The ultrasonic attenuation (UA) technique was developed to measure not only particle size distribution (PSD) but also concentration for on-line and off-line analysis of high concentration dispersions. Another significant characteristic along with particle size is particle shape. Particle shape influences the apparent particle size as measured by various instruments. Shape factors have been calculated from microscopic images using conventional image analysis (IA) techniques. Particle sizing data measured by UA is more representative than by IA because much larger samples are used for analysis. In this study UA, laser diffraction (LD) and IA size measurements are compared and the influence of particle shape is investigated. Data obtained from UA has been combined with information on shape factor from imaging to obtain equivalent particle size distributions. In a previous study [1], the influence of shape on size measurement has been investigated using different sizing techniques for non-fragile materials. These particles showed significant variation in measured PSD with their different shapes. In this paper, the same phenomenon was observed with evolving polymorphs of L-glutamic acid crystals (alpha and beta form), oxalic acid, sucrose and monosodium glutamate.