Skip to content

Analytical Techniques

The Centre for Chemical and Biological Analysis houses a broad range of specialist analytical instrumentation that covers a wide spectrum of applications.  The equipment is run by dedicated, experienced staff and maintained to the highest of standards.  Our analysts have extensive knowledge of many analytical techniques and have demonstrated their expertise through both academic research publications and commercially funded contract research projects.  The Centre can offer a number of approaches to challenging problems by producing and interpreting data from different analytical techniques.

Please contact us if you would like to discuss your project and ways in which we can help; we pride ourselves on being responsive, thorough and competitive.

Preparing GC analysis

GC analysis using the Agilent 6890 with FID

Nuclear Magnetic Resonance

Instruments and facilities

Multi-nuclear JEOL ECA 600 MHz FT NMR Spectrometer

  • Tuneable broadband JEOL Multinuclear High Sensitivity 5 mm solution probe;
  • Nalorac Inverse 1H optimised {13C, 15N} High Sensitivity 5 mm solution probe;
  • DOTY Scientific solid state probe for CP-MAS solids measurements;
  • Variable Temperature Facility (-40 °C to 200 °C);
  • Triple Resonance capability.

Multi-nuclear Bruker AVIII 400 MHz FT NMR Spectrometer 

  • 'SMART' tuneable probe (5 mm solution) for acquisition of any NMR active nuclei;
  • Equipped for 1D and 2D NMR experiments including 1H-X nucleus correlation experiments (HMBC and HMQC);
  • VT experiments (5 °C to 120 °C);
  • SampleXpress 60 position sample changer for fully automated use;
  • Novel Diffusion (DOSY) methods for macromolecular systems.
Bruker 600MHz NMR

600 MHz NMR Spectrometer in the Centre

Chromatography, isolation and purification

The Centre houses a range of chromatographic techniques, including gas (GC) and liquid systems (HPLC, ion-exchange, size exclusion, capillary electrophoresis, column chromatography and preparative HPLC).

We have a range of sample introduction and detection systems that allow analysis of a range of materials with different characteristics:

  • Agilent 6890 and 7890 GCs with FID, TCD and MS detection; liquid and headspace introduction;
  • Waters 2695, 2790 and 2795 HPLCs with UV (VWD / PDA), Fluorescence, ELSD, RI, MS (Q) and MSMS (QQQ) detection;
  • Thermo Accela UPLC with Orbitrap LTQ Ion Trap MSn and HRMS (accurate mass);
  • Agilent 3D Capillary Electrophoresis with UV (PDA) detection.

Our core expertise covers:

  • Developing chromatographic methodology for complex, problematic mixtures and materials not easily detected;
  • Impurity isolation and identification;
  • High-resolution mass spectrometry for accurate mass / molecular formula determination.
GC Laboratory image

Agilent 7890GC with 5975 EI/CI MSD

Particle Characterisation

The Centre offers a comprehensive analytical service for characterisation of solid particulates through combinations of macroscopic, microscopic and diffraction tools.  The Centre can investigate particle size, shape and surface characterisation as well as bulk powder properties such as true density and surface area determination.

Techniques available include

  • Particle Size Distribution (DLS / LD) analysis for powders and liquid suspensions or emulsions;
  • Zeta Potential Measurement;
  • Particle Morphology and Sizing by Polarised Might and Scanning Electron Microscopy;
  • Inverse Gas Chromatography for surface energy and surface area determination;
  • Dynamic Vapour Sorption;
  • Particle or True Density via Helium pycnometry;
  • Raman Microscopy (2-dimensional mapping capabilities for distribution and sizing applications).
Sympatec

Particle sizing by DLS using the Symaptec HELOS/ASPIROS system

Vibrational Spectroscopy

The Vibrational Spectroscopy facility at the Centre offers a range of molecular spectroscopy capabilities for material characterisation and problem solving.  Our experts have practical experience analysing a wide variety of materials using Fourier Transform Infrared (FTIR) and Raman Spectroscopies. An extensive range of instrumentation allowing optimisation of experiment and, though a range of excitation frequencies, opportunities to overcome fluorescence often associated with biomolecular systems.  

Renishaw InVia Confocal microscope:

  • 785, 633 and 514 nm lasers;
  • Line-focus stage for collection of 2-dimensional spectral arrays (maps).

Renishaw Raman RX210 (RIAS)

  • Portable, remote probe;
  • 785 nm laser.

Digilab FT-IR Microscope 

  • Analysis using microscope (ATR);
  • KBr disc;
  • Thin-film / Nujol mull;
  • Liquid and gas cells.

 

Laboratory equipment Raman microscopy

Renishaw InVia Raman Miscroscope

X-Ray Diffraction

The Centre's comprehensive XRD facilities cover automated, variable temperature and high resolution studies; state-of-the-art SCD facilities include the latest CCD cameras and cryo-crystallography systems.

Instruments and Facilities:

  • Bruker X8 APEX:
    • SCD CCD Kappa-four circle instrument; Oxford Cryostream Plus VT facility (80 - 500 K).
  • Bruker D8 Advance:
    • PXRD Bragg-Brentano with 9-sample autochanger for high throughput phase identification & mixture analysis.
  • Bruker D5000:
    • PXRD Bragg-Brentano with Anton Paar TK400 VT Stage.
PXRD instrument

Bruker D8 Advance PXRD

Mass Spectrometry

The Centre houses an impressive range of mass spectrometry apparatus hyphenated to various types of chromatographic systems allowing development / deployment of methods to study complex matrices including biological samples, formulated products and archaeological materials.

  • HRMS; Thermo Accela UPLC with Orbitrap LTQ ion trap MSn and HRMS for accurate mass determination;
  • LCMSMS; Waters 2790 HPLC (UV/RI/ELSD/fluorescence) with Quattro Ultima and QuattroLC triple quadrupole MS systems (ESI, APcI, direct infusion);
  • LCMS; Waters 2790 HPLC (UV/RI/ELSD/fluorescence) with ZMD Single quadrupole systems (ESI, APcI, direct infusion);
  • GCMS; Agilent 7890GC with 5975 Inert MSD (EI/CI ionisation).
Mass Spectrometer image

Thermo Orbitrap LTQ HRMS for accurate mass measurements

Thermal Analysis

We have a great deal of experience in thermal methods for the study of materials and have some bespoke hyphenated approaches that can be particularly useful in obtaining complementary spectroscopic / diffraction data (DSC-Raman and DSC-PXRD).

Areas of Expertise

  • Assessment of amorphous content by DSC, modulated DSC and DMA approaches;
  • API and excipient compatibility;
  • Hydrate and solvate quantification and identification by evolved gas analysed TGA;
  • Simultaneous DSC-spectroscopic (Raman) assessment of materials for physical form / polymorph assessment.

Instruments and Facilities

  • TA Instruments Q2000 Modulated DSC with refrigerated (RCS) and liquid nitrogen (LNCS) cooling; operation in standard and modulated modes;
  • TA Instruments nanoDSC for solution studies;
  • TA Instruments Q5000 IR TGA;
  • TA Instruments Q800 DMA with air and liquid nitrogen (GCA) cooling accessories and RH accessory for humidity control;
  • Zeiss Axioplan 2 Imaging Microscope with Linkam Hot-stage.

 

Thermal analysis instrument

Q2000 DSC

Microscopy

The Centre offers a wide array of microscopic techniques for interrogation of materials including pharmaceuticals (crystal morphology and amorphous materials), polymeric / nano-materials and biological samples.

  • Optical (Light) Microscopy:
    • Zeiss Axioplan polarised light microscope with Linkam hot stage.
  • Electron microscopy:
    • FEI Quanta400 environmental SEM (E-SEM) with Oxford IncaSight EDX;
    • FEI Technai G2 F20 TEM with EDX;
    • JEOL 1200 TEM.
  • Confocal Microscopy:
    • Zeiss LSM510 confocal fluorescence microscope with environmental chamber and 350, 488, 543 and 633 nm lasers;
    • Nikon TE2000 confocal fluorescence microscope with environmental chamber and 405, 488 and 543 nm lasers;
    • Nikon TE2000 equipped with MMI laser dissection set up.

 

 

 

SEM image in laboratory

FEI Quanta 400 E-SEM with Oxford EDX