We have developed a system using ‘forescatter detectors’ for backscattered imaging of specimen surfaces inclined at 50–80° to the incident beam (inclined-scanning) in the SEM. These detectors comprise semiconductor chips placed below the tilted specimen. Forescatter detectors provide an orientation contrast (OC) image to complement quantitative crystallographic data from electron backscatter patterns (EBSP). Specimens were imaged using two detector geometries and these images were compared to those collected with the specimen surface normal to the incident beam (normal-scanning) using conventional backscattered electron detector geometries and also to an automated technique, orientation imaging microscopy (OIM). When normal-scanning, the component of the BSE signal relating to the mean atomic number (z) of the material is an order of magnitude greater than any OC component, making OC imaging in polyphase specimens almost impossible. Images formed in inclined-scanning, using forescatter detectors, have OC and z-contrast signals of similar magnitude, allowing OC imaging in polyphase specimens.

OC imaging is purely qualitative, and by repeatedly imaging the same area using different specimen-beam geometries, we found that a single image picks out less than 60% of the total microstructural information and as many as 6 combined images are required to give the full data set. The OIM technique is limited by the EBSP resolution (1–2°) and subsequently misses a lot of microstructural information. The use of forescatter detectors is the most practical means of imaging OC in tilted specimens, but it is also a powerful tool in its own right for imaging microstructures in polyphase specimens, an essential asset for geological work.

Benleonardite, ideally Ag8(Sb,As)Te253, occurs in ore specimens from the Mayflower and Gies epithermal gold-silver telluride deposits in Montana commonly spatially associated with hessite and tetrahedrite. In these deposits, it is Cu-bearing (up to 2.7 wt.%) and exhibits a slight deficiency in Ag+Cu coupled with a slight excess in S. A cervelleite-like mineral coexists with benleonardite at Mayflower and is unusual in composition in that it is Se-bearing suggesting the possibility of solid solution with aguilarite (Ag4SeS).

The petrology of a massive olivine-sulphide interplanetary dust particle shows melting of Fe,Ni-sulphide plus complete loss of sulphur and subsequent quenching to a mixture of iron-oxides and Fe,Ni-metal. Oxidation of the fayalite component in olivine produced maghemite discs and cellular intergrowths with olivine and rare andradite-rich garnet. Cellular reactions require no long-range solid-state diffusion and are kinetically favourable during pyrometamorphic oxidation. Local melting of the cellular intergrowths resulted in three dimensional symplectic textures. Dynamic pyrometamorphism of this asteroidal particle occurred at ∼1100°C during atmospheric entry flash (5–15 s) heating.

The advantages of X-ray absorption spectroscopy have been utilized to assess the Cu and Zn ordering in aurichalcite, (Cu5−xZnx)(OH)6(CO3)2. We have examined one hydrozincite sample and three aurichalcite samples in which the Cu:Zn ratios are in the range 1:3 to 2:3. Copper 2p XAS confirms that there is no monovalent copper in aurichalcite and that in each sample the copper might be distributed across more than one metal site. EXAFS, at the Cu and Zn K-edges, shows that the copper atoms preferentially enter the Jahn-Teller elongated, octahedral (M2) and trigonal bipyramidal (M4) sites, with the zinc atoms entering the more regular octahedral (M1) and tetrahedral (M3) site. Substantial solid solution towards the zinc rich region is facilitated by the substitution of copper by zinc on the M2 and M4 sites. This information, not easily obtained by X-ray diffraction, substantially enhances the understanding of the structure of aurichalcite.

Frankamenite, K3Na3Ca5[Si12O30]F3(OH)1H2O, from the Yakutian charoitic rocks, has a triclinic unit cell with the dimensions: a = 10.094(3), b = 12.691(3), c = 7.240(1) Å, α = 90.00(2)°, β = 111.02(2)°, γ = 110.20(2)°, sp.gr. = P1, Z = 1. Its crystal structure has been refined to Raniso= 0.059 (Rw = 0.060) using the intensities of 2563 reflections.

The bases of the structure are zig-zag walls of Ca, Na octahedra joined by infinite octagonal cross-sectioned tubes of SiO4 of the composition (Si12O30). Unlike canasite from the Khibini Mountains, the triclinic cell of frankamenite contains only one silicate tube. The atomic coordinates, interatomic distances and angles are topologically similar to those of canasite. Major differences are observed in the distribution of octahedral cations, which reflect the different anion compositions. Frankamenite exhibits six mixed Ca-Na positions, whereas canasite has only one such position. The H2O molecule is located in the centre of the silicate tube between K+ cations.

Pyroxene and mica found in plutonic rocks of the Little Murun ultrapotassic pluton exhibit trends of compositional evolution that permit evaluation of the differentiation sequence of the complex. Pyroxene evolves from diopside in kalsilite and phlogopite pyroxenites through aegirine-diopside in shonkinite to aegirine in late stage charoitite and evolved hypabyssal rocks. The compositional trend is unusual in that the hedenbergite content of the pyroxenes never exceeds 15 mol.% and is thus unlike pyroxene compositional trends found in sodic alkaline complexes. Mica is Al- and Ti-poor and ranges in composition from Fe-rich phlogopite through biotite towards tetraferriannite. Compositional trends of mica found in ‘lamproite-like’ hypabyssal rocks are identical to those observed in the micaceous plutonic rocks; hence the former are considered to be representatives of the lamprophyric facies of the magmas which formed the plutonic series.

Sericitization in three separate pulses of the Rosses Granite Ring Complex, Co. Donegal, Ireland, has been investigated texturally and chemically using electron microscopy, electron microprobe and fluid inclusion thermometry. The sericitization, which is restricted to the cores of plagioclase, is associated with pores which are abundant in the cores, but absent in the margins. Alkali feldspar, although porous, is unaltered. Associated with the sericitization is alteration of the adjacent primary plagioclase within the cores of grains to a more sodic composition.

It is postulated that the sericitization resulted from the action of externally derived secondary hydrothermal fluids, which gained access to the pores in the plagioclase via now sealed microfractures, formed either by contraction during cooling of the Rosses Complex, or more likely by hydraulic fracturing by the fluids themselves. Limited fluid/rock ratios restricted the degree of sericitization within the host plagioclase, whilst an absence of alteration in alkali feldspar may have been due to the inaccessibility of pores in the alkali feldspar to the hydrothermal fluids at the time of alteration. Fluid inclusion data suggest that the fluids were of low salinity, and that the sericitization took place at an early stage in the cooling history of the Rosses Complex at temperatures between 400 and 600°C. It is further contended that greisenization in the Rosses Complex predated the sericitization and that the greisenization may have been due solely to volatile-rich late-stage magmatic fluids.

Golden iridescent, <1–100 mm crystals of alternating lamellae of anthophyllite and gedrite constitute the bulk of orthoamphibolite pods within quartz-cordierite gneisses of the Akulleq terrane at Simiuttat, SW Greenland. X-ray powder diffraction powder gave a = 18.526(7),b = 17.979(15), c = 5.285(23) Å; a single crystal has a = 18.546(7), b = 17.950(16), c = 5.280(1) Å, space group Pnma with some reflections being notably broader than others. Spot EMPA yielded composite analyses: AlIV = 0.89–1.3, Mg/(Mg+Fe2+) = 0.57–0.61, Na/AlIV = 0.22–0.26. AFM imaging of {210} cleavage surfaces, showed a uniform corrugated morphology parallel to [001]; wavelength was 190–350 nm, mean 250 nm, amplitude 3 nm. A plan view resembles TEM images of (010)-parallel exsolution textures of orthoamphiboles. A second set of corrugations may crosscut the [001]-parallel ridges at 20–25°, akin to reported lamellar intergrowths developed parallel to both (010) and (120). Unequivocal evidence linking topography with lamellae is absent. In contrast to the conventional multi-layer reflector model, the ridged surface provides an additional origin for iridescence, acting as a diffraction grating. Included zircons, 50–10 μm, have Hf/Zr = 0.008–0.012, Hf+FeIIc. 0.16. 207Pb/206Pb ages are from 2690 to 2770 Ma, averaging 2732±10 Ma. Coexisting, included Th-, La-, Ce-, Pr-, Nd-, Gd-, Y-monazites have 207Pb/206Pb ages from 2680 to 2720 Ma, averaging 2707±12 Ma. The included crystals grew during a late Archaean metamorphism that produced overgrowths on zircons within gneisses to the north, but with Simiuttat grains showing a more complex history. The lamellae may have developed at the same time, or during a reheating c. 2550 Ma, or in a subsequent Proterozoic metamorphism.

Thermal expansion coefficients were measured for a cancrinite from Bancroft, Ontario, Canada. Measurements of cell parameters and unit-cell volumes were obtained at room temperature and at heating intervals of 50°C over the temperature range from 50 to 1400°C. The unit-cell parameters for cancrinite increase non-linearly with temperature up to 1200°C and shortly thereafter, the mineral melted. The c parameter increases more rapidly than the a parameter, and the c/a ratio increases linearly with temperature. A plausible thermal expansion mechanism for cancrinite, which is based on the framework expansion that occurs as a function of cavity content, is presented. In the thermal expansion of cancrinite, the short Na-H2O in the H2O-Na—H2O chain expands to form equal distances to the two H2O molecules in the chain. This causes the Na atoms to move towards the plane of the six-membered rings and forces the tetrahedra to rotate and the rings become more planar. The Na atoms then form bonds to all six (O1 and O2) oxygen atoms in a ring; the Na-O1 bonds become shorter and the Na-O2 bonds become longer. These effects cause an increase in both a and c, and thus an increase in the c/a ratio. A similar thermal expansion mechanism operates in the sodalite-group minerals where the six-membered rings and Na-Cl bond are involved.

Viséite is a poorly crystalline mineral which is difficult to study by X-ray diffraction pattern. NMR is a very useful technique to study such poorly crystalline minerals, and 31P, 27Al, and 29Si MAS NMR in conjunction with powder XRD results show that at least our Viséite sample is not a single phase with a structure analogous to that of analcime as previously reported. Rather, it is very disordered with a structure similar to that of crandallite and includes other phases including an undefined aluminophosphate, opal, and a framework aluminosilicate, probably a zeolite. The previously reported variations in the Si content of Viséite are probably due to variable amounts of opal and the framework aluminosilicate.

The thermal expansion tensor of crocoite has been determined from high-resolution neutron time-of-flight powder diffraction data. The temperature dependence of the lattice constants between 4.5 K and 290 K have been fitted to a quasi-harmonic Einstein model, and the temperature dependence of the thermal expansion tensor has been calculated for 60 K ≤ T ≤ 290 K. The magnitudes of the principal expansivities and their orientation exhibit saturation behaviour for temperatures above 300 K. The predicted saturated expansion coefficients are α11 = 33.1(1) × 10−6K−1, α22 = 15.72(3) × 10−6K−1, α33 = 3.36(1) × 10−6K−1, with α22 parallel to b and α11 lying at an angle of −37.86(5)° to c for the P21/n setting of the crystal structure. The direction of maximum expansion is approximately parallel to both and the least-squares line passing through the projection of the chromium atoms on (010). The direction of minimum expansion lies approximately parallel to [101]. No evidence was found for either a structural or magnetic phase transition between 4.5 K and 300 K.