The detection of emerging environmental contaminants at trace levels is a huge challenge for analytical research, and when expensive laboratory equipment is required, it is essential to provide a cheaper method that can ultimately undertake real-time sampling, whilst maintaining the sensitivity and reliability of current monitoring procedures. Electrochemical methods are a suitable candidate and studies into the development of submicron-gap generator-collector electrodes are provided alongside a variety of electrochemical methods. The aim of this project is to fabricate novel, low-cost, electrochemical devices with the potential for development into sensors for water quality monitoring. Nitrobenzene, Phosphate and Hydroquinone are the analytes used as they have well-known redox pathways and are known environmental pollutants and/or markers for other emerging contaminants. Initial studies examine the use of square wave voltammetry experiments in generator-collector mode, to provide information on either the fully reduced species or the intermediate species, depending on the buffered conditions used, with a view to detecting short-lived intermediates. Drawbacks with electrode geometry see the development of junction electrodes with larger active areas for greater sensitivity and changes in electrode materials for more robust device with a wider potential window. Generator-collector electrodes are also demonstrated as devices in electrochemical flow injection and for anion transfer at a triple phase boundary.