Double quantum nuclear magnetic resonance measurements exploiting the dipol
e coupling between the phosphorus atoms as well as a novel two-dimensional
exchange experiment using the scalar coupling are described for measuring t
he connectivities of phosphate tetrahedra in glasses. It is shown that bond
ing scenarios of up to four connected tetrahedra can be determined in phosp
hates and phosphate glasses and that estimations of the chain length distri
butions are possible in glasses having shorter chain fragments. Nuclear mag
netic resonance (NMR) is also capable of measuring local order in extruded
phosphate glasses using rotorsynchronized excitation in combination with ma
gic angle sample spinning. Finally, we show that the relative orientations
of chemical shift tensors can be determined by two-dimensional nuclear magn
etic resonance. This determination provides an additional verification of c
onnectivities and can possibly enable access to bonding angle data in the f
uture. (C) 2000 Elsevier Science B.V. All rights reserved.