Upper Triassic sandy horizons in the Paris Basin were sampled at depths ranging from outcrop in the northeast to 2,700 m in the centre of the basin. The smallest clay sub-fractions (<0.2 μm) from the deepest central samples consist mainly of illite and chlorite whose K-Ar age is ∼ 190 Ma. These minerals formed at a relatively high temperature of 220-250°C, as determined from the oxygen isotope fractionation between authigenic illite and associated quartz overgrowths, but at a burial depth of only 500 m. In a nearby drillhole that crosscuts a fault zone reactivated during the 190 Ma event, illite is less well-crystallized and has a higher δ18O value suggesting different physical and chemical conditions of formation during the same hydrothermal episode. Two other generations of illite-smectite mixed-layer clays formed in the same Triassic horizon: one at ∼150 Ma and the other at ∼80 Ma. These younger clays have higher δ18O values and thus may have formed at somewhat lower temperatures. The δ18O values of the fluids from which the different illite-smectite mixed-layer minerals form range from +9 to +13.5 per mil (SMOW).

An Ar diffusion code was used to estimate, on the basis of the Ar loss of the clay-type material, the duration of these events. The results suggest that the duration of the hydrothermal events at 190 Ma and 150 Ma were rather short, <1 Ma, whereas the youngest event was protracted over a much longer period of ∼37 Ma. Comparison between K-Ar ages of the different mixed-layer minerals and sedimentation rates of the sediments since the Palaeozoic shows significant accelerations of the rates at ∼ 190-200 Ma and 150 Ma, and a less important one at ∼80 Ma. These observations provide additional evidence that the first two events were promoted by basement-related tectono-thermal activities. The third event is considered to be of diagenetic origin.

Chemical analyses of the <0.2 μm illite-smectite (I-S) fraction from K-bentonites in Silurian age sediments sampled from three different localities in the Southern Uplands of Scotland and Northern Ireland indicate that the I-S from the three localities shows differences in both K+ content and the degree of Tschermak substitution of octahedral Al3+ for Mg2+. The K+ content correlates with percentage expandability (%E) of I-S as determined by X-ray diffraction (XRD), but both these parameters show poor correlation with palaeotemperature as estimated by organic reflectance methods. Octahedral Mg2+ content shows an inverse correlation with Al3+, and both these parameters show a good correlation with estimated palaeotemperature. Although K-substitution has been retarded at Dob's Linn, the region subjected to the highest temperature, Tschermak substitution of Al3+ for Mg2+ has apparently continued. In these K-bentonites, Tschermak substitution appears to be a better indicator of palaeotemperature than K-substitution.

Current methods of quantitative whole-rock clay mineral analysis of sandstones often provide little more than an estimate of clay mineral abundances, especially where the total clay mineral content is <10 wt% of the sandstone. More accurate determinations of clay mineral abundance in the whole rock can be made by combining thermogravimetry/evolved water analysis (TG/EWA) and X-ray diffraction (XRD) data. The TGA/EWA system incorporates a purpose built thermobalance linked to a water specific infrared detector which is used to measure quantitatively the clay mineral dehydroxylation water evolved from the whole rock when heated from 250°C to 900°C. This gives a measure of the total hydroxyl content of the clay minerals in the whole rock which, when combined with XRD analysis of a separated clay size-fraction, enables individual clay mineral abundances in the whole-rock sample to be determined. Results on artificial sand/clay mineral mixtures prepared with known amounts of different clay minerals (chlorite, illite and kaolinite) show that the accuracy of the combined method is most influenced by the accuracy of the XRD data. Errors associated with TG/EWA were found to be negligible by comparison. A case study is included in which the technique has been used to determine accurately the illite abundance in the Magnus Sandstone Reservoir, Northern North Sea.

Pisolites in the bauxitic laterites of Darling Range, Western Australia may contain up to 50% AI2O3, although no major Al-containing phases can be identified using standard X-ray diffraction techniques. These pisolites have been investigated using a range of techniques, and it has been demonstrated that Al is present in the form of x-alumina, a poorly crystalline form of A12O3. The x-alumina exhibits an indurating morphology and appears to have formed from a hydrated precursor.

Seven samples from a chronosequence of soils developed in historically created polders on the Atlantic coast (Marais Poitevin, Vendée, France) were investigated in order to illustrate the rate of mineralogical change in a clay-dominated system. The oldest polder was constructed in 1665, the last one in 1912; thus the time span of soil evolution is from 80 to 330 years. All the samples had more than 50% clay (<2 μm). The most reactive, fine clay sub-fraction (<0.1 μm) was investigated in detail by X-ray diffraction and chemical analysis. The observed mineralogical changes with increasing age followed the schematic reaction:

smectite + mica = illite + mixed-layer minerals.

The progress of reaction in time appears to be non-linear. This reaction seems to occur in a chemically constant system, and the mineralogical change can be seen as a readjustment of species to a given chemical composition.

Measurements of the kinetics of acid dissolution of synthetic aluminous goethites and corresponding hematites produced by heating of parent Al-goethites at various temperatures were carried out in 1 M HC1 at 30, 40 and 50°C. Dissolution-time curves show sigmoidal shapes for the goethites (110°C), whereas deceleratory shapes were obtained for most of the partly and fully dehydroxylated samples. The dissolution rate for all materials decreased with increasing Al substitution and increased with increasing dissolution temperature, specific surface area and heating temperature. On a unit surface area basis, hematite dissolved ∼ 2–8 times faster than goethite. Dissolution kinetics of most heated goethite samples (200–260°C) were quite well described (R2 > 0.96) by the modified first-order Kabai equation. The activation energy and frequency factor for dissolution increased with increasing Al substitution.

Any X-ray diffraction (XRD) pattern of mixed-layered maximum R1 ordered chlorite-smectite has an exact equivalent R0 smectite-corrensite or R0 chlorite-corrensite. The identification of a mineral as chlorite (0.8)-smectite R1 is, therefore, not evidence that the fundamental layers in such an interstratified structure are actually chlorite and smectite. Furthermore, there are no obvious differences between XRD patterns of R0 and R1 chlorite-smectite at high or low smectite contents. Therefore the frequently supposed identification of R0 chlorite-smectite with high smectite contents is also questionable. It follows that the identification of R1 chlorite (0.8)-smectite by Robinson & Bevins (1994) and of R0 chlorite (≈0.2)-smectite in an earlier publication (Robinson et al.,1993) cannot be used as evidence regarding the debate over the nature of the component layers in interstratified minerals intermediate between trioctahedral smectite and chlorite.

Diffraction patterns of natural mixed-layer chlorite minerals from metabasites often show a strong reflection at 31 Å yet a lack of resolution of other mixed-layer peaks from those of discrete chlorite. These features cannot be matched by any single mixed-layer mineral consisting of layers of chlorite and smectite and were matched by Robinson & Bevins (1994) using a mixture of different chlorite-smectite minerals. However, they can be matched by a single chlorite-corrensite mineral in which there is an element of segregation of layer types. These different possibilities need to be investigated further.