>Magister Scientiae - MSc / Polymer electrolyte membrane fuel cells (PEMFCs) among other fuel cells are considered the best candidate for commercialization of portable and transportation applications because of their high energy conversion and low pollutant emission. Recently, there has been significant interest in high temperature polymer electrolyte membrane fuel cells (HT-PEMFCs), due to certain advantages such as simplified system and better tolerance to CO poisoning. Cost, durability and the reliability are delaying the commercialization of PEM fuel cell technology. Above all durability is the most critical issue and it influences the other two issues. The main objective of this work is to study the durability of membrane electrode assemblies (MEAs) for HT-PEMFC. In this study the investigation of commercial MEAs was done by evaluating their performance through polarization studies on a single cell, including using pure hydrogen and hydrogen containing various concentrations of CO as fuel, and to study the performance of the MEAs at various operating temperatures. The durability of the MEAs was evaluated by carrying out long term studies with a fixed load, temperature cycling and open circuit voltage degradation. Among the parameters studied, significant loss in the performance of the MEAs was noted during temperature cycling. The effect of temperature cycling on the performance of the cell showed that the performance decreases with increasing no. of cycles. This could be due to leaching of acid from the cell or loss of electrochemically active surface area caused by Pt particle size growth. For example at 160°C, a performance loss of 3.5% was obtained after the first cycle, but after the fourth cycle a huge loss of 80.8% was obtained. The in-house MEAs with Pt-based binary catalysts as anodes were studied for CO tolerance, performance and durability. A comparison of polarization curves between commercial and in-house MEAs illustrated that commercial MEA gave better performance, obtaining 0.52 A/cm² at 0.5V and temperature of 160°C, with in-house giving 0.39A/cm² using same parameters as commercial. The CO tolerance of both commercial and in-house MEA was found to be similar. In order to increase the CO tolerance of the in-house MEAs, Pt based binary catalysts were employed as anodesand the performance was investigated In-house MEAs with Pt/C and Pt-based binary catalysts were compared and a better performance was observed for Pt/C than Pt-alloy catalysts with Pt-Co/C showing comparable performance. At 0.5 V the performance obtained was 0.39 A/cm2 for Pt/C, and 0.34A/cm²,0.28A/cm²,0.27A/cm² and 0.16A/cm² were obtained for Pt-Co/C, Pt-Fe/C, Pt-Cu/C and Pt-Ni respectively. When the binary catalysts were tested for CO tolerance, Pt-Co showed no significant loss in performance when hydrogen containing CO was used as anode fuel. Scanning electron microscopy (SEM) revealed delamination between the electrodes and membrane of the tested and untested MEA's. Membrane thinning was noted and carbon corrosion was observed from the tested micro-porous layer between the gas diffusion layer (GDL) and catalyst layer (CL).