NMR cryoporometry with octamethylcyclotetrasiloxane as a probe liquid. Accessing large pores.

Octamethylcyclotetrasiloxane is presented and investigated as probe liquid for NMR cryoporometry or DSC-based thermoporometry. This compound which may imbibe into both hydrophilic and hydrophobic pores is shown to exhibit a melting point depression that is larger than that for other cryoporometric probe materials such as cyclohexane. The transverse relaxation time differs by more than three orders of magnitude between the solid and liquid states, separated by a sharp phase transition. Hence, as demonstrated in controlled pore glasses, octamethylcyclotetrasiloxane can provide pore size distributions for materials with pore sizes up to the micrometer range.

Inorganic salt hydrates as cryoporometric probe materials to obtain pore size distribution.

The depression of the melting temperature of Zn(NO3)2.6H2O was used to obtain the pore size distributions in controlled pore glasses. Measured by 1H NMR, the average value of the temperature depression DeltaT and the known average pore size yield K=DeltaT.d approximately 116 K.nm as the material-dependent factor for Zn(NO3)2.6H2O in the Gibbs-Thompson equation. The melting temperature is close to room temperature. Hence, this salt hydrate and some related other ones are better materials than water (K approximately 50 K.nm) for cryoporometric studies of systems with hydrophilic pores. The data also provide 46 mN/m for the solid-liquid surface tension of this salt hydrate.