Equipment & Capabilities

The instrument we have is a ThermoScientific Scios2 FIB-SEM. It includes a gallium ion column, and semi-automated TEM lemella preparation and slice-and-view 3D imaging. This also includes trinity in-lens detectors and 60mm² SDD EDX systems. The system includes an easylift micromanipulator, and so can be used to fully prepare electron transparent lamellas for the TEM.

LS-AFM: AFM integrated with brightfield/phase contrast/epifluorescence optical microscopy, and a bio-cell, allowing temperature and environmental control.

The instrument we have is an MFT-2000A tribometer from RTEC.

By monitoring the magnetic environment of the atoms we can determine the structure of molecules, either in isolation or when interacting with other molecules. Since every conceivable environmental condition has a cumulative effect on this magnetic environment – such as molecular interactions, temperature, pH, solution environment – NMR spectroscopy is a very versatile method of analysis.

NMR is typically used for structure determination of small molecules, such as chemicals or small biomolecules. NMR can also by used to investigate mixtures of molecules and can even solve 3-dimensional structures of proteins.

NMR spectroscopy relies upon exposing the sample of interest to an enormously strong magnetic field, approximately a quarter of a million times as strong as the magnetic field of the Earth, generated by a superconducting magnet.

Once exposed to these conditions, each atom within the sample becomes a sensitive barometer of its environment, and will report back on any changes it experiences, such as to temperature, pH, concentration or intra- and inter-molecular interactions.

We have the capabilities to routinely analyse a wide variety of elements in a fully automated way, such as hydrogen, carbon, phosphorous and fluorine. Analysis times vary, depending on the sample conditions and analysis desired, but usually take only a few minutes.

NMR works well for the analysis of complex mixtures, such as: formulation, identification and quantification of impurities, food forgery, stability studies, metabolomics, reaction monitoring, and elucidating the chemical and three-dimensional structures of compounds and polymers. NMR spectroscopy can be fully quantitative.

Our instrument is a Bruker Avance III 500 equipped with CP-MAS H/X (solid probe).

By coupling Raman spectroscopy to light microscopy, spatial resolution down to 1 micron of compositional changes within a sample can be achieved. In addition, confocal Raman microscopy can be used to perform depth-profiling of a sample giving 3-dimensional chemical resolution.

Raman is an identification technique which allows specific chemical bonds in a sample to be determined. Consequently Raman is useful as part of formulation studies or examination of unknown samples to determine the presence of compounds of interest.

In addition to determining composition, the technique allows the crystallographic structure of a sample to be determined. This polymorphic information is essential in pharmaceutical studies and can also be used to investigate the crystal structures in mineral and metallurgical samples.

By combining the technique with microscopy, spatial chemical resolution can be performed to determine the heterogeneity of a sample. In addition, depth profiling can be carried out to perform 3D studies to look at the penetration of a chemical through a sample e.g. transdermal drug delivery studies.

The instrument is a Bruker Senterra II microscope coupled to a RAMII FT Spectrometer, and it is equipped with 534 and 785 nm laser, and also an external fibre-optic probe.

Molecules absorb infra-red light at wavelengths that correspond to molecular vibrational energies (e.g. bond stretching). The actual energies of light absorbed depends on the strength of the bond and, in turn, on the atoms at either end of the bond and the bond order. Thus, the pattern of light absorbed by a molecule is a composite of all bonds within that molecule and the result is a unique absorption spectrum for each molecule of interest.

Other aspects of molecule geometry that impinge on bond strengths and rigidity, such as intra- and inter-molecular interactions, alter the wavelength of light absorbed and hence can be probed by FT-IR.

FT-IR is used primarily for the identification of organic compounds due to the readiness of bonds within these molecules to vibrate upon interaction with infra-red radiation. Thus FT-IR is well-suited for the analysis of unknown organic materials such as polymers.

By linking FT-IR to thermal analysis (simultaneous thermal analyser (STA)) a multi-pronged approach to sample identification can be performed to increase confidence and reliability. In addition, thermal stability can be assessed by measuring the volatiles released during thermal analysis.

The Vertex 70v has wide spectral range (near and mid-infrared ), and a number of sampling accessories. These include ATR, DRIFTS and gas sampling. This last method can be coupled to the STA, to measure the spectra of evolved gases from samples as a function of temperature.

At the Bridge we have high-throughput as well as variable temperature and humidity options for powder diffraction to analyse reactions or changes in crystalline forms as a function of environment.

A dual source (Cu/Mo) single crystal diffractometer allows for different wavelengths of x-rays to extend the scope of the analyses. This instrument is cryo cooled to increase data quality whilst a plate stage allows for fast screening of crystals from different solution conditions.

When X-rays are directed at a sample they are reflected from the electrons of the atoms, if the sample is crystalline, i.e. has long range order, these reflections constructively and destructively interfere with each other giving rise to a specific pattern that is measured. This pattern depends on the internal order of the sample and can be considered like a fingerprint of a crystalline material.

Comparison to a database of known patterns helps identify the material in question. Since the X-rays are reflected from the electrons, X-ray diffraction does not give direct evidence on the elements in the material. The analysis of single crystals allows for the determination of the atomic positions in the crystal from the diffraction pattern. This gives rise to accurate molecular elucidation with information on bond lengths and angles in the molecule as well as intermolecular interactions.

Our instruments are a Bruker D8 Discover for single crystal diffraction and a Bruker D8 Advance for powder diffraction.