The present article studies the structure of annealed viscose fibers interferometrically at a constant temperature of 100 ± 1°C at different times. The Pluta polarizing interference microscope has been used for determining the mean refractive indices and mean birefringence. The results were used to calculate the optical orientation function and the angle of orientation. The value (Δα/3α0), which depends on the molecular structure of the polymer, remains constant. Relationships between the mean refractive indices, birefringence, isotopic refgractive index, and polarizabilities per unit volume with different times were given for these fibers. The samples were subjected to X-ray diffraction to clarify the variation of crystallinity with the annealing conditions. Differential thermal analysis measurements were used to determine the glass transition temperature of viscose fiber. Measurements of the volume swelling parameter of the viscose fibers with different liquids were given. Also, determinations of Cauchy's constants, dispersive power, and dielectric constant at infinity were carried out. Illustrations are given using graphs and microinterferograms. © 1999 John Wiley & Sons, Inc. J Appl Polym Sci 71: 361–369, 1999