A quantitative method for determination of montmorillonite in the soil clay fraction, using X-ray spectrometry, is proposed. The method is based on the fact that polyvinylpyrrolidone (PVP) is adsorbed on the interlayer surfaces of montmorillonite, giving a first order c-axis spacing of 26 Å, while it is not adsorbed on other swelling clays. The experimental conditions to obtain a maximum height of the X-ray diffraction peak, and the effect of the mass adsorption coefficient of vermiculite on the intensity of montmorillonite, were investigated. Soil montmorillonite was determined by the method of known additions, measuring the intensity of the X-ray diffraction peak before and after the addition of small and known amounts of Wyoming montmorillonite.

The present paper describes a new mineral species, namely a regularly interstratified chlorite —trioctahedral smectite bearing as much as 24% NiO. The high Ni content proves it to be nickel mineral.

On the diffractogram of the raw sample, an integral series of reflections with l.d(001) = 30·1 Å was obtained. To study the nature of the component layers, X-ray examinations of glycerol saturated samples and also dehydrated by heating were accomplished. Thermal and chemical analyses were performed in the usual way.

The crystallochemical formula can be presented as follows: saponite layer—(Mg,Ni)3·00 (Si3·75Al0·25) O10(OH)2, charge −0·25; Ca0·06 (Mg,Ni)0·06 K0·01, 4·07 H2O, charge +0·25; chlorite layer—(Mg, Ni)2·02(Al,Fe*)0·65(Si3·76Al0·24) O10(OH)2, charge −0·25; (Mg,Ni)2·75 (Al,Fe3+)0.25 (OH)6, charge +0.25.

The full mineral and chemical characteristics lead to precise conclusions concerning the composition and structure not only of the nonexpanding chlorite layers, but especially of the expanding layers. The latter show the chemical composition of saponite but the interlayer material is composed partly of exchange cations and molecular water and partly of “brucite-like pillows”.

A 1–0·2 μm fraction from a soil in the Dominican Republic was studied by X-ray diffraction combined with solvation, cation saturation, and heat treatments. I.R., thermal (DTA, TGA) and chemical analyses were also made. This soil is saline and alkaline and its mineral composition is greatly influenced by the lacustrine parent material and poor drainage.

In addition to swelling chlorite, illite, kaolinite, carbonates and quartz are present in the 1–0·2 μm fraction. The swelling chlorite expanded to over 18 Å when Mg saturated and solvated with glycerol or water. Lower spacings with other cations and ethylene glycol were observed. 1 N HCl treatment partially removed the interlayer hydroxides in the chlorite and 6 N HCl destroyed the mineral. The mineral gave a reflection close to 14 Å up through 600°C but collapsed at higher temperatures to 10·2 Å.

The electron spin resonance of some structural Fe3+ for montmorillonites having low Fe3+ content, is perturbed by electrostatic interaction between exchange cations and structural charge sites. The position of charge centers of organic and inorganic cations in the interlayer can thus be determined at various levels of solvation. Dielectric media between the silicate layers lower the electrostatic attraction between the silicate and the exchange cations. The silicate charge appears to be partially delocalized on structural oxygen atoms as shown by electron spin resonance and i.r. spectroscopy. There is also evidence that divalent exchange cations on dehydrated montmorillonites cause hydrolysis of water; the protons so produced migrate to structural charge sites.

Halloysite (metahalloysite) of various particle sizes has been altered with oxalic and EDTA acids, at room temperature and during different periods of time (5–90 days). The oxalic acid attack at first achieved only a recrystallization of halloysite. The recrystallization is much more significant the smaller the size of the treated halloysite particles. Later the material is destroyed. The EDTA treatment also has provoked during the first days a recrystallization of the halloysitic material which is destroyed again after about 20–25 days. Later kaolinite is formed. The kinetic curve of kaolinite formation is symmetrical with respect to that corresponding to the diminution of amorphous material in the sample. The influence of the halloysite particle size and the complexing effect of the acids in relation to the resulting products are discussed.

An attempt has been made to synthesize nitrogenous clay minerals hydrothermally from silica-alumina gels in the presence of amino acids, namely glycine and lysine. The products have been characterized by X-ray powder diffraction, by analyses for C and N contents, and by their infrared spectra.

Amino acid-montmorillonites have been prepared under hydrothermal conditions of 200–250°C and 1000 atm. Above 250°C the amino acids were degraded to ammonium ions, and ammonium-micas were obtained. Syntheses without the addition of amino acids to gels yielded kaolinite.

The role of organic compounds in the formation of clay minerals seems to be of considerable geochemical significance.

Three sepiolite clays studied showed evidence for the presence of structural hydroxyl groups in three to five different environments depending on the composition of the clay. A 3720 cm−1 i.r. frequency is shown to be characteristic of SiOH at crystal edges which are very abundant in sepiolites. This band has not been seen by most workers because the Nujol, fluorolube or KBr used in sample preparation perturb it sufficiently to obscure it under other OH stretching bands. The 3680 cm−1 band is confirmed as being from the (Mg)3OH and evidence of a very small band near 3640 cm−1 is suggested to arise from limited trioctahedral substitution. The very crystalline Ampandrandava sepiolite shows only the above three bands. The intermediately crystalline Vallecas shows a 3620 cm−1 band in addition which is characteristic of dioctahedral systems and is due to either some vacancy sites or to the presence of attapulgite. This dioctahedral band is greater in the less crystalline Salinelles sepiolite; in addition, it has a smaller 3585 cm−1 band. Mg-Al-vacancy and Mg-Fe‴-vacancy are suggested as the source of the 3620 cm−1 and 3585 cm−1 bands.

The layer structure of kaolinite from Twiggs, Georgia and fire-clay type kaolinite (Frantex B, from France), particle size separates 2–0·2 μm was studied by high resolution electron microscopy after embedment in Spurr low-viscosity Epoxy media and thin sectioning normal to the (001) planes by an ultramicrotome. Images of the (001) planes (viewed edge-on) of both kaolinites were spaced at 7 Å and generally aligned in parallel, with occasional bending into more widely spaced images of about 10 Å interval. Some of the 10 Å images converged to 7 Å at one or both ends, forming ellipse-shaped islands 80 to 130 Å thick and 300 to 500 Å long. The island areas and interleaved 10 Å layers between 7 Å layers may represent a residue of incomplete weathering of mica to kaolinite.

The proportions of micaccous occlusions were too small and the layer sequences too irregular to be detected by X-ray diffraction. The lateral continuity of the layers through the 7-10-7 Å sequence in a kaolinite particle would partially interrupt or prevent expansion in dimethyl sulfoxide (DMSO) and other kaolinite intercalating media. Discrete mica particles were also observed with parallel images at 10 Å, as impurities in both kaolinites. The small K content of the chemical analyses of the kaolinite samples is accounted for as interlayer K, not only in discrete mica particles but also in the micaceous occlusions.

Since 1960 asbestos production of the United States has more than tripled, a phenomenon due in large part to the development of the Coalinga asbestos deposit in western California. Although most asbestos ores contain 5–10 per cent chrysotile in the form of cross- or slip-fiber veins within massive serpentinite bodies, no such veins are to be found in the Coalinga deposit despite the fact that it contains more than 50 per cent recoverable chrysotile. The Coalinga ore consists of soft, powdery, pellet-like agglomerates of finely matted chrysotile surrounding blocks and fragments of serpentinite rock. The highly sheared and pulverized nature of the ore favors its exploitation by simple, open-pit mining, and high quality products can be prepared by either wet or dry milling processes.

Four types of serpentine material are distinguishable: (1) hard, dense blocks of serpentinite rock, ranging from fractions of an inch to several tens of feet in diameter; (2) tough, leathery sheets, resembling mountain leather, up to several square feet in size; (3) brittle blades and plates of green serpentine, a few square inches in size; and (4) friable agglomerates of soft, powdery chrysotile containing appreciable amounts of the other three. Chrysotile is the principal component of all the above materials, with the exception of the serpentinite rock which consists mainly of lizardite and/or antigorite, with small amounts of brucite, magnetite, and very short fiber chrysotile. Although chrysotile fibers up to several microns in length are present in the leathery sheets, most Coalinga chrysotile is much shorter and arranged in a swirling mesh or disoriented, tangled fibers, much like cellulose fibers in paper. Fragments of serpentinite gangue are scattered throughout the ore and contain most of the lizardite, antigorite, and brucite. Chemical, electron probe, and X-ray analyses confirm the iron-rich nature of the brucite, a critical factor in the susceptibility of this phase to oxidation in the surface weathering zone. Here brucite either dissolves, leaving behind a residue of brown, amorphous iron oxides, or transforms in situ to pyroaurite or coalingite. Dissolved magnesium precipitates as hydromagnesite immediately above the water table throughout the deposit.

The abnormally high chrysotile content of this deposit is probably a result of the intensive shearing that it underwent during or after emplacement. If the friable, chrysotile-rich ore was produced during this pulverization episode, (1) lizardite and/or antigorite in the serpentinite must have been transformed into chrysotile and (2) brucite must have been removed. It is likely that early-formed lizardite/antigorite dissolved in the ground waters which pervaded the highly sheared body and that chrysotile later precipitated from these waters, coating all available surfaces.

Possible assignments are suggested for some of the absorption bands in the 1150–400 cm−1 region of the i.r. spectra of serpentines. Polarized light was used to identify the out-of-plane vibrations in antigorites and platy lizardites and the vibrations parallel to the fibre axis in chrysotiles and fibrous lizardites. An attempt is made to correlate some known structural characteristics and the chemical composition of the serpentines with some features of the i.r. spectra.

The Numedal River basin (6000 km2) in central and east Norway contains 3 × 109 m3 of clayey material, corresponding to a clay loam sediment, which contains 2 million tons of absorbed rare earth elements.

The clay mineralogy varies systematically from the till clays to a marine facies. It is concluded that the phyllosilicates of the clay fraction and tills originated from phyllosilicate minerals of the crystalline bedrock through a degradation partly due to preQuaternary weathering which dissolved a great part of the rock-forming minerals.