Chromatography, thermal and electrochemical analysis
GINYS-ICIQ-004
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.).
Services
GAS CHROMATOGRAPHY
Small molecule mass – FID for high and low concentration – TCD Gases detection
HPLC
Chiral and Isomer separation – Semipreparative: purification up to 1g
SFC
Solvent free analysis – Chiral and Isomer separation
UHPLC
Ultrafast analysis with small quantities
DSC/TGA
Melting point – Crystallization – Decomposition – Glass Transition – Oxidative Processes
ITC
Non-Covalent Interactions – Molecular Recognition
KARL FISHER
H2O quantification of hydrates
POTENTIOSTATE
Redox Studies – Oxidation States
Equipment
- Balances: A Mettler Toledo AX205DR scale that allows a maximum weight of 91 g with an accuracy of 0.01 mg, or a maximum weight of 220 g with an accuracy of 0.1 mg. A Mettler Toledo MX5 microbalance that allows a maximum weight of 5.1 g with an accuracy of 0.001 mg.
- DSC and 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 MT1 type scale. Temperature range from room temperature to 1100 ºC, accuracy ± 0.25 ºC. Equilibrium measurement range up to 1 g with a resolution of 1 µg.
- Gas Chromatograph: An Agilent 6890N gas chromatograph coupled to a selective mass detector with electronic impact ionization source and an Agilent 6890N with FID and TCD detectors.
- Glove boxes: MBraun inert gas boxes ensure that the inner chamber of the glove compartment is capable of handling substances sensitive to oxygen and / or moisture.
- HPLC Chromatograph: An Agilent 1100 chromatograph equipped with a 10-port switching valve for 2D chromatography and an Agilent 1200 series, both with multiple detection.
- Microcalorimeter: A Microcal VP-ITC isothermal titration microcalorimeter. Operating temperature range from 2 ºC to 80 ºC with a noise level of 1 nanocal / s (4 nanowatts).
- Osmometer: A KNAUER K-7000 vapor pressure osmometer, which allows the determination of the average molecular mass of polymers in aqueous (= 10000 g / mol) and organic (40 – 40000 g / mol) solutions. Cell working temperature range 20 – 130 ºC.
- Potentiostat: A PARSTAT 2273 potentiostat from Princeton Applied Research that offers a supply voltage of up to ± 100 V (available on the counter electrode), scan range of ± 10 V and current range of ± 2 A.
- Semipreparative chromatograph: A Waters semipreparative chromatograph (up to 40 ml / min) equipped with a 600E multisolvent delivery pump, a Rheodyne 7725i injection valve and a 2487 detector.
- SPS: Solvent Purification Systems (SPS) from Innovative Technologies provide dry organic solvents that prevent distillations for moisture-sensitive reactions.
- Rating coulometer: A Metrohm 756 KF coulometer. Determination range from 10 µg to 200 mg of water, maximum titration rate of 2.24 mg H2O / min and 0.1 µg H2O resolution.
Staff
Adrian Ortega | aortega@iciq.es
| 977 920 200 (ext. 332)
Meritxell Díaz | mdiaz@iciq.es
| 977 920 200 (ext. 332)
María José Hueso | mhueso@iciq.es
| 977 920 200 (ext. 332)
