The ubiquitous presence of microplastics in freshwater sediments can pose detrimental impacts on ecosystems. However, the availability of effective extraction methods, and robust analytical techniques for identification, and quantification are still open questions. Based on sediment samples collected from Kedron Brook's six sites, the current study focused on the development of a cost-effective and reliable method for microplastics extraction which comprised of organic matter digestion with 30% H2O2 and initially CaCl2 and then ZnCl2 for dual-density separation. A light microscope and scanning electron microscope were used for initial visualisation and morphology characterisation. Micro-Fourier Transform Infrared Spectroscopy and pyrolysis gas chromatography-mass spectrometry (Py GC-MS) techniques were utilised for the final identification and quantification of the microplastics. The most common microplastics species were, polyethylene (PE), low density polyethylene (LDPE) and polypropylene (PP) homopolymers, along with PE:PP copolymers, with film and foam shapes being predominant and white, transparent, and brown as the most frequently observed colours. PE and PP reference samples were analysed using Py-GC-MS for quantification, yielding good calibration curves with a linear range and high R² values. These results demonstrate a promising approach for quantifying environmental samples without the need to dissolve plastic polymers in solvents.