Brodie Bonsor, Biochemistry student

Analytical Chemistry Measurement

Drawing on technical expertise and instrumental capability, we carry out analytical measurement services, for various industry sectors and a wide range of applications.

We can perform materials analysis for the chemicals industry, carry out elemental analysis for agriculture and molecular structure determination by proton or carbon NMR for the pharmaceutical industry.

Dr Robert Lewis
Faculty of Science and Engineering
Dr Robert Lewis
Analytical Services Team Leader

The Challenge

Drawing on technical expertise and instrumental capability, we carry out analytical measurement services, for various industry sectors and a wide range of applications. We can perform materials analysis for the chemicals industry, carry out elemental analysis for agriculture and molecular structure determination by proton or carbon NMR for the pharmaceutical industry.

The Approach

Our dedicated Materials Analysis Laboratory and access to the wide range of in-house analytical measurement instrumentation for elemental, molecular, materials and formulation analysis allow us to cater for enquiries from a wide range of industries. We have worked with industrial partners on hundreds of projects for more than twenty years. Dedicated staff mean a fast response to enquiries. We carry out small-scale investigative work and also partner for longer term projects such as KTPs.

Chemistry

OUR AIMS

  • Carry out chemical measurement
  • Identify unknown compounds
  • Solve analytical measurement science problems in numerous industry sectors, such as rubber processing, engineering, plastics processing, automotive component manufacture, domestic heating, industrial filtration, marine surveying, agriculture and pharmaceuticals

We welcome enquiries about new projects and measurement challenges from academia, industry, the public sector and beyond. 

 

Projects

Chemistry PIXcel powder diffractometer

Elemental Analysis

Determining the elemental composition of a material is pertinent to discovering what that material may be, its intrinsic properties and even how it was made. This applies to a range of industries, from testing soil quality in agriculture, identifying unknown compounds in pharmaceutical products to quantification of specific elements in food processing. This can be achieved with a suite of analytical techniques including ICP-OES, EDX and high resolution MS.

LCD

Chemical/Molecular analysis

Analysis of chemicals and molecules in pure form or in mixtures. Molecular analysis is carried out to identify species (qualitative analysis) and sometimes to measure their concentrations (quantitative analysis). Spectroscopic techniques such as NMR, FT-IR, RAMAN) as well as XRD can be employed, in addition to a suite of separation technique (CE, GC, LC) often hyphenated to MS.

Microscopy

Materials Characterisation

Raw or processed materials from a production line may need to be characterised for quality control, perhaps to compare different suppliers, analyse causes of a failed process or to optimise material properties. 

Instrumentation to study material properties include X-Ray diffractometers (powder and single crystal), a range of microscopy (SEM, AFM) and spectroscopic techniques as well as measurement of thermal behaviour (DSC,TGA) and physical properties (viscosity, rheology, contact angle, zeta potential).

Chemical plant

Manufacturing Process Refinement

Optimisation and improvement of industrial processes is an important task that has strict requirements to ensure that each step operates with peak efficiency, minimal waste, and environmental impact. They may involve molecular spectroscopies and physical measurements to improve the process and identify by-products.

Microscope

Product Formulation

Analysis of formulations for example in the pharmaceutical, cosmetics or food industry, may be carried out with chromatography techniques, mass spectroscopy, physical chemistry measurements or a range of molecular spectroscopy techniques.

Crops

Biomolecule and protein analysis

Biomolecular and protein analysis may be carried out with a suite of mass spectrometry and spectroscopy instruments to ascertain the identity, purity, conformation, structure, or activity.

View all projects

Analysis of Lead Paint 

Service Sector – Environmental, Techniques used – ICP, SEM-EDX

A conservation organisation was involved in the refurbishment of a gas holder, dating back to pre-1970, when use of lead paint was restricted. The holder had been painted many times; we were supplied with samples of paint and asked to determine if lead was present. An average lead-value was taken for the sample by preparing it via microwave-acid digestion and analysing it via inductively-coupled plasma optical emission spectroscopy (ICP-OES) by creating atomic ions. Lead was found to be present.

 

We also freeze-fractured samples and investigated each layer by energy dispersive X-ray (EDX) analysis - which creates a signal based on energy dispersed by elements present in the sample. EDX allowed us to confirm which layers of paint contained lead and which didn’t – allowing for safe removal.

 

INVESTIGATION INTO STEEL - SURVEYING WETTABILITY

 

Service Sector – Marine Surveying , Techniques used – SEM-EDX

 

A marine insurance company had a cargo of galvanized steel which was wetted during shipping and rusted. It was important to find whether the wetting was a result of fresh or saltwater exposure – indicating if the exposure occurred on land or at sea. If wetting had occurred at sea, the dry samples we received would contain residual sodium chloride salts.

 

The EDX attachment of the scanning electron microscope (SEM) was utilised as it is sensitive to heavier elements like chlorine. The EDX spectrum showed no chlorine was present, neither was sodium. This concluded wetting could not have occurred at sea enabling the client to identify the parties responsible for their insurance claim. 

 

Material Failure Analysis

 

Service Sector – Materials , Technique used – SEM-EDX

 

A Hull-based company came to us with failing stainless-steel filter meshes due to excess corrosion. Investigating this failure, samples of the corroded filters were analysed by Scanning Electron Microscopy (SEM) with an Energy Dispersive X-Ray Diffraction (EDX) attachment. The high magnification SEM images showed corrosion from a deposited material on the filter. Elemental analysis via the EDX attachment confirmed the deposit to include copper (Cu) – a known accelerant for stainless-steel corrosion, leading to premature failure. Copper was not present in the raw materials used in manufacturing. These results lead the company to investigate its source, potentially arising from copper piping which they had been unaware of. 

 

Chemical Protective Suits

 

Service Sector – Chemical Industry

 

As part of a KTP with Microguard– a hull-based company who manufacture chemical protective suits which require extensive permeation testing. They were using a third-party for this but decided to bring it in-house.

 

Initial trial work was carried out in the Department of Chemistry’s laboratories before building a testing laboratory from scratch at Micrograd’s Hull site. At the end of the two years, Micrograd were in possession of a major facility which was not present before and the KTP program received the highest grade of “Outstanding”.

 

Micrograd has since been taken over by the Ansell Group, who stated the testing laboratory in Hull was a prime factor in their decision.

 

Equipment

We have a wide range of chemical analysis and measurement equipment within our Materials Analysis Laboratory and the Department’s research, teaching and service laboratories.

Mass Spectrometry

For analysis of small molecules , biological and synthetic polymers, organo-metallic compounds, peptides and proteins, oligonucleotides and oligosaccharides, our Mass Spectrometry Facility features GC-MS and HPLC-MS instruments as well as a MALDI-TOF MS with imaging capabilities and a Nano-flow LCMSMS. For elemental analysis of trace elements in biological fluids, we have a an Inductively Coupled Plasma (ICP-MS)with a special laser source.

Molecular Spectroscopy

For structural determination and quantitative analysis, our laboratories feature UV/vis, Infrared (FT-IR with ATR), fibre optic Raman spectrometer and Fluorescence Spectroscopy. We have two 400 MHz JEOL Nuclear Magnetic Resonance (NMR) spectrometers for high resolution solution spectra.

Separation Techniques

For analysis of compounds in a mixture, we can fall back on a suite of GC, HPLC and CE instruments with UV/vis spectroscopic readout as well as our GC/MS and HPLC/MS systems. Gel permeation chromatography (triple detection) is available to determine the average molecular weights of polymers.

X-ray and Material Analysis

We have internationally renowned expertise in Single Crystals X-ray Diffraction (SCXD) and Powder X-ray Diffraction (PXRD). Recent projects have involved determination of the molecular structures of APIs by SCXD and determination of solid forms by PXRD. For example, we have worked with an adhesives manufacturer to identify the solid products formed when their formulation decays. Quantitative and semi-quantitative analysis of mineral samples by X-ray methods are routine. 

Microscopy

Scanning Electron Microscopy (SEM), Atomic Force Microscopy (AFM), Confocal Laser Scanning Microscopy (CLSM) and Thermal polarising microscopy (POM).

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