user a wide range of techniques to carry out chemical reactions under different conditions (high pressure, microwaves, flow reactions, photochemistry), enables the scaling up of reactions, and offers non-intrusive techniques for monitoring reactions in situ. At the same time, the Unit also offers the use of a clean room, a laboratory prepared to carry out photosensitive reactions and two laboratories to carry out reactions under pressure (up to 80 bar) equipped with reactive gases in line and all the necessary safety systems.

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HTE – High throughput experimentation

The High Throughput Experimentation (HTE) laboratory is dedicated to running a large number of reactions and analyzing them in a short period of time with the intention of accelerating the discovery processes; discovery of new reactions, new products or new reaction conditions. The facility is configured to run different types of reactions in 24- or 96-well plates, including those that are air-sensitive, reactions with reactive gases, photochemical reactions or reactions under pressure conditions. In addition, the Laboratory has a large number of reagents, solvents, metals and ligands to carry out the reactions. Regarding the analysis of the reactions, the laboratory is equipped with state-of-the-art chromatographs.

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Photophysics

The Photophysics Unit supports basic and applied research on light-induced physicochemical processes, such as luminescence, electron transfer, and energy transfer, in solution and solid state samples.

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Spectroscopy and characterization of materials

The High Resolution Mass Spectrometry Unit (HRMS) offers access to state-of-the-art mass spectrometry instruments capable of characterizing the wide range of compounds that are usually of interest to the Institute. The apparatus includes most of the ionization options, introduction of chromatographic samples and techniques that are necessary to solve problems of mass spectrometry in chemistry. In addition to the characterization of pure samples, the unit also supports research projects that depend more on mass spectrometry experiments, such as mechanical studies, intermediate identification, characterization of impurities or biochemical applications. In addition, the Unit offers a comprehensive training to guarantee an optimal use of the installations and an adequate interpretation of the data.

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Chromatography, thermal and electrochemical analysis

The Chromatography, Thermal and Electrochemical Analysis Unit offers technical and scientific support in the following techniques: Chromatography is the main technique of the unit. It supports the separation, identification and isolation of chiral and non-chiral compounds. In terms of liquid chromatography, the unit has four high-performance liquid chromatographs, two analytical HPLCs equipped with a diode array, fluorescence, evaporative light scattering and single quadrupole mass detectors, a semi-preparative HPLC ( up to 40 ml / min) and a preparation (up to 40 ml / min). 150 ml / min), both equipped with UV-vis double wavelength detectors. In terms of gas chromatography instrumentation, the Unit has three GCs, two of which are coupled to a selective mass detector and one to flame ionization and thermal conductivity detectors. The thermal analysis instrumentation consists of a differential scanning calorimeter (DSC) and a thermobalance (TG). The main applications are measurements of solid phase transitions within the range -80ºC to 600ºC (DSC) and determination of volatile compounds (MS coupling) and / or thermal decomposition (TG) in the range from room temperature to 1000ºC. An isothermal microcalorimeter (ITC) titrator is also available in this unit. The ITC is used for accurate determinations of binding constants, coordination stoichiometry, and thermodynamic values. The electrochemical instrumentation consists of two titrators (Karl Fischer and potentiometric) and two potentiostats. The main applications are the determination of the water content, acid constants (pKa) and redox processes (voltammetry, electrolysis, etc.). In addition, the unit’s technicians manage open-use instrumentation, such as gloveboxes and solvent purification systems.

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High resolution mass spectrometry

The High Resolution Mass Spectrometry Unit (HRMS) offers access to state-of-the-art mass spectrometry instruments capable of characterizing the wide range of compounds that are usually of interest to the Institute. The apparatus includes most of the ionization options, introduction of chromatographic samples and techniques that are necessary to solve problems of mass spectrometry in chemistry. In addition to the characterization of pure samples, the unit also supports research projects that depend more on mass spectrometry experiments, such as mechanical studies, intermediate identification, characterization of impurities or biochemical applications. In addition, the Unit offers a comprehensive training to guarantee an optimal use of the installations and an adequate interpretation of the data.

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X-ray diffraction

The X-ray Diffraction Unit collects all the techniques that are based on X-ray diffraction on crystalline solids. It supports the characterization of chemical compounds that are available in crystalline state. There are two main techniques available: powder X-ray diffraction (PXRD) and single crystal X-ray diffraction (SCXRD). The PXRD technique is basically used as a primary screening method and offers a fingerprint of each different crystalline form analyzed. This method provides a basic service to all ICIQ users with a system that allows easy sample preparation and short measurement time for a large number of samples. The SCXRD technique offers a three-dimensional atomic-scale structure of a selected crystalline compound. This method is highly specialized with a combined system from high performance components. The aim in this case is to give direct support to research groups by solving problems at all levels of difficulty. This support includes crystallization of problematic samples, preparation of poor quality crystals, and refinement of worrying data sets.

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Nuclear magnetic resonance

The Nuclear Magnetic Resonance (NMR) Unit provides researchers with access to a wide range of NMR experiments both under automation or manual mode. It also advises researchers on the most appropriate experiment to their needs and it trains and instructs researchers in using NMR, what information can be obtained from NMR experiments and how to optimize the instrumental resources available. The techniques available up to now guarantee access to all kinds of NMR experiments in liquid phase for a wide range of nuclei and in gel phase for the more common nuclei (1H and 13C). The NMR unit has successfully introduced researchers to such uncommon techniques as heteronuclear (mono and bidimensional) experiments, diffusion experiments and kinetic measurements. The unit staff also organizes training activities which range from training new users in obtaining NMR spectra automatically and how to use NMR processing software (TOPSPIN), to more general courses about the NMR experiments available and the information they can provide.

New Carbon Reactivity Rules with Radical Carbenoids and Carbyne Equivalents Enabled by Photoredox Catalysis

Ana García Herráiz