A general growth in the polymers production and consumption leads to an increase in the new types of wastes. In conjunction with the lack of secondary recycling power this fact is being a reason for appearance of a new processes that is potentially destructive for the environment. In particular, plastic wastes that is being stored in the wastewater of a large cities under a combination of aggressive factors action such as humidity, mechanical and UV-erosion degrades into a small-size particles, famously known as microplastics (MP). The study presented is devoted to the methodology development for acquisition, quantitative and qualitative analysis of wastewater derived microplastics. An experimental part deals with real wastewater samples collected at different infrastructurally-important objects of Rostov-on-Don and Aksai cities. For all the sampling locations the presence of urban-generated MP particles is approved. The results show that the research methods used are able to satisfy the output data quality conditions. However, the significant time and cost consumption of the research chain developed limits its wide practical application.