Fitted Mössbauer spectra are presented for a set of anthophyllites and gedrites. Despite their complexity it is possible to obtain fits for gedrite spectra and the Mössbauer parameters are consistent with results for anthophyllites from this and previous studies. At least three doublets are required to fit the Fe2+ absorption in gedrites; there is no single model at present to explain the behaviour of the spectra. Fe3+ absorption is also resolved.

Mineral and fluid inclusions were studied in seven gem corundums from gravels of three areas in Sri Lanka. All fluid inclusions are pure CO2. Microthermometry results on primary fluid inclusions suggest formation of corundum under granulite facies metamorphism (>630°C, 5.5 kbar). Secondary fluid inclusions indicate different retrograde events of post-metamorphic cooling and uplift for different source areas.

Accessory minerals are often difficult to investigate with light optics as the mineral grains tend to be small and the refractive indices high. Textural features due to variations in composition are well displayed in such minerals by backscattered electron imagery under circumstances designed to select only the composition contribution to electron backscattering and displayed as atomic number (Z)-contrast imagery (ZCI). It is shown by this technique that compositional zonation patterns are very common and sector zoning in titanite is described for the first time. The compositional basis for zonation of titanites in this study is shown to be controlled by coupled substitutions involving the REE. The technique is particularly good at revealing rounded cores to zircon grains which are normally taken to be refractory grains from the magma source region, and ZCI studies may improve targeting of grains for U-Pb geochronological investigations. Several examples are presented of applications of the technique to accessory minerals encountered in polished thin sections of granitoids in the Caledonian of Scotland. The consequences of ZCI studies for trace element modelling of REE in granitoid petrogenesis are discussed.

Holtite, (Si2.25Sb0.75)B[Al6(Al0.43Ta0.27□0.30)O15(O,OH)2.25], is orthorhombic a = 4.6914(5), b = 11.896(2), c = 20.383(4)Å, space group Pnma. Full-matrix least-squares refinement yielded a final R = 0.030, for 1664 reflections with I ⩾ 3σ(I). Its crystal structure is closely related to that of dumortierite, but with the difference that extensive substitution of Si by Sb occurs in holtite. SbO3 triangular pyramids replace the SiO4 tetrahedra arranged around the inside edge of the hexagonally shaped tunnels which are the feature of the dumortierite and holtite structures. Associated with these replacements is the replacement of Al by Ta in the octahedral site centred in these tunnels, and the development of vacancies in this metal site and its attached oxygens.

This second recorded occurrence of yimengite, K(Cr, Ti, Fe, Mg, Al)12O19, is in a Precambrian kimberlitic sill in the Guaniamo District of Bolivar Province, Venezuela. The paragenesis is similar to that of the type area in Shandong Province, China, where the mineral is in kimberlite dykes. At both localities the yimengite is a K, Ti-bearing metasomatic product of chromium-rich spinel. In the Venezuela rocks the spinels are of the type occurring both as diamond inclusions and as a component of diamond-related Cr-rich garnet harzburgite mantle xenoliths. Yimengite contains significant amounts of barium (up to 3.4wt.% BaO) and is thus transitional to the recently described mineral hawthorneite, Ba(Cr, Ti, Fe, Mg)12O19. Both members are part of a suite of titanate minerals found in kimberlites and their inclusions which has been described by Haggerty and coworkers; they formed as a result of mantle metasomatism generated by K- and Ba-rich fluids. In Venezuela, metasomatism of this type would appear to be deeper than that usually recorded, namely in the basal lithosphere. The metasomatizing fluids are derived from the underlying, more oxygenated asthenosphere. The host kimberlitic rocks are not significantly enriched in K and Ba, but these elements are concentrated in later micaceous dykes which are conjectured to have been generated within similar metasomatized mantle.

Quartz-gahnite-sillimanite asssemblages are described from a supracrustal enclave at Kraaifontein, 45 km south-west of Springbok in the Namaqualand Metamorphic Complex, South Africa. The assemblage formed by prograde reaction in the granulite facies zone during the 1100 Ma Namaqua event, possibly as the result of desulphidation of sphalerite. Subsequent lower-amphibolite-facies retrogression occurred in close proximity to shear zones during an early Pan-African metamorphic event at 700 Ma. Zincian staurolite formed as overgrowths on gahnite in a hydration reaction involving the consumption of gahnite, quartz, and sillimanite. Compositional zoning to more zinc-rich rims in gahnite at Kraaifontein is unrelated to the retrograde reaction, but is interpreted as a result of changing conditions during the prograde Namaqua event.

Mössbauer spectroscopy has been used to identify the iron-containing products that are formed during the thermal decomposition of ankerite in a CO2 atmosphere. The decomposition takes place in three stages and evidence is produced to show that the first stage involves decomposition of ankerite to yield a periclase-wustite solid solution, (Mg,Fe)O, along with calcite and CO2, the periclase-wustite then reacting with CO2 to produce magnesioferrite (MgFe2O4) and CO. In the second stage the magnesioferrite and calcite react to produce periclase and dicalcium ferrite. The third stage does not involve reaction of Fe-containing phases and corresponds to the decomposition of calcite to CaO.

EXAFS and Mössbauer data on synthetic silver-rich tetrahedrite, (Cu, Ag)10+xFe2−xSb4S13, reveal the presence of Fe2+ and Fe3+ the former occupying trigonal planar sites and the latter tetrahedral sites. There is also a clear relationship between increased silver substitution and an increase in Fe2+. The amount of Fe3+ incorporated in the synthetic tetrahedrites is proportional to the excess of Cu+ (Cu + Ag > 10 atoms) in the mineral, thus maintaining a charge balance. The iron in the natural tetrahedrites and the tennantite examined is mainly tetrahedrally co-ordinated Fe2+.

Saddle dolomite is a common product of late-stage diagenesis and hydrothermal activity. It has been suggested that during growth Ca enrichment occurs towards crystal edges leading to a lattice expansion relative to face centres. However, backscatter scanning electron microscopy of eight samples has revealed that, instead of edge associated Ca enrichment, saddle dolomites have a series of edge associated Mg enriched wedges, between 5 and 20 µm thick and 300 µm long. Wedge geometry implies development of extra lattice layers at edges relative to face centres. It is suggested that the wedges develop during rapid, transport-controlled, crystal growth. The wedges possibly reflect a switching from continuous growth across the face to edge-nucleated growth as the boundary layer solution becomes progressively depleted. Continuous growth might be reinstigated through convective turnover of the boundary layer presenting fresh solution to the growing crystal.

Titanian aegirine in a pegmatoid differentiate from leucitite sensu stricto (i.e. without modal plagioclase) was found to contain significant K (up to 0.07K atoms per formula unit; 0.11 wt.% K2O) by electron probe microanalysis. A transmission electron microscope study showed that this pyroxene contained a lamellar amorphous phase and other more irregular, amorphous domains where K and Al are concentrated. The microstructures suggest that the aegirine-amorphous phase system did not achieve textural equilibrium. Also, the chemistry of this phase is variable, particularly in Ca and Mg, suggesting lack of chemical equilibrium within the liquid from which the phase derived. The average composition of the latter approaches that of the coexisting K-richterite and is interpreted as trapped residual liquid, i.e. glass, from pyroxene crystallization which failed to develop a crystalline amphibole. In view of the extensive stability of richterite coexisting with pyroxene to high pressure, the reported occurrence of ‘K-bearing pyroxene’ may not be considered as a homogeneous K-bearing phase and a predictable potassium carrier in the petrogenesis of K-rich rocks like leucitites and lamproites.

Nodules of manganoan fayalite occur in schlieren pegmatities in the vicinity of Strzegom, Lower Silesia. The fayalite, Na0.02(Fe1.812+Mn0.16Mg 0.03)Si0.99O4, is unzoned and non pleochroic. 2Va = 42° a 4.826(3), b 10.500(2), c 6.102(2) A, d130obs. = 2.83 Å, d130calc. = 2.833 Å, D = 4.35 g cm-3, Dcalc. = 4.353 g cm-3. The role of Na+ ions in the fayalite chemistry is discussed. The fayalite underwent multi-stage hydrothermal alteration beginning at the highest temperature (440°C) of homogenization of gaseous-fluid inclusions in quartz adjacent to the fayalite grains. Increase in fO2 and then in PH2O resulted in the formation of magnetite-quartz and Mn-grunerite-magnetite-quartz aggregates within the fayalite grains. The fayalite is mantled by a Mn-greenalite-magnetite rim, Mn-grunerite-magnetite-Mn-minnesotaite zone in a stilpnomelane or greenalite-rich groundmass. The minnesotaite is believed to have formed at the expense of grunerite. Stilpnomelane, the most abundant silicate phase in the rim, is the product of biotite and presumably greenalite alteration at the second stage of increasing Na activity (the crystallization of cleavelandite) in the pegmatites. The fayalite is also heavily altered to iddingsite—a composite mixture of amorphous FeOOH and silica. The iron-hydroxide recrystallized partially to poorly-crystalline goethite.

Cathodoluminescence emission spectra and luminescence excitation spectra of Mn2+ in calcites, dolomites, magnesites, a manganocalcite and a rhodochrosite have been measured at both room temperature and 77 K. Ligand-field parameters have been calculated from the excitation spectra which reflect the size of the metal cation site in which the Mn2+ ion resides. The technique of luminescence excitation spectra has enabled the absorption profile of Mn2+ in Mg and Ca sites in dolomite to be separately determined. The variation of the distribution of Mn2+ between Mg and Ca sites in dolomites is demonstrated and discussed in terms of a simple model. It is concluded that the distribution of Mn2+ in dolomites may well provide information about its conditions of formation and/or subsequent alteration.

Anisotropic opaque minerals viewed in reflected light microscopy show two sets of colours: the colours seen in plane polarized light which change as the section is rotated on the microscope stage, and the colours seen between crossed polars which change as the analyser is uncrossed. These latter colours are known variously as polarization colours or anisotropic rotation tints, but are here referred to as anisotropy colours. They are commonly a diagnostic aid to correct mineral identification. All these colours occur as a consequence of the dispersion of the relative permittivity (dielectric) tensor—the variation in the values of the tensor with wavelength of incident light and in low symmetry crystals, the variation in the directions of the principal axes of the tensor with wavelength.

In this paper, it is shown that the colour seen in plane polarized light and the anisotropy colours can be predicted for any orientation of section, at any stage angle, and for any degree of uncrossing of the analyser by calculations based on the dielectric tensor values, and these predicted colours compare favourably with the observed values. Three minerals are studied in this paper as examples: stannite, covelline, and bournonite.

Strictly reproducible syntheses of the trimorphs of composition Cu2Cl(OH)3, atacamite, paratacamite, and botallackite, have been developed. In syntheses involving direct precipitation, or reaction of aqueous solutions with solid phases, reliable results are obtained only if the temperature and time of reaction are carefully controlled. Botallackite, the rarest of the naturally occurring trimorphs, is a key intermediate and crystallizes first under most conditions; subsequent recrystallization of this phase to atacamite or paratacamite, or of the latter from the former, depends upon the precise nature of the reaction medium. The crystallization sequence indicates that paratacamite, as has long been suspected, is the thermodynamically stable phase at ambient temperatures. Spertiniite, Cu(OH)2, can be reproducibly synthesized via one route in the non-commutative titration of aqueous copper chloride with aqueous sodium hydroxide solutions.

Vochtenite, a new mineral from the Basset Mine, southeast of Camborne in Cornwall, England, is a ferrous-ferric magnesium-bearing hydroxy uranyl phosphate mineral. It is monoclinic with a = 12.606, b = 19.990, c = 9.990 Å, β = 102.31° Z = 3; the ideal formula is:

The strongest lines in the X-ray powder diffraction pattern are: 9.998(100)(020), 4.999(30)(040), 4.892(45)(002), 3.475(70)(311), 3.333(50)(060), 3.087(40)(232), and . Vochtenite is brown in colour with a bronzy lustre and is non-fluorescent. Mohs hardness is 2.5 and the density (calc.) = 3.663 g/cm3. There is a prominent (010) cleavage. Vochtenite is optical biaxial negative, 2V (calc.) = 89(3)° its dispersion is indiscernible. Refractive indices are α = 1.575(2), β = 1.589(2), γ = 1.603(2), and the pleochroism is very weak. Orientation X(α)∥b is perpendicular to (010) and Z(γ)∧c is small. The mineral occurs as subparallel (0.5–1.0 mm) crystal aggregates with a pseudo-quadratic outline. The mineral is named vochtenite after Prof. Dr. Ing. R. F. C. Vochten of the State University of Antwerpen, Belgium.

Vaughanite, idealized formula T1HgSb4S7, is a very rare primary constituent of the Golden Giant orebody of the Hemlo gold deposit, Hemlo, Ontario, Canada. It was found in two polished sections from one drill core; as a 450 by 300 µm aggregate associated with pääkkönenite, stibnite, realgar, and native arsenic; and as a 40 µm anhedral grain associated with stibarsen and chalcostibite. Vaughanite is opaque with a metallic lustre and a black streak. No cleavage was observed but parting, produced by indentation, was detected as a series of weak parallel traces. It is brittle, with an even, occasionally arcuate, fracture. VHN25 is 100–115, mean 104. Mohs hardness (calc.) = 3−3½. In refected plane-polarized light in air the bireflectance is weak to moderate; the pleochroism is also weak, from a somewhat greenish grey to slightly darker bluish grey. Anisotropism is moderate to strong, with rotation tints in shades of green, yellow, purplish brown to brown. Reflectance spectra and colour values are tabulated. The colour in air is light grey. Internal reflections are rare but are arterial-blood-red on indentation fractures. X-ray studies have shown that vaughanite is triclinic with refined unit-cell parameters a 9.012 (3), b 13.223 (3), c 5.906 (2) Å, α 93.27 (3)°, β 95.05 (4)°, γ 109.16 (3)°, V 659.46 (80) Å3, a:b:c = 0.6815 : 1 : 0.4466 and Z = 2. The space group choices are P1 (1) or (2), diffraction aspect P*. The five strongest lines in the X-ray powder pattern [d in Å (l) (hkl)] are: 4.343 (30) (), 4.204 (100) (), 3.313 (60) (130), 2.749 (40) (, 131) and 2.315 (30) (, 122). The average of five electron microprobe analyses gave T1 18.3 (2), Hg 17.5 (2), Sb 43.4 (3), As 1.1 (1), S 20.5 (5), total 100.8 wt. %, corresponding, on the basis of total atoms = 13, to T10.98Hg0.95(Sb3.90As0.17)Σ4.07S7.00. The calculated density is 5.56 g/cm3 for the empirical formula and 5.62 g/cm3 for the simplified formula. The mineral is named for Professor David J. Vaughan.

Synthetic pentlandite surfaces were subjected to oxidation by a range of inorganic oxidants, and the resultant alteration of the surface studied by a range of surface-sensitive spectroscopic techniques. The oxidants used were air during heating to relatively low temperatures (150°C), steam, ammonium hydroxide, hydrogen peroxide, and sulphuric acid. Electrochemical oxidation was also undertaken. X-ray photoelectron spectroscopy (XPS), Auger electron spectroscopy (AES), conversion electron Mössbauer spectroscopy (CEMS), and spectral reflectance measurements were used to characterize the surface compositions. New data for the binding energies of core electrons in pentlandite and violarite, based on the fitted XPS spectra, are proposed. For pentlandite and violarite respectively, values of 707.3 eV and 708.4 eV for the Fe 2p3/2, 853.0 eV and 853.2 eV for the Ni 2p3/2, and 161.2 eV for the S 2p in both sulphides, were obtained. After oxidation the pentlandite surfaces indicated nickel enrichment in the subsurface, with the formation of violarite. The immediate oxidized surface, of approximately 10Å thickness, indicated a range of iron oxides and hydroxides (Fe3O4, Fe2O3 and FeOOH, with possible Fe1−xO and Fe(OH)3), nickel oxide (NiO), and iron sulphates (FeSO4, Fe2(SO4)3). The proportions of the phases present in the surface layer are inferred to be a consequence of both the strength of the oxidant employed, and the thermodynamic stability of the phases, as can be illustrated using partial pressure and Eh/pH diagrams. A sequence of oxidation is proposed, accounting for the sub-surface enrichment in violarite, and the development of the oxidized surface, which is inferred to have a major affect on the rates of oxidation.

Gypsum crystals were grown at 25, 35, and 45 °C from solutions containing different ionic impurities (Mg2+, Na+, Cd2+). Curved gypsum crystals formed from the solutions enriched in magnesium or cadmium, whereas, in the presence of sodium, gypsum always grew undeformed. The mechanism of the curvature is described and an interpretation based on crystallographic considerations is given. Curvature is the result of impurity incorporation followed by crack formation and mechanical twinning which releases the internal stresses.

The nomenclature of CaZrTi2O7 minerals has become very confused, such that zirconolite, zirkelite and polymignite each have acquired multiple meanings and represent five different crystal structures. To resolve these inconsistencies, the IMA approved resolutions as follows. Zirconolite is the non- crystalline (metamict) mineral or mineral with undetermined polytypoid of CaZrTi2O7. Zirconolite-3O is the three-layered orthorhombic polytypoid of CaZrTi2O7. Zirconolite-3T is the three-layered trigonal polytypoid of CaZrTi2O7. Zirconolite-2M is the two-layered monoclinic polytypoid of CaZrTi2O7. Polymignite (metamict) is discarded as equivalent to zirconolite. Zirkelite is the cubic mineral with formula (Ti,Ca,Zr)O2−x.

Quantitative measurement of relative flexibility have been made on amphibole fibres based on calculation of bending strain of maximally bent fibre segments. Enhanced flexibility was found to be an inverse function of fibre diameter. Asbestos is therefore a morphological entity. These conclusions are supported by consistent observations of fibre diameter/flexibility relationships in amphiboles, serpentine, and rutile. Flexibility may arise from growth of thin crystals (primary flexibility), or from crystal diameter reduction (secondary flexibility). Mechanisms for secondary flexibility in amphiboles include splitting and solution along cleavage planes. Gross morphological characteristics are a poor indicator of microscopic habit, since coarsely fibrous minerals such as picrolite antigorite may not be fibrous after particle width reduction, and secondary asbestiform fibres are often derived from minerals with a non-fibrous morphology on gross examination.