Origin of mixed-layered (R1) muscovite-chlorite in an anchizonal slate from Puncoviscana Formation (Salta Province, Argentina)

Mica-chlorite mixed-layering was identified by X-ray diffraction (XRD) as a major or subordinate constituent in several slates of the Puncoviscana Formation from Sierra de Mojotoro (Eastern Cordillera, NW Argentina). In order to determine the crystallochemical characteristics of these mixed-layered sequences and interpret their petrological meaning, anchizonal slate P90 was chosen for TEM observations. In this slate, dioctahedral mica and chlorite form interleaved phyllosilicate grains (IPG) or stacks, up to 110 um long, preferentially oriented with (001) planes at a high angle to the slaty cleavage but also oblique to S0.In agreement with XRD results, the main phyllosilicates identified by transmission electron microscopy (TEM) were dioctahedral mica and random mixed-layer muscovite-chlorite, with chlorite in subordinate amounts and scarce smectite. In the lattice-fringe images of mixed-layer packets, a sequence of irregular stacking that produced apparent 24 Å (10 + 14) layers was observed, but it was frequently possible to distinguish the 10 Å layers from adjacent 14 Å layers. In nearly all packets, 14 Å layers prevail, exhibiting 14 Å:10 Å ratios between 1:1 and 3:1. Some elongated lenticular fissures which are probably a consequence of layer collapse caused by the TEM vacuum were identified in these packets. The straight, continuous appearance of lattice fringes plus the scarce evidence of collapsed layers identified suggest that these packets correspond principally to mixed-layer muscovite-chlorite, which is confirmed by analytical electron microscopy analyses. However, smectite-like layers are probably the third component of some of these mixed-layer sequences, which may account for their high Si and low (Fe + Mg) contents, their low interlayer charge in relation to theoretical interlayer muscovite-chlorite, and for the presence of Ca in the interlayer site.Textural relationships between chlorite and muscovite packets in IPG along with the observed transformations from 14 Å to 10 Å along the layer, is compatible with a prograde metamorphic replacement of chlorite in stacks by dioctahedral mica layers, probably in the presence of an aqueous fluid.

Quantitative mineralogy of sedimentary rocks with emphasis on clays and with applications to K-Ar dating

Clays are the most complicated objects in quantitative mineral analysis of sedimentary rocks. Complex quantitative analysis of clays comprises four major steps: measuring bulk quantities, quantifying the mixed layering, determining the three-dimensional organization, and measuring the particle size. Computerization has resulted in major progress in all four areas during the last decade. X-ray diffraction remains the major tool of the quantitative studies of clays, supported by Fourier Transform Infrared Spectroscopy (bulk quantities), chemical analysis (bulk quantities) and electron microscopy (particle size). This contribution reviews recent developments in the techniques used for quantifying clays and their properties, and looks at the use of these quantification techniques in K-Ar dating of geological processes.

An empirical Scherrer equation for weakly swelling mixed-layer minerals, especially illite-smectite

The Scherrer equation links the measured width of an X-ray diffraction peak (Scherrer width, SW) to the number of stacked cells (N) in the direction normal to the diffracting planes. The formula is only valid for one d-value occurring in the coherently diffracting domain. This equation can be modified for weakly swelling mixed-layer minerals. This assumes that the peak broadening caused by the mixed-layering is proportional to the amount of swelling component (S) and that the effects of size and mixed-layering are additive.If two SW can be measured on XRD patterns from samples treated in two different ways (such as air dried or glycolated), N and S can be determined. This equation is applicable to illite-smectite mixed-layer minerals with high illitic content. The results are most accurate for N>30. The use of Scherrer's equation is discussed.

Diagenesis-very low-grade metamorphism of clastic Cambrian and Ordovician sedimentary rocks in the Iberian Range (Spain)

Cambrian and Ordovician pelites and greywakes from the Iberian Range were studied using XRD, EMPA and AEM/TEM techniques, lllite and chlorite are the main phases in Cambrian <2 µm fractions. Illites show crystallinities (IC) from 0.28 to 0.23°2θ the 2M1 is almost the only polytype; they do not have expandable layers, and they are heterogeneous in composition. Chlorites show two compositional types, both containing variable proportions of smectite-like layers. Clinochtores growing over bedding surfaces are also present. An evolutionary trend from anchizone to near the anchizone-epizone limit has been proposed for Cambrian samples.In the Ordovician <2 µm fractions, illites are associated with minor chlorites and kaolinites. The ICs range from 0.68-0.28°2θ the 2M1 polytype dominates over 1M, and it is associated with illitesmectite mixed-layering (R3 ordering). An evolutionary trend from diagenesis to low grade anchizone has been inferred.Chemical analyses of coarser detrital micas indicate muscovite and phengite compositions. The compositional heterogeneity exhibited by authigenic and detrital phases suggests that chemical equilibrium was not attained.

Structural investigations of mixed-layer smectite-illite clay minerals from North Sea oil source rocks

The purpose of the present investigation is to identify mixed-layering between illite and smectite in oil source rocks with HREM and electron diffraction. Smectite and mica are both groups within the 2:1 type of layer silicates. Illite is a commonly used term for micas in the fraction less than 2 microns. Illite has a fixed d(001) spacing of 10A. Smectite is able to swell from 10A to more than 18A under uptake of water or organic polar molecules. Mixed-layer illite-smectite is built of alternating layers of illite and smectite. Smectite and illite layers are recognized by x-ray diffraction (XRD) from their swelling characteristics, but cannot be distinguished in this way in HREM, because smectite layers tend to contract to 10A by evaporation of water in the vacuum of the microscope. Illites are identified by HREM as small packets showing very regular lattice fringes and smectites as highly imperfect, anastomosing layers showing very irregular lattice fringes (1).

Compositional variations in glauconite

Variation in composition, Fe3+/Fe2+ ratio, per cent mixed-layering, and d(060) spacing have been determined both between and within grains of glauconite from the Folkestone Beds at 286.5 m in the Tollgate bore, Sandwich, Kent. Grains extracted from the rock were classified on the basis of size into large (> 1 mm) and small (< 1 mm), and on colour into light and dark green. Large grains have a progressive increase in Fe3+/Fe2+ ratio with increase in total iron, while small grains have variable ratios; the largest variation is in the dark grains. The effect of the range of Fe3+/Fe2+ ratio variations on structural formula (e.g. R3+) is discussed. The per cent mixed-layering is not related to colour. There is a greater variation in Al, Fe, and K contents in and between large grains than small grains. Both sizes of grains may be separated on d(060) spacings determined by X-ray diffraction. Glauconite from coral and gastropod casts has different d(060) spacings than that from bryozoan casts and variegated grains, but is similar to the small grains. Large light grains may have developed from small light grains but it is unlikely that the large dark grains developed from small dark grains. The large grains probably all formed under similar conditions, with a common origin; the small from several sources or from a single source under a variety of conditions.