In situ high temperature single crystal X-ray diffraction (XRD) experiments have been performed on a chemically quasi-ideal omphacite sample up to 1000°C. The lattice parameters were studied as a function of temperature, and their thermal expansion coefficients determined. The b and c cell edges show discontinuities as a function of temperature which are interpreted here in terms of intracrystalline cation diffusion processes. Structure refinements have been carried out using data collected at room temperature, at 800°C and at ambient conditions after cooling. The structural behaviour as a function of temperature of chemically quasi-ideal omphacites is compared with those of jadeite and diopside.

The mineralogical status of ilmenite from a prominent modern placer deposit of India is illustrated using different techniques. Compositional, powder XRD, TGA and SEM analyses prove that consistent low temperature alteration took place in Chavara ilmenite leading to the formation of a pseudorutile-hydrated-ilmenite stage. Except for the indication of a geochemical zonation at the southern tip of the deposit, the Chavara ilmenite points to a common origin throughout its 22 km stretch along the coast. We advocate a major segregation activity by marine factors to the accumulated sediments in the shelf zone in order to originate such a huge deposit of homogeneous composition.

The coarse-grained wolgidite variety of lamproite from the Wolgidee Hills of the West Kimberley District of Western Australia has previously yielded three new minerals. Two of these, wadeite and magnophorite (Prider, 1939), were discovered and described by the author when working as a research student under Professor Tilley's supervision and the third, priderite (Norrish, 1951), resulted from an X-ray study of material previously considered by the author to be rutile.

A Granite (G-1) from Westerley, Rhode Island, and a diabase (W-1) from Centerville, Virginia, were recently analysed by some 34 analysts in different countries for the purpose of obtaining thoroughly reliable rock standards for spectrochemical analysis. Most determinations were made by so-called classical methods of chemical analysis. The results of the investigation have been discussed by Fairbairn and others. Fairbairn examined the results statistically and, using the relative deviation (standard deviation expressed as a percentage) as a measure of precision, concluded that precision deteriorated with a decrease in the concentration of a constituent. In the present paper this general observation will be demonstrated quantitatively by means of a graphical presentation, thus providing the petrologist with a guide for rapidly assessing and comparing the precision of classical methods of chemical analysis over considerable concentration ranges.

Relict clinopyroxenes from metadolerites of the Early Permian Petroi Metabasalt formation, studied by electron microprobe, show a limited compositional range near the diopside-augite boundary in the pyroxene quadrilateral. Clinopyroxene analyses from three metadolerites, grouped in approximately equal Fs contents, define an overall smooth trend between Fs10 and Fs16. This is typical of clinopyroxenes from mildly alkaline basic magmas. Pyroxene stoichiometry suggests high Fe3+ contents (0.04 to 0.20 a.f.u.), which with high Al (0.10 to 0.31 a.f.u.) and Ti (0.03 to 0.08 a.f.u.) implies that CaTiAl2O6 and CaFe3+AlSiO6 are important ‘other components’. Relative Alz in CaFe3+AlSiO6 decreases and consequently CaTiAl2O6 increases with progressive fractionation. This, with the Fe2+:Fe3+ ratios in the Petroi clinopyroxenes, suggests falling ƒO2 in the magma with fractionation. The ƒO2 controlled entry of Alz, Tiy and Nax into the clinopyroxenes and hence the Petroi clinopyroxene trend.

The occurrence is reported of a saline spring water from Weardale, which compositionally closely resembles other saline waters derived from the Carnmenellis granite, southwest England. The total dissolved solutes achieve approximately 38 000 mg/L, and alkali geothermometers suggest equilibration temperatures of approximately 150°C, equivalent to a depth of 4 km. Using Na, K and Li it is possible to compare the composition of the spring water with those of other spring waters derived from Carboniferous sequences adjacent to the North Pennine Orefield and with published data for fluid inclusions from North Pennine fluorite. These compositional parameters suggest that the ancient mineralizing fluids resemble modern Carboniferous sediment-derived waters and contain a relatively minor component of granite-derived water. Data for Br and Cl indicate that a significant component of the present day Weardale spring waters was probably ultimately derived from organic-rich sedimentary sequences while data for K, Na and Li indicate the importance of a component derived from a permeable granite aquifer. The Weardale springwaters continue to have ‘mineralizing’ potential, in view of the possibility that they may have precipitated quartz or chalcedony during their ascent.

Luboržákite, ideally Mn2AsSbS5, is a new mineral from the Vorontsovskoe gold deposit, Northern Urals, Russia. It forms long-prismatic crystals up to 70 × 20 μm and anhedral grains of the same size embedded in the matrix of Mn-bearing dolomite and Mn-bearing calcite. Associated minerals include pyrite, orpiment, realgar, stibnite, aktashite, alabandite, boscardinite, chabournéite, coloradoite, clerite, écrinsite, gold, routhierite, sphalerite and twinnite. Luboržákite is black, opaque with metallic lustre and has a black streak. It is brittle and has an uneven fracture. No cleavage and parting have been observed. Mohs hardness is 4–4½. Dcalc = 4.181 g cm–3. In reflected light, luboržákite is tin-white, weakly anisotropic with rotation tints varying from dark grey to grey. The chemical composition of luboržákite is (wt.%; electron microprobe, WDS mode): Mn 21.23, Cu 0.29, Ag 0.56, Pb 1.90, As 15.25, Sb 27.03, S 33.23, total 99.49. The empirical formula based on the sum of all atoms = 9 apfu is Mn1.86Pb0.04Ag0.03Cu0.02As0.98Sb1.07S5.00. The new mineral is monoclinic, space group C2/m with a = 12.5077(6), b = 3.8034(2), c = 16.0517(8) Å, β = 94.190(4)°, V = 761.57(6) Å3 and Z = 4. The crystal structure of luboržákite was solved from the single-crystal X-ray diffraction data to R = 0.0383 for 712 observed reflections with I > 3σ(I). Luboržákite is a new member of the heterochemical isostructural series of ‘unit-cell twinned’ structures, named the pavonite series. The new mineral honours Lubor Žák, a prominent Czech crystallographer and the professor of the Charles University in Prague, Czech Republic.

Whiteite-(CaMnMn), CaMnMn2Al2[PO4]4(OH)2·8H2O, is a new hydrous phosphate of Ca, Mn and Al, which is closely related to both jahnsite-(CaMnMn) and the minerals of the whiteite group. It is monoclinic, P2/a, with a = 15.02(2), b = 6.95(1), c =10.13(3) Å, β = 111.6(1)°, V = 983.3(6) Å3, Z = 2 (from powder diffraction data) or a = 15.020(5), b = 6.959(2), c = 10.237(3) Å, β = 111.740(4)°,V = 984.3(5) Å3, Z = 2 (from single-crystal diffraction data). The mineral was found in the Hagendorf Süd granitic pegmatite (Germany) as small (up to 0.5 mm in size) crystals elongated on a and tabular on {010}. The crystals are either simply or polysyntheticallytwinned on {001}. They crystallize on the walls of voids within altered zwieselite crystals or form coronas (up to 1 mm in diameter) around cubic crystals of uraninite. The mineral is transparent, colourless to pale yellow (depending on Al–Fe3+ substitution), with a vitreouslustre and a white streak. The cleavage is perfect on {001}, the fracture is stepped and the Mohs hardness is 3½. In transmitted light, the mineral is colourless; dispersion was not observed. Whiteite-(CaMnMn) is biaxial (+), α = 1.589(2), β = 1.592(2), γ = 1.601(2)(589 nm), 2Vmeas = 60(10)°, 2Vcalc = 60.3°. The optical orientation is X = b, Z^a = 5°. The calculated and measured densities are D calc = 2.768 and D meas = 2.70(3) g cm–3, respectively.The mean chemical composition determined by electron microprobe is Na2O 0.53, MgO 0.88, Al2O3 11.66, P2O5 34.58, CaO 4.29, MnO 17.32, FeO 8.32, ZnO 2.60 wt.%, with H2O 19.50 wt.% (determined by the Penfield method), giving atotal of 99.68 wt.%. The empirical formula calculated on the basis of four phosphorus atoms per formula unit, with ferric iron calculated to maintain charge balance, is (Ca0.63Zn0.26Na0.14)Σ1.03(Mn0.60Fe0.40 2+)Σ1.00(Mn1.40Fe0.37 2+Mg0.18Fe0.06 3+)Σ2.01(Al1.88Fe0.12 3+)Σ2.00[PO4]4(OH)2·7.89H2O.The simplified formula is CaMnMn2Al2[PO4]4(OH)2·8H2O. The mineral is easily soluble in 10% HCl at room temperature. The strongest X-ray powder-diffraction lines [listed as d in Å (I) (hkl)]are as follows: 9.443(65)(001), 5.596(25)(011), 4.929(80)(210), 4.719(47)(002), 3.494(46)(400), 2.7958(100)(022). The crystal structure of whiteite-(CaMnMn) was refined for a single crystal twinned on (001) to R 1 = 0.068 on the basis of 5702 unique observed reflections. Itis similar to the structures of other members of the whiteite group. The mineral is named for the chemical composition, in accordance with whiteite-group nomenclature.

The structure of a synthetic sample of analcime has been determined as a function of temperature between 30–300 K by high-resolution neutron powder diffraction. Although there are some reports of samples of analcime having non-cubic structures, the sample in our experiments remained cubic (space group la3d), and hence disordered, down to low temperatures. The absence of phase transitions involving ordering of the orientations of the water molecules, ordering of the sodium positions, or a displacive instability as in leucite and related materials, is discussed. We speculate that part of the reason for the absence of ordering of the water molecules or sodium cations is associated with the Al/Si disorder, which cannot order at low temperatures. We also discuss the likely distribution of the orientations of the water molecules at low temperatures, and propose that the water diads lie close to any of the crystal diads with the H-H Vectors lying close to the triads.

Mineralogical, bulk and field leachate compositions are used to identify important processes governing the evolution of discharges from a coal spoil heap in County Durham. These processes are incorporated into a numerical one-dimensional advective-kinetic reactive transport model which reproduces field results, including gas compositions, to within an order of magnitude. Variation of input parameters allows the effects of incorrect initial assumptions on elemental profiles and discharge chemistry to be assessed. Analytical expressions for widths and speeds of kinetic reaction fronts are developed and used to predict long-term development of mineralogical distribution within the heap. Results are consistent with observations from the field site. Pyrite oxidation is expected to dominate O2 consumption in spoil heaps on the decadal timescale, although C oxidation may stabilize contaminants in effluents on the centennial scale.

Manganotantalite replacement by (1) microlite and (2) ferrotantalite, and changes in composition of uranoan microlite from rare-metal pegmatites in South Africa and Namibia have been investigated with the electron microprobe. A uranmicrolite from Karibib, Namibia contained 14.35% UO2, 1.03% PbO, 56.12% Ta2O5, 13.18% Nb2O5, 0.58% Fe2O3, 6.87% CaO, 0.54% SrO, 0.59% MnO, 0.86% Na2O and 0.47% F. Analyses along traverses across a 1.3 mm uranoan microlite, Tantalite Valley, Namibia, revealed two essentially distinct compositions: a more hydrated rim area of 200 µm radius containing 7% higher Ta2O5, 10% lower CaO and 1.3% lower F than a main central area of slightly variable composition. Back-scattered electron images reveal zoning and distinctive subspheroidal structures. New data and structural features are given for radioactive uranoan microlite from Namaqualand, South Africa. These crystals contain remnants of a bismuth phase and are in various stages of replacement. In the microlites replacing manganotantalite, the microlite reflects the composition of the replaced mineral. At Rubicon Mine, Karibib, a narrow marginal zone of mangantantalite is replaced by ferrotantalite along cleavages; a zone of intermediate composition is apparent. Detailed traverses have been completed across all of these crystals.

North Motzfeldt is an intrusive igneous centre within the Igaliku (formerly spelt Igaliko) complex, Gardar Province, South Greenland. A detailed field description of the centre is given, with preliminary geochemical and isotopic data. The North Motzfeldt centre is intruded into Ketilidian granitoid basement rocks, and current exposure retains parts of the original roof against earlier Gardar eruptives and clastic sediments of the Eriksfjord formation. The unconformity between the Ketilidian and the overlying Eriksfjord is believed to have been crucial in the siting of the centre. The centre is subdivided into two major units, NM1 and NM2. This was followed by significant peralkaline nepheline microsyenite in sheets, characterized by rare element-rich accessory minerals including rinkite-mł sandrite, pyrochlore and låvenite. A significant microsyenite body is called NM3. A preliminary Rb-Sr isochron of 1226±27 Ma indicates a far younger age for the centre than previously thought (~;1350 Ma). Cross-cutting relationships between North Motzfeldt and rocks of the adjacent Motzfeldt centre require a reappraisal of the chronology of Motzfeldt magmatism. We suggest that rocks previously believed to comprise the Motzfeldt centre represent the products of multiple phases of magmatism from Early- to Mid-Gardar times.

Electron probe analyses have been made of eight kaersutites from San Carlos, Arizona, and one from Kakanui, New Zealand; also of olivine, clinopyroxene, ilmenite, and spinel from San Carlos. There is not as yet adequate evidence that the kaersutite is an upper mantle phase.

Differential thermal analysis of a rapidly reversible transition in carnegieite to 7 kbar shows the transition temperature increases from ⪝ 707°C (on heating) at I bar with initial slope ≈ 8·0 deg kbar−1 and anomalous curvature (d2T/dp2 > o), with hysteresis between heating and cooling signals that decreases with pressure. DTA of rapidly reversible transitions in nepheline shows the very subtle transition near 185°C (on heating) at 1 bar decreases with pressure to ≈ 170°C near 2-3 kbar and hardly varies in temperature up to 6 kbar; and the higher temperature transition increases from ≈ 872°C (on heating) at 1 bar with slope ≈ 25 deg kbar−1, to 5 kbar, with the hysteretic interval remaining essentially unchanged in the investigated range.

The degree of metamorphism affecting the Devonian-Carboniferous rocks of the Palaeozoic Cinco Villas massif has been studied by (a) petrographic techniques, (b) illite crystallinity, and (c) degree of graphitization of the carbonaceous material. Some mineralogical differences have been found between the Devonian and Carboniferous rocks; paragonite and mixed-layer paragonite/muscovite, typical of anchimetamorphic areas, appear in the Devonian but are not found in the Carboniferous rocks. These are characterized by the local appearance of chloritoid, garnet, amphibole, epidote, andalusite and biotite, and the generalized presence of muscovite/chlorite. Illite crystallinity shows a metamorphic zonation (anchizone epizone) towards the granitic Aya massif, and a concentric pattern around the intrusive body.

The optical analysis shows that the first effects of the regional metamorphism began before the D2 deformation, reaching its paroxysm during this phase and continuing afterwards. The degree of graphitization evolves progressively with metamorphism, and this fact is reflected in an exponential relationship between d(002) and crystallinity Lc(002). The similarity in the degree of graphitization between homologous materials within and outside the Aya aureole suggests a similar kinetic factor for both the thermal and regional metamorphisms, or a similar duration time. This fact, as well as the distribution and relationship between the deformation and recrystallization of the minerals, suggests a syn-plutonic regional metamorphism developed at low pressures, in accordance with the value of the b0 parameter for the white micas, and probably a maximum temperature of about 500°C.

Niccolite and other nickel-bearing minerals have been found in magnetite-rich ore at Lady's Rake Mine [NY 8063 3414] in the North Pennines 5.5 km NW of Langdon Beck, Teesdale, Co. Durham. Associated ore minerals include galena, sphalerite, chalcopyrite, pyrite, and pyrrhotite. Similar magnetite-rich ores, in places bearing ugrandite garnets, have been located at two nearby localities, though without nickel minerals. Petrographic study indicates that this unusual assemblage developed in a skarn environment, probably related to the intrusion of the Whin Sill. Field evidence suggests an association with the Teesdale Fault system. Electron microprobe analyses show that Lady's Rake niccolite is near to end-member composition: analyses of other North Pennine niccolites show up to 25 at. % substitution of S and Sb for As.

The new mineral novograblenovite, (NH4,K)MgCl3·6H2O, was found on basaltic lava from the 2012–2013 Tolbachik fissure eruption at the Plosky Tolbachik volcano, Kamchatka Peninsula, Russia. It occurs as prismatic, needle-like transparent crystals together with gypsum and halite. Novograblenovite was formed due to the exposure of the host rocks to eruptive gas exhalations enriched in HCl and NH3. Basalt was the source of potassium and magnesium for the mineral formation. Novograblenovite crystallises in the monoclinic space group C2/c, with unit-cell parameters a = 9.2734(3) Å, b = 9.5176(3) Å, c = 13.2439(4) Å, β = 90.187(2)°, V = 1168.91(2) Å3 and Z = 4. The five strongest reflections in the powder X-ray diffraction pattern [dobs, Å (I, %) (h k l)] are: 3.330 (100) (2 2 0), 2.976 (45) ($\bar{1}\; 1\; 4$), 2.353 (29) ($\bar {2}\; 2\; 4$), 3.825 (26) (2 0 2), 1.997 (25) ($\overline {4\; 2} $ 2). The density calculated from the empirical formula and the X-ray data is 1.504 g cm–3. The mineral is biaxial (+) with α = 1.469(2), β = 1.479(2) and γ = 1.496(2) (λ = 589 nm); 2Vmeas. = 80(10)° and 2Vcalc. = 75.7°. The crystal structure (solved and refined using single-crystal X-ray diffraction data, R1 = 0.0423) is based on the perovskite-like network of (NH4,K)Cl6-octahedra sharing chlorine vertices, and comprises [Mg(H2O)6]2+ groups in framework channels. The positions of all independent H atoms were obtained by difference-Fourier techniques and refined isotropically. All oxygen, nitrogen and chlorine atoms are involved in the system of hydrogen bonding, acting as donors or acceptors. The formula resulting from the structure refinement is [(NH4)0.7K0.3]MgCl3·6H2O. The mineral is named after Prokopiy Trifonovich Novograblenov, one of the researchers of Kamchatka Peninsula, a teacher, naturalist, geographer and geologist.

In 1884, Lorenzen proposed the formula MgAl2SiO6 for his new mineral kornerupine from Fiskenæsset and did not suspect it to contain boron. Lacroix and de Gramont (1919) reported boron in Fiskenæsset kornerupine, while Herd (1973) found none. New analyses (ion microprobe mass analyser and spectrophotometric) of kornerupine in three specimens from the type locality, including the specimens analysed by Lorenzen and Herd, indicate the presence of boron in all three, in amounts ranging from 0.50 to 1.44 wt.% B2O3, e.g. (Li0.04 Na0.01 Ca0.01) (Mg3.49 Mn0.01 Fe0.17 Ti0.01 Al5.64)Σ9.30 (Si3.67 Al1.02 B0.31)Σ5 O21 (OH0.99 F0.01) for Lorenzen's specimen. Textures and chemical compositions suggest that kornerupine crystallized in equilibrium in the following assemblages, all with anorthite (An 92–95) and phlogopite (XFe = atomic Fe/(Fe + Mg) = 0.028–0.035): (1) kornerupine (0.045)-gedrite (0.067); (2) kornerupine (0.038–0.050)-sapphirine (0.032–0.035); and (3) kornerupine (0.050)-hornblende. Fluorine contents of kornerupine range from 0.01 to 0.06%, of phlogopite, from 0.09 to 0.10%. In the first assemblage, sapphirine (0.040) and corundum are enclosed in radiating bundles of kornerupine; additionally sapphirine, corundum, and/or gedrite occur with chlorite and pinite (cordierite?) as breakdown products of kornerupine. Kornerupine may have formed by reactions such as: gedrite + sapphirine + corundum + B2O3 (in solution) + H2O = kornerupine + anorthite + Na-phlogopite under conditions of the granulite facies. Boron for kornerupine formation was most likely remobilized by hydrous fluids from metasedimentary rocks occurring along the upper contact of the Fiske⇒set gabbro-anorthosite complex with amphibolite.

Molybdenite from two porphyry copper mineralisation sites within the South Urals was studied by electron microprobe (EMPA), micro x-ray diffraction (μXRD) and electron backscattered diffraction (EBSD) methods. Elevated contents of rhenium (0.2 to 0.4, sometimes up to 1.1 wt.%) form linear zones from several to tens of micrometres wide and up to hundreds of micrometres long parallel to the elongation of molybdenite flakes. In most cases Re-rich zones are composed of the rhombohedral (3R) polytype of molybdenite, while the rest of the molybdenite flakes with ca. 0.1 wt.% of Re consist of hexagonal (2H) molybdenite. In rare cases Re-rich zones are confined to grain boundaries of molybdenite-2H. It is shown that both μXRD and EBSD are the most appropriate tools to distinguish different polytypes within a single grain of molybdenite.