We use a vast range of products directly or indirectly in everyday life. These range from soups to baby-foods to feed us; paints and coating products to provide robust structural materials; plastics and composites to create many products; and pharmaceutical drugs to fight disease. They share a similar manufacturing method in which raw materials (or reagents) are combined through physical or chemical means, and known as a 'process'. This takes place in a 'process vessel', which is often sealed, under pressure and at elevated temperature. Critical aspects of such processes are efficiency, product quality, energy use and emissions impact. The core aim of this project is to stimulate new sensing products that can enhance these aspects and exploit their markets through licences.The project builds upon our background science and experimental technology, which an estimation of the internal (invisible) distribution of process materials. These innovations harness two principles: spectroscopy - the identification of specific materials; and, tomography - the identification of the distribution of components within the process vessel (similar to methods to 'see inside' human bodies for medical diagnosis). Electrical energy using a 'compressed wide-band' is used, both to give the 'spectral' coverage and to provide fast response to suit dynamic processes. The project aims to provide a demonstration level for specific trial applications; to offer licensees a clear path for onward development into the two product forms: a 'point sensor' form, to identify materials in its immediate vicinity; and a 'zone sensor' form, to identify the distribution of specific materials. Increased knowledge empowers design and/or control to deliver major benefits to process end users: increased productivity and product quality, reductions in emissions and waste products, reduced energy demand and resulting carbon impacts. In illustration we can consider the advantages offered in two product examples. Pharmaceutical compounds are produced using crystallisation processes which are highly variable and can have poor yields such that some batches may not meet tight product specifications. This results in waste of energy, raw materials, and in the costly disposal of the useless out-of specification product. Here a Spec_zone sensor can transform 'process-knowledge' to allow 'smarter control, and gain a major increase in 'on-specification' yield, gaining obvious major benefits. These are very high value products and hence financial business savings can be large. The manufacture of foodstuffs follows a conventional recipe: such as mixing and cooking natural ingredients such as chopped vegetables in water. Unwanted objects in the product such as natural materials such as stalks and large seeds, and unnatural materials such as small pieces of metal or plastic are a possibility. Although these may be unpleasant for adults in products such as soups (but still present a serious 'brand' quality issue for the manufacturer) they may be dangerous if present in baby-foods. It is easy to find metals, using x-ray detectors on a pipeline, but much more difficult to find small objects, such small pieces of plastic or wood which can be detected by the 'wide-band' Spec_point sensor.In conclusion the ability to estimate the presence and concentration of specific materials and their distribution offers major benefits in effective process management. The project will provide demonstrations and concept details to enable licensees to develop future products, based on the Spec_point and Spec_zone concepts. It will include detailed application sectors studies to highlight potential early adopters. It is supported by two instrumentation suppliers who have expressed a keen interest in evaluation, and both have diverse markets and customers who are likely to be involved in evaluations.

Summary: A novel laboratory scale continuous hydrothermal flow synthesis (CHFS) system has been developed for the controlled synthesis of inorganic nano-materials (particles <100nm) with potential commercial applications from sunscreens and battery materials to fuel cell components and photocatalysts. The CHFS system has many advantages; it is a green technology (using supercritical water as the reagent), which utilises inexpensive precursors (metal nitrate salts) and can controllably produce high quality, technologically important functional nano-materials in an efficient single step (or fewer steps than conventionally). This project seeks to move the existing laboratory scale CHFS system (developed over the past few years at QMUL) towards a x10 pilot scale-up (nano-powder production of up to 500g per 12h depending on variables). The proposed research will initially compare the ability to control particle characteristics of the CHFS system at the laboratory scale over a large range of process variables (flow rates, temperatures, pressures, etc), building full operational envelopes that will describe reactor variables versus particle properties for each material. In particular, we will utilise process analytical technology (PAT)and the data will help develop univariate and multivariate understanding of the temporal operational spaces and interactions between process variables and product quality. PATand chemometrics incorporated with combined computational fluid dynamics modelling of hydrodynamics/mixing and population balance modelling of particle size evolution via nano-precipitation will be used to study alternative nozzles designs and other potential bottleneck factors. This will lead to a generic strategy for scaling up and controlled manufacture of nanomaterials with consistent, reproducible and predictable quality. The scale up quantities of nano-powders from the pilot plant will allow industrial partners to perform prototyping or comprehensive commercial evaluation of nano-powders in a range of applications which they have hitherto not been able to conduct due to lack of sufficient high quality material. Importantly, the know-how acquired on the project and the proposed feasibility studies will reduce the risk and commercial barriers for industry that might consider building a larger industrial scale CHFS plant in the future.

The current advancement of technology very much depends upon the discovery of new materials. It has been known for some time that combinations of elements not involving carbon (called inorganic materials) can have important uses in areas from electronics, computing and UV protection in products, to harnessing energy from the sun. In particular, when inorganic particles are very small, typically made up of a few hundred atoms (called nanomaterials), they can have unusual and exciting properties. The discovery of such nanomaterials is very much hampered by our inability to make these materials fast enough and then to be able to test them adequately for their properties.The proposed research seeks to develop a new, faster way of making and discovering inorganic nanomaterials that can absorb sunlight (as an free energy source), and use this energy to split water into its constituents, hydrogen and oxygen (in a process known as photocatalysis). The hydrogen can then be used for powering cars or devices of the future. Such a process is important to sustain the energy requirements of mankind on this earth when our fossil fuels (e.g. oil) are exhausted.

Research on particle shape is extremely important to many industrial applications such as pharmaceuticals, biopharmaceuticals, human health products and speciality chemicals. For example, for pharmaceuticals, the morphology can affect important properties such as dry powder density, cohesion, and flowability, that can have major impact on a company's ability to formulate drug particles into finished products. Moreover, crystal morphology can affect drug dissolution, potentially affecting formulated product bioavailability and, in extreme, resulting in a companies loss of the license to making the drug product. However, despite the availability of various Process Analytical Technology (PAT) instruments for measuring other properties of particulate systems, there have been no effective on-line instruments capable of providing real-time information on particle shape during the processing of particles in unit operations such as crystallisation, precipitation, granulation and milling. In the past few years, on-line high speed imaging has shown to be a very promising PAT instrument for real-time measurement of particle shape on-line which has resulted in the development of some new instrumentation products just released to the market such as the PVM (Process Vision system) of Lasentec (uk.mt.com), the PIA (Process Image Analyser) of MessTechnik Schwartz GmbH (www.mts-duesseldorf.de), the ISPV (In-Situ Particle Viewer) of Perdix (www.perdix.nl) in Netherlands, and the On-line Microscopy systems of GlaxoSmithKline, some of which incorporate a probe design which allows easy access to a processing reactor vessel. However, all these techniques are essentially limited in that they can only provide 2D information of the particle shape. Hence, this proposed research aims to develop a new instrument Stereo Vision Probe which can directly image the full 3D shape of particles within a practical processing reactor. This basic mode of operation is based on the mathematical principle that if the 2D images of an object are obtained from two different angles, the full 3D particle shape can be recovered. The potential impact on research capability and industrial applications is predicted to be major but the proposed research will focus on the development of the Stereo Vision Probe and the 3D construction method from the two 2D images obtained from two different angles. The testing of the system will be mainly via the use of a variable temperature crystallisation cell.

A radical new technique is proposed for in-line process particle measurement at sizes from 0.1micron to 10micron and concentrations up to 50% by volume without interfering in the process. The method involves calculation of optical refractive index of the suspension from critical angle measurements at several wavelengths. This technique requires no light passage through the suspension so its turbidity does not restrict the method. In practice, the critical angle is not clearly marked for turbid suspensions but there is a substantial variation of reflectance in the vicinity of the critical angle.Measuring the suspension refractive index has significant advantages over other widely used non-invasive methods of particle analysis such as spectral extinction and laser diffraction: - The relationship between refractive index and volume fraction is linear for volumetric concentrations up to 50%.- Mie scattering theory can be used to calculate the refractive index of concentrated suspensions of spheres. - Suspension refractive index is sensitive to particle size and size distribution.