This thesis is a study into the application of separation techniques to the analysis of both industrial and environmental sample matrices. Chapter 1 is a literature survey into the background of adhesives (both anaerobic and cyanoacrylic adhesives). The literature survey also details the composition of adhesives and their analysis. Chapter 2 details an analytical study into the decomposition of the key reducing agents found in anaerobic adhesives, including acetyl phenylhydrazine, tetrahydroquinoline, dimethyl-/?-toluidine and (p-toluene suphonyl) hydrazine. A suitable HPLC separation system was developed, which was then used to monitor any decomposition of the reducing agents. Investigation of the above was carried out in the presence of saccharin, maleic acid and cumene hydroperoxide (both in the presence and absence of the transition metals, copper and iron). Comparison of the rates of decomposition of the reducing agents revealed some information into the role of the acids and peroxide in the overall reaction mechanism. The products produced as a result of these reactions were also identified using preparative TLC and techniques such as IR, NMR and mass spectrometry. Chapter 3 details the development of a suitable method of anion separation using capillary electrophoresis. A suitable extraction technique was also developed which could extract the anions from the adhesive mixture (both crude and distilled preparations), into an aqueous medium. The method developed was amenable to the analysis of the full range of cyanoacrylate adhesive mixtures (methyl-, ethyl-, butyland methoxy ethyl-cyanoacrylates). Chapter 4 involved the development of an electrochemical system that was capable of detecting microcystins. The work also involved HPLC mobile phase optimisation, microcystin purification and microcystin extraction (both from ‘pure bacterial cultures’ and field samples). An electrochemical detector was developed which was capable of detecting microcystins, it was also capable of detecting other polypeptides (found in partially purified microcystins) which were not detected using UV detection. The main problem encountered was the detection of the microcystins in field samples as other proteins found in field samples were also electrochemically active. Conclusions drawn from the work carried out in the thesis, and suggestions for future research are outlined in Chapter 5.