We present a protocol to remove polyvinyl chloride-based microplastics (MPs) from aquatic environments using jute stick activated charcoal (JSAC) as an adsorbent. We describe steps for preparing JSAC by pyrolyzing jute sticks at high temperatures without oxygen, followed by chemical activation with HCl. We also detail the procedures for the post-functionalization of JSAC and for the collection, processing, and measurement of MPs. For complete details on the use and execution of this protocol, please refer to Alom et al.