Accurate mass balance is an important requirement, especially for mass calibration procedures. It has been observed that with high-resolution apparatus, some volume underestimation, probably due to dead times during channelization, may occur. In this paper, a procedure based on poly(styrene-divinylbenzene) latex standard suspensions is proposed to assess the accuracy of volume measurements. Such a procedure was followed to evaluate the volume measurement accuracy and precision of a Coulter Counter TAII, which is generally considered an accurate counter, and of a Coulter Multisizer II (software 2.1), a high-resolution apparatus. No differences in accuracy and precision were found between the two instruments. Both of them were found suitable for particulate volume measurements provided that an adequate number of replicates is performed.