Siltstones from the Precambrian Freda Formation in Wisconsin have been studied by scanning, scanning-transmission and analytical electron microscopy (SEM, STEM and AEM), and X-ray diffraction (XRD). XRD data for drill core samples show a change from smectite-rich Illite-Smectite (I-S) in shallow samples to illite in deeper samples, implying a transition during burial diagenesis.

Transmission electron microscopy (TEM) observations of shallow samples reveal the presence of three clearly distinguishable kinds of dioctahedral clay minerals: (1) detrital grains of micrometer-sized, mature muscovite; (2) small packets in the matrix consisting of dominant (Reichweite) R1 I-S or (3) small packets of illite. The illite and I-S stacks occur separately and have similar textures, with packet thicknesses averaging ∼400 Å, within the range of anchizonal illite. Illite and detrital muscovite commonly display strain features typical of the effects of tectonic stress. Void space within I-S or illite packets is inferred to be a strain feature, and to have served as pathways for fluids. Detrital muscovite shows abundant alteration features including (001) boundaries which are continuous with parallel packets of I-S; individual layers commonly show along-layer transitions of muscovite to smectite or I-S. Trioctahedral clays consist primarily of detrital chlorite which commonly shows direct alteration to R1 I-S and smectite, as with detrital muscovite.

Deep samples contain only unaltered, coarse detrital muscovite, and thin packets of illite forming stacks and comprising most of the matrix. The texture of the illite appears to be identical to that of shallow samples, with characteristics such as packet size typical of anchizonal illite. Trioctahedral clays consist almost entirely of detrital grains of chlorite and corrensite. They occur as separate grains with rather constant composition, without signs of alteration.

The data imply that all of the studied rocks have been subjected to a uniform anchizonal grade of metamorphism in which detrital grains were largely unchanged but matrix clays were transformed to packets of illite. The unusually abrupt transition with depth from highly expandable I-S to illite is inferred to actually be the result of subsequent alteration of authigenic illite and detrital chlorite and muscovite to R1 I-S and smectite in shallow rocks. This late overprinting of the anchimetamorphic clay mineral assemblage is inferred to have been locally caused by fluids with temperatures less than those of peak metamorphism. This process, called “retrograde diagenesis”, gave rise to a sequence of dioctahedral I-S and illite which mimics classic prograde sequences. Interpretations of such sequences as being prograde, especially in cases of ancient rocks, should be interpreted with caution when high-resolution images of textures are not available.

Variations in clay mineral assemblages, changes in Kübler index (KI), and the chemical composition of chlorites are used to identify source areas in the lacustrine materials in the Lower Cretaceous Leza Limestone Formation of the Cameros Basin, northern Spain. This formation has fairly homogeneous lithological characteristics and facies associations which do not allow for identification and characterization of local source areas. The Arnedillo lithosome of the Leza Limestone Formation contains a clay mineral association (Mg-chlorite, illite and smectite) indicative of its provenance. Chlorite composition and illite KI values indicate that these minerals were formed at temperatures higher than those reached by the Leza Formation which indicates its detrital origin. The similarity in the Mg-chlorite composition between the Arnedillo lithosome and the Keuper sediments of the area indicates that these materials acted as a local source area. This implies that Triassic sediments were exposed, at least locally, at the time of deposition of the Leza Formation. The presence of smectite in the Leza Formation is related to a retrograde diagenesis event that altered the Mg-chlorites in some samples.

This study characterizes the effects of fluid migration into a predominantly shale cover which seals the active geothermal system of Mt. Amiata (Tuscany, Italy). During Alpine orogenesis the shale unit was affected by regional metamorphism at the limit of the diagenesis-anchizone. Subsequently, the phyllosilicate clay minerals of the shales underwent significant alteration at diagenetic temperatures (175±25ºC as determined by the geochemical model) by the pervasive circulation of fluids activated by the geothermal field. The overall mineralogical assemblages indicate that the main transformations consisted mostly of destabilization of illite and formation of kaolinite together with large amounts of I-S mixed layers, with higher smectite content and decreased Reichweite I-S ordering (from R3 to R1) with respect to the original, unaltered phases. Application of computer modelling indicates that the circulation of CO2-rich geothermal fluids into the shale unit was responsible for the observed phyllosilicate clay mineral transformations.