Poly-N-isopropylacrylamide (PNIPAm), a thermorresponsive polymer, highly soluble in water below its lower critical solution temperature (LCST), is widely used in biomedical applications like drug delivery. Being able to measure PNIPAm size and aggregation state in solution quickly, inexpensively, and accurately below the LCST is critical when stoichiometric particle or molecular ratios are required. Dynamic light scattering (DLS) is probably the most widely available, and inexpensive nanoparticle sizing technique, but there are limitations with respect to sample polydispersity. Here, we first investigated factors governing the ability of DLS to accurately measure PNIPAm size in solution at 25 °C as part of a quality study of five different molecular weight, commercially sourced PNIPAm. All samples were polydisperse and accurate particle size distribution (PSD) data was only obtained from distribution fitting, being consistent and accurate down to ∼ 0.1 wt%. In water at 1 wt%, R