By avoiding chemical fixation and using a freeze-drying technique, it proved possible to examine the enamel organ of rat mandibular incisors histologically while retaining the adjacent enamel of the same tooth for chemical analysis. The dramatic alterations which occur in enamel organ histology, such as ameloblast shortening and the development of hte papillary layer, could then be compared directly with mineral uptake and mineral content of the adjacent enamel. Both enamel and adjacent enamel organ were sampled as a continuous series of pieces, 0.5 mm in width, from youngest (apical) to oldest (incisal) tissue. Short ameloblasts were associated directly with the beginning of a rapid uptake of phosphate ions during the maturation phase and also coincided with the beginning of a steep rise in mineral content. By implication, some loss of matrix may also occur at this point. Development of the highly vascular papillary layer preceded ameloblast shortening and may be associated with changes in the organic matrix prior to its disappearance from the tissue. Further development of this layer was associated with ameloblast shortening. This may also therefore be associated with mineral uptake during maturation.