A novel isotachophoresis (ITP) injector geometry was designed and was the subject of a joint patent application with Siemens. This design enabled variable volume sample injections to be performed reliably and simply. Prototype devices were fabricated from polymethylmethacrylate (PMMA) using a rapid direct micromachining technique. The use of these microdevices with a purpose designed and constructed fluid handling system (which enabled automatic delivery of samples and electrolytes) allowed the suitability of the devices for on-line monitoring to be assessed. Based on the outcome of this an industrial MEWAPREV monitoring system was designed and constructed which enables on-line at site analysis of aqueous sample streams. Software was specifically written to permit full control of all the equipment required (i.e. HV power supplies, valves, pumps and detectors). In addition extensive work has been carried out on the development of electrolyte systems for separation of numerous metal ions (Ca, Mg, Mn, Cr, Co, Fe, Ni, Zn, Cu). The developed systems were applied to the analysis of provided metal waste streams. Although in this project only metal ions were studied, there is a huge potential market for analysing other ionic species present in industrial process streams. The instrument itself could also be used for analysing process streams from different industries.