We analyze the individual properties of the resulting materials using optical microscopy and subsequently we use complementary techniques to confirm our findings. While most 'naturally' formed microplastics are generated at temperatures similar to room temperature, further investigations and comparisons with existing models are required to understand any discrepancy between the resulting size and shape distributions of cryo-milled and naturally formed MPs. We briefly demonstrated the utilization of the obtained materials in an exemplary method development process: a broad range of particulate matter is present in an environmental sample, but the µ-Raman analysis does not allow for conclusive results (partly due to the unspecific rubber signal). Spiking with a known sample allows for optimization of measurement conditions and paves the way for streamlined MP identification and quantification.