The morphology of polymer nanocomposites is usually characterized by various methods like X-ray diffraction (XRD) or transmission electron microscopy (TEM). In this work, a new approach for characterizing nanocomposites is developed: the results of small angle x-ray scattering, on-line extensional rheometry (level of melt strength) and Young's modulus out of tensile test are correlated with those of near infrared (NIR) spectroscopy. The disadvantages of the common characterization methods are high costs and very time consuming sample preparation and testing. In contrast, NIR spectroscopy has the advantage to be measured inline and in real time directly in the melt. The results were obtained for different aggregate states (NIR spectroscopy and on-line rheotens test in melt state, tensile test, and XRD in solid state). Therefore, important factors like crystallization could not be considered. Nevertheless, this work demonstrates that the NIR-technology is perfectly suitable for quantitative in-line characterization. The results show that, by the installation of a NIR spectrometer on a nanocomposite-processing compounder, a powerful instrument for quality control and optimization of compounding process, in terms of increased and constant quality, is available.

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In product development, it is crucial to choose the appropriate drug manufacturing route accurately and timely and to ensure that the technique selected is suitable for achieving the desired product quality. Guided by the QbD principles, the pharmaceutical industry is currently transitioning from batch to continuous manufacturing. In this context, process understanding and prediction are becoming even more important. With regard to hot melt extrusion, the process setup, optimization and scale-up in early stages of product development are particularly challenging due to poor process understanding, complex product-process relationship and a small amount of premix available for extensive experimental studies. Hence, automated, quick and reliable process setup and scale-up requires simulation tools that are accurate enough to capture the process and determine the product-process relationships. To this end, the effect of process settings on the degradation of the active pharmaceutical ingredient (API) in a lab-scale Leistritz ZSE12 extruder was investigated. As part of the presented study, the limitations of traditional process analysis using integral process values were investigated, together with the potential that simulations may have in predicting the process performance and the product quality. The results of our investigation indicate that the average melt temperatures and the exposure times in specific zones along the screw configuration correlate well with the API degradation values and can be used as potent process design criteria to simplify the process development.