Measurement of clay particle size invariably presents data in the form of equivalent spherical diameters. For asymmetric particles the equivalent spherical diameter varies with the method of measurement. Based upon an understanding of the theoretical concepts involved, a method has been proposed whereby comparison of data on a given sample from two different techniques can reveal information about the minor dimension of the particle. Theoretical expressions are given for the equivalent spherical diameter of cylindrically symmetric rods and discs from which it is shown that some of the existing measurement methods are more dependent upon size than the degree of non-sphericity whilst for others the reverse is true. It is shown how for rods and discs one can obtain information on both an average axial ratio and the distribution of this parameter for heterogeneous samples. Illustrated data are given for three kaolin samples. Far from showing inconsistency between the variable spherical diameters yielded by different instruments, the data produce compatible size and thickness parameters which match those observed in supplementary, unreported electron microscope experiments. A method of measuring particle major and minor parameter distributions is indicated.

Characterization of platiness of kaolin pigments was derived from the divergence of measurements of their particle size distribution by two different techniques: sedimentation and light scattering. A numerical shape factor, which is related to the ratio of kaolin particle face diameter to its thickness, can be calculated to provide a quantitative measure of such platiness. Two sets of kaolin pigments were prepared from a Middle Georgia kaolin: delaminated and non-delaminated. Shape factors of delaminated samples were higher than those of non-delaminated ones. Maximum platiness was found between equivalent volume diameters of 1·0 and 2·0 μm. Examples are presented where properties of coated paper are correlated with the size and shape of kaolin pigments.

Large quantities of clay minerals (and other micron-sized mineral powders) are used widely in materials science. Mineral fillers are major components, for example, of paints, rubber, plastics and paper and board. While the original object of such incorporation was to reduce costs, performance is now being “engineered” by design or choice of the relevant mineral particles. This paper concentrates on the use of mineral powders in polymer and paper science. In both application areas, the size and shape of the mineral particles can affect mechanical properties such as stiffness and tensile and impact strength. However, other characteristics are also modified. For example, the drainage rate in paper formation and the rheology of a polymer melt, properties which are critically important to the rate of processing of the relevant materials, can be greatly affected. Finally, the size and shape of the mineral particles also affect appearance, i.e. the smoothness, uniformity, optical properties etc. Mechanical and rheological data are presented for mineral-filled polypropylene, as are mechanical and optical data for filled and coated paper.

Modem disc centrifuge technology has extended the range of application of sedimentation particle size analysis to include the submicron region. An overall size range of approximately 10 nm to 100 pm is now accessible. The principles of both the disc centrifuge photosedimentometer, which employs optical detection with full Mie light scattering corrections, and the X-ray disc centrifuge are described. Examples of their application to a variety of samples are given to illustrate the performance characteristics of the instruments including a direct comparison of resolving power with that of the laser diffraction technique.

The use of transmission electron microscopy in association with other methods is described for the characterization of Brazilian industrial clays, especially kaolinitic-halloysitic clays. Examples are presented from: (a) tubular 7 Å-halloysites and the characterization of mixtures with ordered and disordered kaolinites in residual china clays; (b) tubular kaolinitic clay from Piedade, São Paulo; (c) platey 10 Å-halloysite from Poģos de Caldas, Minas Gerais; (d) rolled forms similar to 10 Å-tubular halloysite formed by repeated K Ac intercalation in well ordered kaolinite; (e) use of particle shape and size of kaolinite crystals in the São Simão, São Paulo ball clays as orientation for good sanitaryware ball clays; (f) characterization of gibbsite crystals in high alumina gibbsite/kaolinite clays; (g) antigorite as a clay mineral; (h) electron optical studies of thermal phase transformations involving tubular kaolinite, halloysites, antigorite, chrysotile, talc and pyrophyllite mono crystals.

The effect of gypsum additions on the physical performance of lime-stabilized kaolinite has been determined. Kaolinite containing different amounts of lime (i.e. 6 and 14 wt%) and gypsum (i.e. 2,4,6 and 8 wt%) was compacted into cylinders and moist cured at 30°C and 100% r.h. for periods from 2 days up to 20 weeks. Unconfined compressive strength, expansion during curing and subsequent soaking, and water absorption and swelling pressure were determined. The addition of lime and subsequent moist curing was found to reduce substantially the water absorption, linear expansion and swelling pressure of the kaolinite. Although small amounts of gypsum further reduced these parameters, higher gypsum levels (up to 8 wt%) produced substantial water absorption, extreme expansion and high swelling pressures. This excessive volume instability when in contact with water was found, for a particular lime content, to be very sensitive to both the initial moist curing time and the gypsum content. The results indicate that the overriding expansion mechanism operating is imbibition of water or transfer of water by osmosis. The question of what drives this process is the subject of Part II of this paper.

The results of detailed analyses of the samples discussed in part I are reported. The chemical, morphological and microstructural changes which occurred during moist curing and soaking have been determined using thermal analysis, X-ray powder diffraction analysis, and scanning and transmission electron microscopy combined with EDAX. The analytical results together with the physical observations have shown that the period of volume instability and swelling coincides with the period of gypsum consumption and ettringite formation. However, swelling is not caused by growth of crystalline ettringite but is the result of water absorption. An osmotic mechanism is proposed in which concentration gradients are generated within a surface colloidal layer on the clay particles. Ettringite rods nucleate and grow within this layer and C-A-S-H gel is produced in the areas between the rods. This results in concentration gradients at the clay particle surfaces which provide the driving force for osmosis. The implications of these findings are discussed in relation to lime- stabilization of soils.

Les traitements classiques appliqués pour disperser les argiles et les séparer des carbonates, des phosphates et des sulfates, sont souvent agressifs vis a vis de celles-ci. Une méthode de traitement utilisant les résines échangeuses de cations (REC) a été mise au point. La résine utilisee est l’amberlite IRC-50H. Elle a été éluée ã HCl 1·5 N et utilisée a une température de 60°C. Ce traitement a permis une très bonne dispersion des suspensions de matière d’argile, et l’élimination complete des carbonates, des sulfates et des phosphates. En raison de leur structure silicatée et de leur composition chimique, les argiles sont peu attaquees par les REC, de plus elles sont protegees par les minéraux susceptibles d’être dissous par les REC (carbonates, phosphates et sulfates).

Regression analysis of high-precision structural and chemical data on trioctahedral and dioctahedral micas yielded interrelationships between unit-cell parameters, chemical composition and structural details. Regression equations relating b and csinβ parameters of micas to composition were used for estimating composition from cell data in order to analyse P-T conditions of rock formation. Algorithms for computing atomic coordinates for 2M1 37' and 1M dioctahedral micas having either centrosymmetric or non-centrosymmetric layers and 1M trioctahedral micas are presented. Deviations of computed atomic coordinates from experimental values are, on average, 0·002 Å for octahedral cations and 0·005-0·010 Å for other atoms. Discrepancies between calculated and experimental individual interatomic distances seldom exceed 0·01 Å. Computed atomic coordinates were used to calculate X-ray diffraction patterns for glauconite and illite. Results indicate a close fit between the calculated and experimental patterns. The local structure around an octahedral cation of interest can be determined.

In Upper Jurassic sandstones of the Magnus Sandstone Member from the Magnus Oilfield in the North Sea, diagenetic kaolinite morphology and isotopic composition vary away from the Late Cimmerian unconformity. Near the unconformity, coarse-grained (15-30 μm) vermiform kaolinite morphology is most common, whereas downdip, 3 km away, fine-grained (∼10 μm) blocky morphology is prevalent. Kaolinite abundances increase downdip, away from the unconformity, and kaolinite near the unconformity has low δ18O (12·5-14·9%o smow) compared to that downdip (15·9−17·5%o). This reflects replacement of marine depositional pore-waters by meteoric water near the erosion surface. However, isotopic temperature estimates suggest that the majority of kaolinite formed at elevated burial temperatures of ~80°C, and not during subaerial exposure of the sandstone. The δD of kaolinite close to the unconformity is also lower than that downdip. Kaolinite morphology and isotopic composition record meteoric water ingress during Late Cimmerian subaerial erosion and retention of meteoric-derived water in the crest of the Magnus structure during burial diagenesis. Kaolinite formation during subaerial exposure is not of significance to the sandstone reservoir quality.

Glauconite and Fe-smectite, which can be distinguished by their peculiar morphology and stacking sequences, coexist in the Galapagos Spreading Centre hydrothermal mounds. Analytical electron microscopy (AEM) data suggest that Fe is entirely in octahedral sites in Fe-smectite whereas glauconite is K-rich with Fe in tetrahedral and octahedral sites. However, the Mossbauer spectra, recorded at various temperatures for samples containing both smectite and glauconite, were satisfactorily analysed with three overlapping doublets corresponding to Fe in octahedral sites. The contradictory results obtained with the two methods are explained by the presence of small particles of iron oxide intimately associated with glauconite. These particles were detected in Mossbauer spectra obtained at 77 K and 4·2 K and were observed by transmission electron microscopy. Iron oxide is a secondary phase formed by alteration of smectite. These data are in good agreement with the hypothesis that the smectite-glauconite reaction, which occurs at 30 m and low temperature in the Galapagos hydrothermal mounds, is a dissolution-precipitation process, dissolution of Fe-rich smectite being followed by precipitation of glauconite and iron oxides.