This paper presents results of steady state fluorescence spectra measu
rements on polyindene (PIN) and polyacenaphthylene (PAN) samples of di
fferent molecular weights, in dilute solution at constant temperature,
25 degrees C. Solvents were prepared by mixing a solvent and a precip
itant in different proportions. Large changes in the size of the parti
cles in solution (determined by turbidimetric methods) caused by incip
ient phase separation were necessary to produce significant changes of
the excimer to monomer fluorescence ratio for both PIN and PAN. A lin
ear relationship between the excimer to monomer fluorescence ratio and
the volume of the polymer aggregates is found. Such a relationship is
solvent viscosity independent. Several conclusions are drawn about th
e phase separation process in very dilute polymer solutions.