Important new information about the crystal structure of dicalcium pho
sphate (DCP) powders was obtained using the P-31 NMR technique. There
were two types of powders under investigation. One type includes pure
DA (CaHPO4) and DH (CaHPO4 . 2H(2)O) powders, and their mixtures in di
fferent proportions. The other includes powders from an industrial pro
duction. They were obtained by DH heating. An effective and fast metho
d of identification of the structure of the nuclear nearest surroundin
gs is presented, Determination of the concentration of nearest surroun
dings corresponding to DA or DH types for the P-31 nuclei was demonstr
ated on examples taken from production powders. Good agreement was fou
nd in comparison with data obtained by chemical analysis, Especially i
nteresting information is obtained by using the CP MAS NMR technique.
This method allows the following conclusions about the production samp
le structure to be drawn: it is a powder consisting of DH-type microcr
ystals, but with numerous vacancies at the positions of water molecule
s which disappeared during heating.