In this study X-ray investigations of distilled and partly pyrolysed p
itches were performed at moderately small scattering angles. The avera
ge molecular diameters, determined from the peak maxima at moderately
small angles, increase with the temperature of heat treatment. In the
case of pitch distillation, the increase of the molecular diameter cor
relates with the increase of the glass transition temperature measured
by differential scanning calorimetry (d.s.c.). It was found that both
X-ray and d.s.c. methods are well adapted to check pitch transformati
on during heat treatment.