During the construction of recording head devices, corrosion of metal features and subsequent deposition of corrosion by-products have been observed. Previous studies have determined that the use of N-methylpyrrolidone (NMP) may be a contributing factor. In this study, we report the use of a novel multiplatform analytical approach comprising of pH, liquid chromatography/UV detection (LC/UV), inductively coupled plasma optical emission spectroscopy (ICP-OES), and LC/mass spectrometry (LC/MS) to demonstrate that reaction conditions mimicking those of general photoresist removal processes can invoke the oxidation of NMP during the photolithography lift-off process. For the first time, we have confirmed that the oxidation of NMP lowers the pH, facilitating the dissolution of transition metals deposited on wafer substrates during post-mask and pre-lift-off processes in microelectronic fabrication. This negatively impacts upon the performance of the microelectronic device. Furthermore, it was shown that, by performing the process in an inert atmosphere, the oxidation of NMP was suppressed and the pH was stabilized, suggesting an affordable modification of the photolithography lift-off stage to enhance the quality of recording heads. This novel study has provided key data that may have a significant impact on current and future fabrication process design, optimization, and control. Results here suggest the inclusion of pH as a key process input variable (KPIV) during the design of new photoresist removal processes.