Thermoporometry (TPM) was applied to hydrotalcite precipitates prepared with carbonate, bicarboxylic acids and chloride. It was used to measure the formation of an ice body between the hydrotalcite particles. Before TPM could be applied, the dried hydrotalcite precipitate had to be soaked for two weeks in water. The mean value of a factor F measured by TPM, which described the shape of the ice body in hydrotalcite, was 1.7. This value was between those of a purely cylindrical (F = 2) and a purely spherical ice body (F = 1), indicating the formation of ice lenses. From the radius of the ice body, R
n, ice volume, V
n and shape factor F, the corresponding specific surface area of the hydrotalcite particles could be assessed. The TPM indicated that the distance between the separate hydrotalcite crystals in water, which is equal to 2(R
n+0.9) nm, was a function of the type of anion incorporated at the interlayer, such as chloride and bicarboxylic acid. The pore volume and surface area of the hydrotalcite particles measured by TPM were compared with those determined by the traditional nitrogen sorption technique on dried hydrotalcite. It appeared that sorption of N2 yielded much lower values than TPM. This difference was interpreted as being due to slow penetration of N2 through the dried hydrotalcite samples to the interparticle voids.