Analytic Services Laboratory

Metals, Anions and Elemental Analysis

A range of analytical techniques and instrumentation is available to businesses.

• Determination of most metals from percent to ultra trace levels.
• Samples include: alloys, dusts and particulates, geological materials (rocks and sediments), contaminated soils and waters, organic materials such as foodstuffs.
• A full range of preparative techniques (most demanding of sample types possible).
• Microwave-assisted digestion, open beaker acid attack (including HF/HClO4), alkali fusion and sequential extraction.
• Quantification by one or more instrumental techniques: ICP-MS, ICP-OES, XRF, AA, and SEM-EPM.
• Laser ablation ICP-MS for direct spatial analysis of solids.
• Anions by ion chromatography.
• C, H, N and S by combustion analysis.

Organics

Our Analytical Services Laboratory has experience in the analysis of organic compounds and pharmaceutical materials within a range of sample matrices.

• Separation and quantification of compounds using gas chromatography (GC) or liquid-chromatography (HPLC) with a variety of detector types.
• GC-MS and LC-MS including triple quad, and Q-TOF instrumentation.
• Measurement of accurate mass.
• Direct sample analysis by DART.
• Sample extraction and clean-up techniques.
• Headspace, and purge and trap accessories for automated extraction.
• Method development and validation.

Imaging and Surface Analysis

Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray Analysis (EDX) can be used to image and investigate the properties and compositions of a broad range of sample types.

• High resolution surface inspection and backscatter analysis of samples.
• Non-destructive, semi-quantitative elemental analysis of solids using energy dispersive X-ray microanalysis.
• Wide area X-ray mapping and line profiles.
• Surface measurements and roughness characterisation using stereo-imaging
• Low vacuum variable pressure for examination of uncoated material
• Digital export of images
• Carbon and gold coating of non-conducting samples.
• Cold FEG instrumentation available for very high resolution imaging (also fitted with a TEM detector).

X-Ray Diffraction

• Powder X-ray diffraction, capillary and small sample low background sample holders are available.
• Copper and Cobalt X-ray tubes.
• Phase identification.
• Search match via ICDD databases and semi-quantitative analysis using Siroquant (Rietveld analysis via Topas).
• Separation and characterisation and quantification of clays and other mineral phases.

Nuclear Magnetic Resonance

The following instruments are housed in our NMR suite:

• 400 MHz Jeol FT NMR
• 5mm Multinuclear Liquid Probe
• 300 MHz Jeol FT NMR
• 6mm Multinuclear HS MAS Solid Probe
• 5mm Multinuclear Liquid Probe
• 500 MHz Jeol FT NMR, with pulsed field gradients.
• 5mm, Multinuclear, Direct Detected, Liquid Probe
• 5mm, Multinuclear, Inverse Detected, Liquid Probe
• 5mm, Multinuclear, HR MAS DOTY Probe
• 400MHz Bruker FT NMR
• Range of liquid probes

In addition to providing a routine spectral service, these instruments can be used for a range of structural studies with solid or liquid samples:

• Nuclei include 1H, 13C, 19F, 31P, 27Al, 29Si and 23Na
• Almost any type of non-ferromagnetic organic and inorganic material
• Non-destructive technique (sample can be recovered)
• Measurement of diffusion coefficients to allow insights into colloidal and self-assembling systems

UV-visible

UV-Visible, Infra-Red (FTIR) and Laser Raman Spectroscopy.

We offer routine and specialist services for the characterisation (molecular analysis) of solid, liquid (solution) and sometimes gaseous compounds and surface characterisation of crystalline and amorphous solids.

Techniques/equipment include:

• FTIR, ATR FT IR and IR microscopy.
• UV-Vis (temperature-controlled) spectroscopy.
• Reflectance UV-Vis spectroscopy,.
• FT Raman spectroscopy/Imaging with mapping capability.
• See also 'Imaging and Surface Analysis'.

Material characterisation

We can characterise solids, such as polymers, minerals, powders and particulate formulations, using a range of techniques for quantifying macroscopic behaviour including:

• Particle size analysis by laser diffraction or dynamic light scattering
• Rheology (controlled stress/shear and temperature)
• Electron Microscopy
• Aqueous gel permeation chromatography (GPC).

Thermal properties

• Calorific value using bomb calorimetry
• Thermogravimetric Analysis (TGA), TGA-FTIR:
  • water content
  • oxidation
  • degradation pathway and decomposition
• Hot Stage Microscopy (HSM):
  • phase transitions
  • softening
  • crystalline habits
  • size distribution
• Differential Scanning Calorimetry (DSC):
  • 1st and 2nd order transitions
  • glass transition, polymorphic transitions, crystallisation, melting
• Thermally Stimulated Current (TSC) Spectroscopy:
  • α, β and γ transitions in materials
  • molecular motions over a wide temperature range (-160C to 250C)
  • cooperative and non-cooperative rearrangements
  • relaxation map analysis
  • calculation of activation energies for relaxation processes

These techniques can be provided with the backing of considerable knowledge in the particular areas of pharmaceutical formulation science and technology, characterisation of clays and other minerals and in structural and material engineering.

Mass Spectrometry

We have a suite containing nine modern organic mass spectrometry instruments.

Learn more about the equipment, applications and our experts on our dedicated page.