Characterisation

Based at St Andrews

• CW X-band EPR spectrometer from the Bruker, 3.8K - 350K. In Physics
• CW 94/188/280 GHz home-built EPR spectrometer, 3.8K - 350K
• pulsed/CW X/Q-band Bruker EPR spectrometer with PELDOR/ENDOR extension, 3.8K - 350K
• pulsed/CW home-built small dead-time W-band EPR spectrometer with PELDOR/ENDOR extension, 3.8K - 350K

• The SIRCAMS website contains information about the Mass Spectrometry service for external users.

The School of Chemistry is equipped with a suite of MS instruments for a range of analyses. These include -

• Small molecule nominal and accurate mass measurement.
• Complex mixture mass analysis (by FT-ICR MS)
• MALDI MS-imaging
• Metal analysis by inductively coupled plasma mass spectrometry
• Biomolecular mass spectrometry analysis
  • intact protein mass analysis
  • peptide mass fingerprinting
  • top-down fragmentation
  • native mass spectrometry for macromolecular assembly characterisation
  • ion mobility MS analysis

Specific Instruments Available

• 12T Bruker SolariX.  Fourier Transform Ion Cyclotron Resonance Mass Spectrometry (FT-ICR MS) . Several techniques are available for these instruments: principally electrospray or nanoelectrospray ionisation (ESI) via an automated Advion Nanomate as well as matrix-assisted laser desorption ionisation (MALDI) imaging. Equipped with Dionex HPLC. APPI is also available.
• Bruker Ultraflex MALDI TOF TOF: a MALDI Time-of-Flight system for peptide, protein analysis. Also suited for MALDI imaging.
• Bruker HCT  high capacity ion trap with ESI and nESI interface. Equipped with nano HPLC.
• Bruker ESI Micro-Tof equipped with LC for automated small molecule mass analysis
• Waters Synapt G2. A Mobility capable Q-ToF with nanoESI and ESI and an LC interface.
• Waters Q-TOF  with an extended mass range quadrupole, equipped with nanoESI and ESI and an LC interface.
• ThermoElectron MAT 900 Sector instrument A number of ionisation techniques are available, including Electron Impact (EI), Fast Atom Bombardment (FAB) and electrospray ionisation (ESI). GC and LC MS analysis is also possible for accurate mass analysis.
• Two LCQ Thermo Finnegan instruments with LC ESI.
• A GC-MS platform. Instruments are available for open access use following training.
• ICP-OES for trace analysis of metal elements (0.0002-1000ppm) and a limited number of non-metallic elements (e.g. S, P). Perkin Elmer Optima 5300 DV ICP-OES.
• ICP-MS for isotope ratio studies and ultra trace analysis of metal elements (0.0005-100ppb), and a limited number of non-metallic elements (e.g. S, P). Agilent 7500ce ICP-MS.
• LC-ICP-MS is suitable for speciated metal analysis and compounds with metals bound that are separable by LC techniques. Agilent 1200 series HPLC with MS hook-up.

External enquiries should be directed to Dr Logan MacKay.

Liquid State Spectrometers Based at Edinburgh

NMR is an extremely powerful technique for investigating the structure of chemical species, primarily those in solution, by the radio-frequency interrogation of the sample held in a powerful magnetic field.

• Discuss your project with our highly skilled NMR staff, which can customize techniques and ways of acquiring NMR spectra and design experiments according to your needs.
• Use the fully automated 800MHz NMR spectrometer, offering the highest resolution and sensitivity in Scotland, as well as a suite of automated 600 – 400 MHz spectrometers supporting wide range of NMR experiments for small and large molecules.
• High throughput service underpinned by cryoprobe technology – increased service speed and sensitivity providing cheaper solution to your problems.
• Spectrometers operate with sub-milligram quantities of samples.
• Unique Reaction mechanism analysis equipment that enables monitoring of fast reactions in situ.
• Come and use the facility yourself – after brief training, you can use it on a drop in basis, saving time and organization.

We Can Answer Your Questions

• “What’s the structural composition of this?”
• “What’s happening as this reaction takes place?”

For more information please contact Dr Juraj Bella.

Solid State Spectrometers Based at St Andrews

A solid-state NMR service is available in St Andrews with access to 400 MHz HFXY and 600 MHz Bruker Avance III spectrometers. A wide range of double- and triple-resonance experiments have already been implemented and, in addition to routine experiments, fast MAS (up to 40 kHz on the 400 MHz machine and 60 kHz on the 600 MHz machine) and variable-temperature experiments are also possible.

For more information please contact Dr Daniel Dawson.

Cutting edge computational facilities for all EaStCHEM researchers, specifically designed for researchers with no previous computational experience. A wide range of computational chemistry software packages are available that encompass both quantum mechanical and classical simulation methods. Training and support provided for all research active staff and students.

• Calculate IR, Raman, EPR, UV/Vis spectra.
• Molecular structure.
• Binding energies.
• Redox potentials

Structural characterisation by single crystal X-ray diffraction is a major analytical and research tool in chemistry providing both definitive sample identification and detailed structural analysis. We offer a complete single crystal diffraction service to our industrial partners, through the provision of dedicated analysis, interpretation and consultancy services.

Single Crystal X-ray Diffraction

•  Ideal for detailed study of organic or organometallic complexes.
•  Provides definitive chemical identity, bond dimensions, molecular conformation and crystal packing analysis.
•  Variable temperature measurements in the range 80—500 K.
• Over 15 years experience

Powder X-ray Diffraction

• Ideal for bulk analysis for phase identification, polymorphism, or identifying structural change in response to environmental changes.
• Rapid and non-destructive.

We Can Answer Your Questions

• “How can I grow crystals of this?”
• “I’ve got this crystal, what is it? 

Based at Edinburgh

Raman Microscopy and FTIR spectroscopy for material characterisation.

Raman spectroscopy and Infrared spectroscopy are complementary techniques used to observe characteristic vibrational transitions in materials. These can be used to provide a “fingerprint” of the chemical composition of a sample. The provided combination of Raman and/or Infrared spectroscopy with optical microscopy provides a non-destructive way of identifying, characterising and providing surface mapping (on a micron scale) of a wide-range of materials of relevance for materials science, nanotechnology, geosciences, and biosciences among others.

• Discuss your project with our expert researchers, who can propose the best ways of acquiring vibrational spectra from your materials.
• Use the facility yourself – get training on the Raman/FTIR facility suitable for your application; after training, you can use it with available help of expert researchers.
• Get help with analysis of spectral data after measurement; compare the results from  infrared spectroscopy with the materials spectral library data.

Note:  Requires milligram quantities for measurements

SPM Microscopy

Scanning probe microscopy (SPM) is a microscopy technique for measurements on surfaces and particles covering the sub-nanometer up to the micrometer scale. It can provide information on the morphology (AFM), electrical and magnetic, elastic and frictional properties of surfaces and has a number of applications in material science, chemical physics and life sciences.

• Discuss your project with expert researchers, who can customize techniques and ways of acquiring atomic force microscopy (AFM) or other SPM images according to your needs.
• Get training on SPM for your specific application and access the instrument yourself with real time help available from expert researchers
• Off-line analysis of images can be accessed to provide detailed information on surface roughness, particle size analysis, surface conductivity etc.

We Can Answer Your Questions:

• “What is the chemical composition of this?”
• “What are the properties of the surface of this material? 

Based at St Andrews

• Jobin-Yvon Labram and T64000 Raman spectrometers equipped with He-Ne (633nm), He-Cd (442nm) and Ar-ion (488/514nm) lasers.