Facilities

Our Lab

Our Lab

The Goicoechea Group is based in the Chemistry Research Laboratory and benefits from the state-of-the-art facilities the building has to offer. In addition, we have access to resources available in the Inorganic Chemistry Laboratory building and in other departments within the University of Oxford. These slides provide a flavour of the frequently used group and communal resources.

Schlenk Lines

Schlenk Lines

Many of the materials that the group works with are highly air and moisture sensitive, requiring special equipment to manipulate them in order to avoid contact with the air. All of the laboratory fume hoods are fitted with dual manifold Schlenk lines so that attached vessels can be purged of air and water prior to their contact with reagents.

Gloveboxes

Gloveboxes

Air-sensitive reagents and products are routinely handled in the group’s gloveboxes which have computer controlled atmospheres of nitrogen. Both water and oxygen levels are maintained below 0.1 ppm. The gloveboxes also contain dehydrated solvents which permits small scale, sensitive reactions to be carried out within the glovebox itself.

Solvent Drying

Solvent Drying

Dry solvents are essential for the types of reactions undertaken by the group. The communal MBraun SPS800 solvent drying systems provide ten dry solvents in a readily accessible fashion, which can be used directly without further purification.

Solvent Distillation

Solvent Distillation

For solvents not supplied on the SPS, and more difficult to dry solvents (hygroscopic), we utilize to solvent stills. Distilling solvents over a drying agent allow us to collect large volumes of solvent for use in particularly air- and moisture-sensitive reactions.

NMR Spectroscopy

NMR Spectroscopy

Solid-state crystallographic data is frequently supported by solution techniques such as Nuclear Magnetic Resonance (NMR) spectroscopy. On the 2^nd floor of the CRL we have access to a fully automated Bruker Avance III HD nanobay 400 MHz spectrometer for the running of routine samples. In the basement, we have access to a Bruker Avance III 500 MHz spectrometer which can be used for less common NMR active nuclei such as ²⁹Si and ¹¹⁹Sn or for more customised experiments such as DOSY. Finally, the department also has a submission service for running samples on a Bruker Avance 500 MHz spectrometer equipped with a cryoprobe.

X-Ray Diffraction

X-ray Diffraction

The primary structural characterisation technique we use is single crystal X-ray diffraction. This technique allows us to determine the chemical structure of reaction products. The CRL basement houses one Nonius Kappa-CCD and two Oxford Diffraction/Agilent SuperNovae single crystal diffractometers, which are all fitted with low temperature nitrogen cryostreams, allowing for the collection of data from air sensitive samples at a range of temperatures.

Arc Welding

Arc Welding

Zintl phase starting materials such as or K₃P₇ or K₄Ge₉ are directly synthesised by the combination of elements in sealed niobium tubes that are heated in a high temperature furnace for several days. The tubes are sealed in the absence of oxygen using a custom built arc-welder with a chamber that can be evacuated and filled with argon. Niobium is used to avoid side reactions taking place with the metal vessel at the high temperatures. The tubes are placed in larger silica glass ampoules which are evacuated before sealing with a glass blowing torch.

IR and Raman Spectroscopy

Infrared and Raman Spectroscopy

Vibrational spectroscopy is commonly used to characterize novel compounds and is particularly informative when studying unconventional chemical bonding. We have convenient access to both a Thermo Scientific iS5 FTIR spectrometer and a Thermo Scientific DXR3 Raman spectrometer on the 2nd floor of the CRL, as well as several methods for preparing samples under inert atmospheres.

UV-Vis Spectrocopy

UV-Vis Spectroscopy

We use UV-Vis spectroscopy to elucidate pertinant electronic transitions within novel compounds. These measurements allow us to build an accurate understanding of the electronic structure of these compounds, and provide a physical foundation by which we may validate and strenghten computational modeling. We have access to multiple spectrometers within the department, capable of both absorption and fluorescence measurements.

Glassblowing

Glassblowing

We are fortunate to be in a department with a phenomenal in-house glassblowing workshop. Having reliable, bespoke glassware is a must-have for performing our experiments - most of which require handling sensitive chemicals under inert atmospheres. These range from relatively simple pieces such as quartz tubes for solid-state reactions, to complex pieces of glassware like Schlenk lines and distillation setups.

Refreshments

Refreshments

Coffee and biscuits are an essential resource in every office space, and our group is no exception. Whether you need a lift in the morning after group meeting, or some extra motivation to power through a late cannula filtration that just isn't playing ball, we've got the caffeine to get you through.

Facilities

Our Lab

Schlenk Lines

Gloveboxes

Solvent Drying

Solvent Distillation

NMR Spectroscopy

X-ray Diffraction

Arc Welding

Infrared and Raman Spectroscopy

UV-Vis Spectroscopy

Glassblowing

Refreshments

Prof. Jose Goicoechea