Leyssens, TomGraffeo SabrinaAerts LucBostijn NilsMagnée, HectorHectorMagnée2025-07-022025-07-022025-06-0420252025-06-04https://hdl.handle.net/2078.2/43395This thesis investigates the miniaturisation and optimisation of polymorph screening techniques in the pharmaceutical industry, with a focus on high-throughput development and solid-state characterisation. Conducted in collaboration with UCB Pharma, the research is divided into two main parts. The first part investigates and compares spectroscopic techniques- NIR hyperspectral imaging, MIR microscopy and Raman microscopy- for their ability to detect and map polymorphs and low-dose compounds within pharmaceutical solids. Particular emphasis is placed on method development, sample holder evaluation and compound discrimination in complex matrices. The second part presents the design, validation and application of a high throughput platform capable of supporting XRPD and Raman transmission analysis. Using customised well plates (Kapton, quartz and silicon), this platform allows the simultaneous analysis of multiple samples while significantly reducing material consumption, waste and preparation time. Experiments on model compounds such as mannitol and brivaracetam demonstrated the robustness, reproducibility and sensitivity of the platform. Data processing methods such as PCA and cluster analysis further streamlined the interpretation of large data sets. Overall, this work demonstrates a promising approach to sustainable and efficient polymorph screening by combining analytical method development with technical innovation. The results have direct implications for early phase pharmaceutical development, enabling faster decision making and reducing resource use.XRPDpolymorphhigh-throughputspectroscopymulti well platesilicon plateMiniaturisation of polymorph screening, potentials and developmenttext::thesis::master thesis