The peculiarities of viscosity data treatment for two series of polymer systems exhibiting associative properties: brush-like amphiphilic copolymers—charged alkylated N-methyl-N-vinylacetamide and N-methyl-N-vinylamine copolymer (MVAA-co-MVACnH2n+1) and charged chains of sodium polystyrene-4-sulfonate (PSSNa) in large-scale molecular masses (MM) and in extreme-scale of the ionic strength of solutions were considered in this study. The interest in amphiphilic macromolecular systems is explained by the fact that they are considered as micellar-forming structures in aqueous solutions, and these structures are able to carry hydrophobic biologically active compounds. In the case of appearing the hydrophobic interactions, attention was paid to discussing convenient ways to extract the correct value of intrinsic viscosity [η]
from the combined analysis of Kraemer and Huggins plots, which were considered as twin plots. Systems and situations were demonstrated where intrachain hydrophobic interactions occurred. The obtained data were discussed in terms of lnηr
vs. c[η]
plots as well as in terms of normalized scaling relationships where ηr
was the relative viscosity of the polymer solution. The first plot allowed for the detection and calibration of hydrophobic interactions in polymer chains, while the second plot allowed for the monitoring of the change in the size of charged chains depending on the ionic strength of solutions.