Interactions of ammonium sulphates and various silicate and oxide minerals have been studied by X-ray heating methods and simultaneous TG-DTA. Kaolinite and other clay minerals were found to be very susceptible to these sulphating treatments, (NH4)3Al(SO4)3, (NH4)Al(SO4)2 and Al2(SO4)3 being formed successively with increasing temperature from 350 to ∼550°C. The same reaction products were obtained on heating mixtures of (NH4)2SO4 and γ-Al2O3, Al(OH)3 and bauxite. Fe-, Mg- and Ti-silicates and oxides gave NH4-double sulphates below 400°C and the corresponding metal sulphates above this temperature.

X-ray diffraction, optical and microprobe studies of a kaolinized oligoclase—orthoclase—two-mica—granite (Southern Armorican Massif) indicated that low-temperature metasomatism had produced three series of minerals. 1. Partial alteration of muscovite resulted in the formation of ferrous-magnesium-phengite. Biotite was destabilized to a kaolinite-titanium oxide assemblage. 2. Phengite, unreacted muscovite and feldspars recrystallized to an aluminous, magnesian 1M sericite mineral ranging in composition from mica to illite. 3. Feldspars were entirely destabilized to produce the assemblage potassic-beidellite-kaolinite—Al-illite. Kaolinite was the predominant mineral in the most altered rock. A fourth stage of mineral equilibrium was also observed; this occurred after material from stage 3 had been reworked. In this environment, the potassic-beidellite was replaced by a calcic-montmorillonite. Potassic-beidellite was not stable under weathering conditions.

La determinación del orden o desorden en la dirección perpendicular a las láminas en una nontronita anhidra ha sido efectuada a partir de las reflexiones 001 y 003 y de una parte de la difusión a pequeños ángulos. Mediante la comparación de diagramas experimentales y curvas calculadas a partir de modelos, se pretende poner en evidencia si el sistema es ordenado o desordenado y en el segundo caso la manera de establecer un modelo que traduzca el desorden del sistema. Se llega a la conclusión de que la nontronita potásica anhidra es un sistema desordenado en la dirección perpendicular a las láminas en el que aparecen espaciados correspondientes a varias distancias discretas afectadas por proporciones determinadas.

Under the influence of a pulsed field, dilute clay sols become birefringent as the particles undergo orientational order. The rate of decay of the birefringence on removal of the field is characteristic of the particle geometry. Measurement of the decay rates under two specific experimental conditions provides sufficient information from which the particle-size distribution can be evaluated in terms of a two-parameter function. Experimental data are reported and analysed in terms of a log-normal distribution of particle sizes for attapulgite (rods), kaolinite (discs) and halloysite (ellipsoids) sols and compared with success to electron microscopic data. The ability of the method to determine size distributions in terms of the major dimensions of the clay particles, rather than those of the often used equivalent sphere, is highlighted.

Le mécanisme de dispersion dans l'eau d'une smectite a été étudié en fonction de 2 paramètres: la nature du cation interlamellaire, la nature du feuillet de smectite. Pour cela, on a observé l'évolution du diagramme de diffusion aux petits angles en fonction de la température (entre −15°C et la température ambiante) d'une série de dispersions contenant 20 g d'argile dans 100 g d'eau. La méhode d'interprétation des diagrammes est basée sur la comparaison entre courbes expérimentales et calculées. Les résultats obtenus montrent le rôle, dans l'aptitude au gonflement de la smectite, du cation interlamellaire, de la charge cu feuillet et de sa localisation. Ils montrent également quelles caractéristiques de la structure sont conservées entre la dispersion finale et le solide initial, ce qui permet d'en déduire le mécanisme de dispersion pour chaque smectite.

During weathering of forsterite and tephroite under the humid, tropical conditions of the Ivory Coast, intermediate Mg,Fe3+− or Mn2+-smectites appear prior to widespread development of iron or manganese oxyhydroxides. In forsterite, the smectite varies from an Mg-trioctahedral variety near the centres of altered crystals to an Mg,Fe3+,Al-di/trioctahedral variety near the edges. The Al-content of this latter smectite is supplied by dissolution of adjacent minerals, notably enstatite. An Mn2+-trioctahedral smectite forms in cracks in tephroite crystals.

La phase <2 µm issue de l'évolution géochimique superficielle d'une trachydolérite de Provence s'est révélée être presque exclusivement constituée d'une smectite. Son examen, grâce à plusieurs techniques, et notamment l'identification des produits de recristallisation à haute température, montre qu'il s'agit d'un minéral 2/1, surtout magnésien. L'établissement de sa formule structurale approchée, calculée sur la base de 11 oxygènes, en ferait un minéral intermédiaire entre les smectites diet trioctaédriques, avec une occupation de 2.55 cations en sites octaédriques. Cette smectite de Provence n'est pas une saponite au sens strict, compte-tenu du nombre des cations R3+ = 0.94 en position octaédrique, plus élevé que celui de ces minéraux, tandis que la part des cations R2+ en ces mêmes sites est inférieure au seuil de 85%.

In the past, two factors have impeded the quantitative estimate of Fe-oxides in soils by X-ray diffraction. First, Fe-oxides are still quite often considered X-ray amorphous, although numerous results, e.g. a low ratio of oxalate- to dithionite-soluble Fe, have indicated the opposite. Second, even if crystalline, the cocentration of Fe-oxides in many soils is low, thereby complicating their identification by XRD. Recently, however, more sensitive methods such as Mössbauer spectroscopy and Differential-XRD (Schulze, 1981) have been introduced, which substantially reduce the lower limit of detection. Because these two methods are not generally available and, especially in the case of M&oum;ssbauer spectroscopy, are rather time consuming, ordinary XRD should be adapted for quantitative estimation of Fe-oxides.

Determination can be facilitated by using samples in which the Fe-oxides are concentrated by particle-size separation and a 5 M NaOH boiling treatment (Norrish & Taylor, 1961). The latter treatment is particularly suitable for kaolinitic soils as the Fe-oxides are unaffected―provided certain precautions are taken (Käimpf & Schwertmann, 1982a). This paper gives details of a procedure for the quantitative estimation of goethite (Gt) and hematite (Hm) by XRD.

Amorphous iron oxides in soil are often extracted by an ammonium oxalate solution (Schwertmann, 1964). This treatment may, however, also dissolve crystalline iron oxides and iron silicates (McKeague & Day, 1966; Baril & Bitton, 1969; McKeague et al., 1971; Arshad et al., 1972; Pawluk, 1972; Schwertmann, 1973; Taylor & Schwertmann, 1974; Borggaard, 1976).

It has been shown that EDTA can selectively extract amorphous iron oxides from soils (Borggaard, 1979, 1981) and a synthetic mixture of amorphous iron oxide, goethite, and hematite (Borggaard, 1976). As pointed out previously (Borggaard, 1979), the EDTA method should also be tested on selected minerals to decide if it can serve as a reference method against which other less time-consuming methods may be tested.

Green-blue Fe(II)Fe(III)-and Fe(II)Al(III)-hydroxycarbonates with a pyroaurite structure were prepared by Taylor & McKenzie (1980) and Taylor (1980). They were thought to be related to the unstable mineral phases which occur naturally in the dark green-blue mottles of wet, anaerobic horizons of gleyed soils. These synthetic compounds are unstable to oxidation, suffering structural and colour changes, with the ultimate products depending on the environmental conditions. This instability makes it difficult to identify them and study their characteristics by X-ray diffraction and other methods.

The technique described in this note has been found to stabilize the synthetic green-blue compounds satisfactorily. It involves handling and storage of the compounds in a CO2 atmosphere, such as might occur under natural anaerobic conditions in a soil below the ground-water level. The same principles can be applied to collect field samples and maintain them in a stable state.

The explosive ejection of material from a volcanic vent produces pyroclastics. These are stratigraphically important because of their isochronous nature, lateral extent and potential for absolute age determinations. The pyroclastics also provide information on the nature of the volcanic activity, which is possibly the only record because of non-preservation in other areas. The recognition of pyroclastics is therefore important, but often difficult,because the high-temperature igneous material is susceptible to alteration in the diagenetic environment. In Quaternary sediments the composition of glass shards is an important aspect of tephrochronology (Westgate & Briggs, 1980) but in older sediments glass shards are usually altered to clay minerals. Exceptionally, shards are preserved unaltered, as in the case of early carbonate and silica cementation (Francis et al., 1968; Jeans et al., 1977). According to Ross (1928), features that are diagnostic for the recognition of a volcanic clay (bentonite is the term used by Ross) are, in order of apparent reliability: (i) presence of glass relict structure; (ii) presence of minerals and crystal forms characteristic of volcanic rocks, including biotite, feldspar, pyroxenes and hornblende; (iii) absence of minerals that do not have a volcanic origin, including microcline, garnet, muscovite, kyanite and andalusite; (iv) waxy lustre; (v) reaction to water; (vi) optical properties; (vii) chemical properties.