We present a methodology for mass and size dispersity analysis by MALDI-TOF mass spectrometry of lyothermally grown 2.5-3.7 nm ZnS nanocrystals having a Zn blende crystal structure. These results correlate with information obtained by TEM and absorption spectroscopy. The use of MS methods to probe size and size dispersity provides a convenient method to rapidly analyze II-VI materials at the nanoscale. We believe these results represent the first mass spectrometric analysis of size and size dispersities on II-VI nanocrystals.