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Chromatography, Thermal Analysis & Electrochemistry

Chromatography supports the separation, identification and isolation of chiral and non-chiral compounds. Thermal Analysis serves mainly for measurements of solid phase transitions, and Electrochemistry main applications are the determination of water content, acidic constants and redox processes

About

The Chromatography, Thermal Analysis and Electrochemistry Unit provides technical and scientific support in the following techniques:

Chromatography is the main technique in the unit. It supports the separation, identification and isolation of chiral and non-chiral compounds. Regarding liquid chromatography, the unit has four High Performance Liquid Chromatographs, two analytical HPLCs equipped with diode array, fluorescence, evaporative light scattering and single quadrupole mass detectors, one semi preparative HPLC (up to 40 mL/min) and a preparative (up to 150mL/min), both equipped with UV-vis dual wavelength detectors. Concerning gas chromatography instrumentation, the Unit has three GC, two of them coupled to a mass selective detector and one to flame ionization and thermal conductivity detectors.

Thermal Analysis instrumentation consists of a differential scanning calorimeter (DSC) and a thermobalance (TG). Main applications are measurements of solid phase transitions within the range -80ºC up to 600ºC (DSC) and determination of volatile compounds (MS coupling) and/or thermal decomposition (TG) in the range from room temperature up to 1000ºC. An isothermal microcalorimeter titrator (ITC) is also available in this unit. ITC is used for accurate determinations of binding constants, coordination stoichiometry and thermodynamic values.

Electrochemistry instrumentation consists of two titrators (Karl Fischer and potentiometric) and two potentiostats. Main applications are the determination of water content, acidic constants (pKa) and redox processes (voltammetries, electrolysis, etc.)

In addition, the unit’s technicians manage open use instrumentation such as glove boxes and solvent purification systems

Equipment

Balances

A Mettler Toledo AX205DR balance allowing a maximum weight of 91 g with a precision of 0.01 mg, or a maximum weight of 220 g with a precision of 0.1 mg. A Mettler Toledo MX5 microbalance allowing a maximum weight of 5.1 g with a precision of 0.001 mg.
DSC&TGA

A Mettler Toledo DSC822 with a 56-point Au-AuPd thermopile FRS5 sensor. Measuring range from room temperature up to 700 ºC, accuracy ± 0.2 ºC and resolution < 0.4 µW. A Mettler Toledo TGA/SDTA851 with a balance MT1 type. Temperature range from room temperature up to 1100 ºC, accuracy ± 0.25 ºC. Balance measuring range up to 1g with a resolution of 1µg.
Gas chromatograph

An Agilent 6890N gas chromatograph coupled to a mass selective detector with electronic impact ionization source and an Agilent 6890N with a FID and TCD detectors.
Glove boxes

MBraun inert gas boxes ensure that the glovebox interior chamber is able to handle substances that are sensitive to oxygen and/or moisture.
HPLC chromatograph

An Agilent 1100 chromatograph equipped with a 10 port switching valve to carry out 2D chromatography and an Agilent 1200 series, both with multiple detection.
Microcalorimeter

An isothermal titration microcalorimeter Microcal VP-ITC. Operating temperature range from 2 ºC up to 80 ºC with a noise level of 1 nanocal/sec (4 nanowatts).
Osmometer

A vapour pressure osmometer KNAUER K-7000, allowing the determination of the average molecular mass of polymers in aqueous ( = 10000 g/mol) and organic (40 – 40000 g/mol) solutions. Working temperature cell range 20 – 130 ºC.
Potentiostat

A Princeton Applied Research PARSTAT 2273 potentiostat offering compliance voltage up to ± 100V (available at the counter electrode), ± 10 V scan range and ± 2 A current range.
Semipreparative chromatograph

A Waters semipreparative chromatograph (up to 40 mL/min) equipped with a 600E multisolvent delivery pump, a Rheodyne 7725i injection valve and 2487 detector.
SPS

Innovative Technologies solvent purification systems (SPS) provide dried organic solvents avoiding distillations for sensitive moisture reactions.
Titration coulometer

A Metrohm 756 KF coulometer. Determination range from 10 µg up to 200 mg of water, maximum titration speed of 2.24 mg H2O/min and 0.1 µg H2O of resolution.