Five different molecular weight phenolphthalein poly(aryl ether ketone) (PEK-C) fractions in CHCl3 were studied by static and dynamic laser light scattering (LLS). The dynamic LLS revealed that the PEK-C samples contain some large polymer clusters. These large clusters can be removed by filtering the solution with a 0.1-µm filter. We found that the persistence length of PEK-C in CHCl3 at 25°C is ∼2 nm and the Flory characteristic ratio, C∞, is ∼25. Our results showed that 〈Rg 2 〉z 1/2 ) (3.50 ( 0.20) × 10 -2 Mw 0.54(0.01 and 〈D〉 ) (2.37 ( 0.05) × 10 -4 Mw -0.55(0.01 , with 〈Rg 2 〉z 1/2 , Mw, and 〈D〉 being the z-average radius of gyration, the weight-average molecular weight, and the z-average translational diffusion coefficient, respectively. A combination of static and dynamic LLS results enabled us to determine D ) (2.20 ( 0.10) × 10 -4 M -0.555(0.015 , where D and M correspond to monodisperse species. Using this calibration between D and M, we have determined molecular weight distributions of five PEK-C fractions from their corresponding translational diffusion coefficient distribution.