The rehydration and rehydroxylation properties of homoionic rectorites (saturated with Ca2+, Mg2+, Na+, or K+) were further investigated. The rehydration properties of the rectorite were characterized as follows: (1) basal spacings of rehydrated materials after heating above 500°C changed to 22.5 Å for H2O-complexes, 26.85 Å for ethylene glycol-complexes, and 27.65 Å for glycerol-complexes; (2) rehydrated Ca- and Mg-materials exhibited single layer hydrates at <50% RH, and rehydrated K-material showed double layer hydrates at 80% RH; (3) IR absorption spectra due to rehydrated H2O and OH exhibited the same or very close absorption intensities and frequencies to each other; (4) DTA-TGA curves of rehydrated materials indicated that the amount of rehydrated H2O approached about 4.2 wt. %, and about one-half of OH was rehydroxylated after heating at 800°C; and (5) interlayer cations of expandable layer components became non-exchangeable after heating above 500°C. These results suggest the following rehydration mechanism of rectorite: the interlayer cations migrate into the hexagonal holes of the SiO4 network by thermal dehydration. The cations migrated below 400°C easily return to the interlayer space and their original hydrated configurations have been recovered completely on rehydration. However, those migrated above 500°C are fixed to the hexagonal holes but water molecules are regained in the interlayer space. Consequently, electrostatic effects of interlayer cations on formation of water molecule layers are considerably reduced.

The sedimentary series from Academician Ridge, Lake Baikal, eastern Siberia, was examined using cation exchange capacity (CEC) to estimate the amount of expandable clay minerals (ECM) and high-temperature X-ray diffraction (HT-XRD) to determine their basic classification. The comparison of the magnetic susceptibility (MS) at sub-millennial resolution and the δl8O record of a reference Atlantic core (ODP 980) was used to create an age model. The most closely studied part of the series covered the major part of the last glacial cycle (120–20 ky BP). The HT-XRD analysis is based on monitoring the course of ECM dehydration with 5°C steps between 25 and 250°C and enabled us to improve the discrimination between ECM, chlorite and micas. The CEC obtained at millennial resolution showed that the neoformation of ECM in warmer periods of the last interglacial was either insignificant or fully compensated by their dissolution or dilution. The CEC record was correlated with the main climatic stages in the period studied. Both MS and CEC records reflected the environmental changes at about millennial resolution, including climatic instabilities between 117 and 73 ky BP (late MIS5).