The mineralogical characteristics of halloysite in rectorite pelite in the Zhongxiang area, Hubei, China, were investigated using X-ray diffraction, scanning electron microscopy and high-resolution transmission electron microscopy methods. The results show that halloysite crystals exhibit euhedral lamellar, tubular or club-like, and needle-like or fibre-like morphologies, indicating that they crystallized from a significantly water-saturated environment. The mineral assemblage of the rectorite pelite is rectorite, halloysite, illite, gypsum, pyrite and rutile, suggesting a weak supergene alteration. Several features related to crystallization of halloysite were noted. Growth of halloysite on rectorite edge surfaces in voids and twins of halloysite on a nanometer scale with composition plane (110) were found in the Zhongxiang rectorite pelite, and, in particular, the tapered ends of tubes suggest that halloysite crystallized from solution. Disaggregation of lamellar halloysite particles into parallel clusters of single tubular halloysite crystals suggests that because of significant [H2O] activity in the environment, halloysite may have been derived from the alteration of rectorite.

A set of pyribole structures can be derived from a model I-beam containing two distinct silicate chains in which the tetrahedra are rotated by different amounts. The model allows some tetrahedral distortion and is not bound by the parity rule (Thompson, 1970). A subset of pyribole structures which includes all the commonly occurring types can be defined using a new rule: that the structure may contain two types of tetrahedral layer, but no tetrahedral layer may contain two types of tetrahedral chain. This rule is more fundamental than the parity rule and has its origin in the optimization of the edge-to-edge packing of the tetrahedral chains into layers. Pnm21 (amphibole) and Pbc21 (pyroxene) emerge as space groups for ‘low protopyriboles’. The approach used here leads naturally to the − and × -chains notation of Thompson used by Veblen and Burnham (1978).

Published data from pyrrhotine-vapour equilibrium experiments are used to make inferences concerning the high-temperature thermodynamic mixing properties of pyrrhotine. Darken's quadratic formalism provides the justification for plotting activity of sulphur data against (1−X)2, where X is used in Fe1−XS to express the composition of non-stoichiometric pyrrhotine. Such plots show that the thermodynamic behaviour of pyrrhotine appears to be different on either side of X = 0.125, the Fe7S8 composition.

The new mineral species braccoite, ideally NaMn2+5[Si5AsO17(OH)](OH), has been discovered in the Valletta mine dumps, in Maira Valley, Cuneo province, Piedmont, Italy. Its origin is probably related to the reaction between ore minerals and hydrothermal fluids. It occurs as subhedral crystals in brown-red coloured thin masses, with a pale-yellow streak and vitreous to resinous lustre. Braccoite is associated with tiragalloite, for which new data are provided, as well as gamagarite, hematite, manganberzeliite, palenzonaite, quartz, saneroite, tokyoite, unidentified Mn oxides, organic compounds, and Mn arsenates and silicates under study.

Braccoite is biaxial positive with refractive indices α = 1.749(1), β = 1.750(1), γ = 1.760(1). It is triclinic, space group P1̄, with a = 9.7354(4), b = 9.9572(3), c = 9.0657(3) Å, α = 92.691(2), β = 117.057(4), γ = 105.323(3)°, V = 740.37(4) Å3 and Z = 2. Its calculated density is 3.56 g/cm3. The ten strongest diffraction lines of the observed powder X-ray diffraction (XRD) pattern are [d in Å, (I), (hkl)]: 3.055 (69)(22̄1), 3.042 (43)(102), 3.012 (65)(32̄1̄), 2.985 (55)(23̄1̄), 2.825 (100)(213̄), 2.708 (92)(220), 2.627 (43)(23̄2̄), 2.381 (58)(41̄1̄), 2.226 (25)(214̄) and 1.680 (433̄)(36). Chemical analyses by wavelength-dispersive spectroscopy electron microprobe gave (wt.%): Na2O 4.06, CaO 0.05, MnO 41.76, MgO 0.96, Al2O3 0.04, CuO 0.02, SiO239.73, As2O5 6.87, V2O5 1.43, SO3 0.01 and F 0.04. H2O 2.20 was calculated on the basis of 2OH groups p.f.u. Raman spectroscopy confirmed the presence of (SiO4)4–, (AsO4)3– and OH groups. The empirical formula, calculated on the basis of Σ cations-(Na,K) = 11 p.f.u., in agreement with the results of the crystal structure, is Na1.06(Mn2+4.46Mn3+0.32Mg0.19V3+0.01Al0.01Ca0.01)[Si5(As0.48Si0.37V5+0.15)O17(OH)](OH0.98F0.02); the simplified formula is Na(Mn,Mg,Al,Ca)5[Si5(As,V,Si)O17(OH)](OH,F).

Single-crystal XRD allowed the structure to be solved by direct methods and revealed that braccoite is the As-dominant analogue of saneroite. The structure model was refined on the basis of 4389 observed reflections to R1 = 3.47%. Braccoite is named in honour of Dr Roberto Bracco (b. 1959), a systematic minerals collector with a special interest in manganese minerals. The new mineral was approved by the International Mineralogical Association Commission on New Minerals, Nomenclature and Classification (IMA 2013-093).

Amphibole in the lower parts of the Lilloise layered intrusion occurs interstitially and as a replacement of pyroxene; in the upper rocks it is a major cumulus phase. There is an overall trend of increasing Fe/(Fe + Mg) with height. Coupled substitutions which effect the variation in composition of the amphiboles are chiefly Na,K(A)+Al(T) for □A+SiT) and Ti+Al(T) for Fe3+(C)+ Si(T). There is considerable variation in composition both on the specimen scale and within individual grains. This variation, plus scatter found in plots of the coupled substitutions, is partly attributed to many of the amphiboles having replaced pyroxene and also to the effects of magmatic-hydrothermal fluids.

Non-stoichiometric, carbon-containing crandallite from Guatemala and plumbogummite from Cumbria have been characterized using electron microprobe (EMPA) and wet-chemical analyses, Rietveld analysis of powder X-ray diffraction (PXRD) patterns, and infrared (IR), Raman and cathodoluminescence (CL) spectroscopies. The samples contain 11.0 and 4.8 wt.% CO2, respectively. The IR spectra for both samples show a doublet in the range 1410–1470 cm–1, corresponding to CO3 vibrations. Direct confirmation of CO3 replacing PO4 was obtained from difference Fourier maps in the Rietveld analysis. Carbonate accounts for 67% of the C in the plumbogummite and 20% of the C in the Guatemalan crandallite, the remainder being present as nano-scale organic carbon. The CO3 substitution for PO4 is manifested in a large contraction of the tetrahedral volume (14–19%) and by a contraction of the a axis, analogous to observations for carbonate-containing fluorapatites. Stoichiometric crandallite from Utah was characterized using the same methods, for comparison with the non-stoichiometric, carbon-bearing phases.

Sodic-calcic and alkali amphiboles from benmoreitic members of the Igaliko Dyke Swarm contain up to 4.13 wt. % ZrO2. It is proposed that Zr enters the amphiboles by a coupled substitution of

(where C = octahedral site and T = tetrahedral site) to produce the richest Zr-bearing amphiboles so far identified, with compositions ranging up to

These amphiboles crystallize at a late stage from magmas which were Zr-rich, highly peralkaline and hydrous, with an fo2 close to the synthetic QMF buffer. The incorporation of Zr in to the amphibole is a consequence of the failure of other Zr-bearing phases (such as zircon, baddeleyite, eudialyte) to crystallize.

Several bodies of moderately foliated and porphyroblastic metabasites crop out on the SE side of the metamorphic cover of the Karkonosze granite within metapelites of the Sowia Dolina area (West Sudetes, Saxothuringian zone). Depending on the microstructural setting of the Ca-amphiboles in the rocks, different mineral-chemical trends have been determined for Si, XMg, AlVI, A[Na+K] which serve as semi-quantitative indicators of temperature and pressure changes. Porphyroblasts and prisms oblique to the main foliation in schistose metabasites show zoning from Mg-hornblende and actinolite to tschermakite, and then to Mg-hornblende (or actinolite). Matrix amphiboles and those in pressure shadows around some porphyroblasts have tschermakitic cores and actinolitic rims. Rarely, Ca-amphibole is accompanied in schists by late- to post-tectonic cummingtonite. Thermobarometric calculations involving empirically calibrated amphibole equilibria enable a reconstruction of P-T paths for individual rocks and the unravelling of the metamorphic evolution of the metabasites. Peak metamorphic temperatures of 615–640°C and pressures of 7.3–8.2 kbar were preceded by a variably preserved earlier stage (T = 370–550°C, P = 2.8–6.2 kbar). The final metamorphic episode took place at 450–550°C and 2.5–4.8 kbar and is recorded particularly in rocks close to the Karkonosze pluton. The metabasites shed new light on the history of metamorphism in the Sowia Dolina area. The first two stages of MP-MT metamorphism, coeval with Variscan deformation events (continental collision, burial and subsequent exhumation), took place under epidote-amphibolite then amphibolite facies conditions. The last stage partly concurred with the final stages of Variscan deformation and overlapped the onset of thermal activity associated with the Karkonosze granite. This metamorphic event is documented by metabasites (occasionally cummingtonite-bearing) outcropping close to the granite. Finally, a prehnitebearing assemblage reflects retrograde re-equilibration under greenschist/sub-greenschist facies conditions (T <300–350°C, P <2.5–3 kbar), which might also be partly due to hydrothermal activity around the pluton.

Identification of clinopyroxene lamellae in Bushveld-type orthopyroxene from the Greenhills Ultramafic Complex has been made on the basis of partial analysis by electron microprobe as well as by unit cell determination by prolonged exposure to X-rays of single crystals of orthopyroxene. Lamellae averaging Ca42Mg47Fe11 in composition with an approximate unit cell a 9·79, b 8·90, c 5·29 Å, β 106° 14′, occur in orthopyroxene Ca2Mg67Fe31 with unit cell a 18·28, b 8·85, c 5·20 Å. The Greenhills lamellae are of orientation identical to those described by Hess (1960), which share c and b axes with host orthopyroxene.

Edingtonite and yugawaralite showing sectoral textures were studied by polarized optical microscopy and X-ray analysis. In edingtonite, the m{110} sector (2Vα = 22°) is optically triclinic and the c{001} sector (2Vα = 52°) is orthorhombic. In yugawaralite, the k{011} sector is optically monoclinic, whereas the v{120} sector is triclinic. Their crystal structures were determined. The results of refinement showed that the space groups of the k{011} (Rw = 4.5%) and v{120} (Rw = 5.1%) growth sectors are monoclinic Pc and triclinic P1, respectively. In the v{120} sector, several interatomic distances, bond angles and site occupancies are different with respect to a symmetrical plane of the structure, and therefore the monoclinic c glide is extinct. Thus, the X-ray symmetry correlates with the optical one. From the relationship between the surface and internal texture, the symmetry and sector can be explained by cation (Al/Si) ordering during non-equilibrium crystal growth.

Short-range order in the oxygen co-ordination shell of the Ca ion in a glass of composition Ca3Mg4Al2Si7O24 is investigated by analysis of the extended X-ray absorption fine structure. The estimate of disorder in the short-range oxygen co-ordination is no greater than that for crystalline samples of diopside and bytownite. An estimate of the oxygen environment of calcium in the particular glass is included.

A new method to measure thermal diffusivity in samples at simultaneous high pressure and high temperature is presented. The sample is placed inside a cylindrical heater and subjected to a heater power that varies sinusoidally with time. The diffusion of the temperature variations into the sample is monitored using radiographic imaging of marker foils. This provides measurements of the phase lag and amplitude variation of the temperature cycle at a range of radii from the sample axis without the need for multiple thermocouples. The technique is tested using a NaCl sample at 4 GPa; the best-fit thermal diffusivity for NaCl at 4 GPa and 673 K is 2.4±0.5x10-6 m2/s.

The separation of iron-titanium oxide droplets and the formation of olivine, in the Freetown layered gabbro, depleted the magma in iron and enriched the magma in copper. In magma injections in which the sulphur fugacity was sufficiently high, this resulted in the separation of immiscible copper sulphide droplets closely associated with the iron-titanium oxide droplets, and both were subsequently enclosed by olivine. A lower sulphur fugacity in other injections of magma suppressed the separation of the copper, which later appeared as native copper associated with euhedral titanomagnetite, and was enclosed by feldspar. Crystallization of the iron-titanium oxide droplets and subsolidus diffusion has resulted in granular exsolution of ilmenite from the droplets and lamellar exsolution of ilmenite in the euhedral titanomagnetite.

Two sediment cores retrieved at the northern slope of Sakhalin Island, Sea of Okhotsk, were analysed for biogenic opal, organic carbon, carbonate, sulphur, major element concentrations, mineral contents and dissolved substances including nutrients, sulphate, methane, major cations, humic substances and total alkalinity. Down-core trends in mineral abundance suggest that plagioclase feldspars and other reactive silicate phases (olivine, pyroxene, volcanic ash) are transformed into smectite in the methanogenic sediment sections. The element ratios Na/Al, Mg/Al and Ca/Al in the solid phase decrease with sediment depth indicating a loss of mobile cations with depth and producing a significant down-core increase in the chemical index of alteration.

The crystal structure of antimonian asbecasite in an ejectum of hypabyssal origin occurring at Tre Croci near Vetralla, Vico volcanic complex, Roman potassic province, Latium, Italy, has been refined to R = 0.042, and is compared to the original crystal structure determination carried out on the Sb-free asbecasite of hydrothermal metamorphic origin from the type-locality, Cherbandung in Binna valley, Monte Leone nappe, Switzerland. New electron microprobe analyses of samples from both localities demonstrate crystal-chemical features that permit distinction between asbecasites from the two occurrences, so far the only known localities for this mineral.

Wilhelmgümbelite, ideally [ZnFe2+Fe33+(PO4)3(OH)4(H2O)5]·2H2O, is a new secondary phosphate mineral related closely to schoonerite, [ZnMnFe22+Fe3+(PO4)3(OH)2(H2O)7]·2H2O, from oxidized zones of the Hagendorf-Süd pegmatite, Hagendorf, Oberpfalz, Bavaria, Germany. Wilhelmgümbelite occurs as radiating sprays of needle-like rectangular laths, up to 0.2 mm long and with colour varying from light yellow brown to orange red. Cleavage is perfect parallel to {010}. The mineral is associated closely with an oxidized pseudomorph of phosphophyllite, recently named steinmetzite. Other associated minerals are albite, apatite, chalcophanite, jahnsite, mitridatite, muscovite and quartz. The calculated density of wilhelmgümbelite is 2.82 g cm–3. It is optically biaxial (+) with α = 1.560(2), β = 1.669(2), γ = 1.718(2), 2V(meas) = 63(1)° and 2V(calc.) = 65°. Dispersion is weak with r > v, orientation X = b, Y = c, Z = a. Pleochroism is weak, with coloursZ = orange brown, Y = yellow brown, X = light yellow brown, Z >> Y > X. Electron microprobe analyses (average of seven analyses, seven crystals) with H2O and FeO/Fe2O3 calculated on structural grounds, gave FeO 5.8, Fe2O3 25.0, MnO 2.6, ZnO 16.4, P2O5 28.7, H2O 23.4, total 101.9 wt.%. The empirical formula, scaled to 3 P and OH– adjusted for charge balance is Zn1.50Mn0.272+Fe0.602+Fe2.333+(PO4)3·(OH)2.73(H2O)8.27. The structural formula is [Zn(Mn0.27Fe0.733+)∑1.0(Zn0.25Fe0.152+Fe0.603+)∑1.0(Zn0.25Fe0.452+)∑0.7Fe3+(PO4)3(OH,H2O)9]·2H2O.Wilhelmgümbelite has orthorhombic symmetry, Pmab, Z = 4, with the unit-cell parameters of a = 10.987(7) Å, b = 25.378(13) Å, c = 6.387(6) Å and V = 1781(2) Å3. The strongest lines in the powder X-ray diffraction pattern are [dobs in Å(Iobs) (hkl)] 12.65 (100) (020); 8.339 (5) (120); 6.421 (14) (001); 6.228 (8) (011); 4.223 (30) (120) and 2.111 (7) (0 12 0). Wilhelmgümbelite is an oxidized form of schoonerite, with the Mn2+ replaced principally by Fe3+. Its structure differs from that of schoonerite in having the Zn partitioned between two different sites, one five-coordinated as in schoonerite and the other tetrahedrally coordinated. Wilhelmgümbelite also differs structurally from schoonerite in having partial occupation of one of the Fe sites, which appears to be correlated with the Zn partitioning.

Gypsum evaporites are forming under desiccating conditions in relict cave passages in Mynydd Llangattwg, south Wales. Sulphur isotope compositions of these sulphates indicate that oxidation of diagenetic pyrite in the overlying Millstone Grit is the source of sulphate solutions, rather than dissolution of evaporitic sulphate in the limestones.

Katophorite has the ideal formula ANaB(NaCa)C(Mg4Al)T(Si7Al)O22W(OH)2 (Hawthorne et al., 2012). No published analyses of amphiboles fall in the katophorite compositional field, except that of Harlow and Olds (1987) for an amphibole from near Hpakan in the Jade Mine Tract, Myanmar. This amphibole was approved by the International Mineralogical Association Commission on New Minerals, Nomenclature and Classification (vote 2013-140) as katophorite, and is reported here. Holotype katophorite is monoclinic, space group C2/m, a = 9.8573(8), b = 17.9617(15), c = 5.2833(4) Å, β = 104.707(2)°, V = 904.78(13) Å3, Z = 2. The calculated density is 3.091 g cm–3. In plane-polarized light, katophorite is pleochroic, X = pale blue (medium), Y = light blue-green (strongest), Z = colourless; X ∧ a = 30.6° (β obtuse), Y || b, Z ∧ c = 15.8 (β acute). It is biaxial negative, α = 1.638, β = 1.642, γ = 1.644, all ± 0.002; 2Vobs = 73(1)°, 2Vcalc = 70°. The eight strongest lines in the powder X-ray diffraction pattern are [d in Å (I)(hkl)]: 2.700 (100)(151), 3.129 (69)(310), 2.536 (65)(202), 3.378 (61)(131), 8.421 (55)(110), 2.583 (46)(061), 2.942 (43)(221) and 2.334 (41)(351). Electron-microprobe analysis of the refined crystal gave SiO251.74, Al2O37.38, TiO2 0.14, FeO 1.55, Fe2O3 2.82, MgO 18.09, CaO 8.17, Na2O 6.02, K2O 0.24, F 0.06, H2Ocalc. 1.80, Li2Ocalc. 0.09, sum 100.55 wt.% (Li2O and H2O based on the results of single-crystal structure refinement). The formula unit, calculated on the basis of 24 (O,OH,F) with (OH + F + O) = 2 is: A(Na0.85K0.04)Σ=0.89B(Ca1.22Na0.78)Σ=2.00C(Mg3.76Al0.43Fe0.303+Cr0.273+Fe0.182+Li0.05Ti0.014+)Σ=5.00T(Si7.21Al0.79)Σ=8.00O22W[(OH)1.67O0.30F0.03)]Σ=2.00.