Transparent and colorless AlPO4 gel and glass are prepared via a simple aqueous sol-gel route using aluminum lactate and phosphoric acid as precursors. The stoichiometric AlPO4 glass derived from this sol-gel route has a mesoporous structure with a surface area of 504 m(2)/g after calcination to 600 degrees C. With increasing gel-to-glass processing temperature, the average degree of P/Al connectivity increases. After sample calcination at 600 degrees C for 4 h, Al-27 MAS NMR spectra indicate that aluminum is almost completely converted into AlO4 units. Al-27{P-31} rotational echo double resonance and P-31{Al-27} rotational echo adiabatic passage double resonance NMR experiments as well as Al-27 and P-31 MAS NMR results further confirm that the prepared AlPO4 glass has a three-dimensional network based on alternating Al(OP)(4) and P(OAl)(4) tetrahedral units in analogy to the local structure of crystalline AlPO4.