While undergoing 'dry' homogenization at 980°C the 2̄01 X-ray reflections of sodic lowalbite- microcline microperthites show that phase compositions recapitulate (but in a reverse timesense) the unmixing history of ordered feldspars about a solvus with a critical composition near 26 mole per cent KAlSi3O8.

Rapid, accurate silica determinations have been made titrimetrically following decomposition by HClO4-HF in a ‘Teflon’ vessel, the volatilized silicon tetrafluoride being precipitated as K2SiF6 in a HF-KF-glycerol-alcohol mixture. After filtration and washing with alcohol the precipitate is dissolved in boiling water, then titrated with NaOH. This method has many advantages over conventional gravimetric or spectrophotometric procedures.

Favourability of uranium mineralization in six tertiary granitic plutons of the Alaska Range in the Talkeetna and Mt McKinley quadrangles was studied. The uranium concentrations of drainage sediment samples, which were collected and analysed by the Los Alamos Scientific Laboratory for the National Uranium Resources Evaluation, were statistically evaluated and compared to those of the surrounding area using factor and cluster analyses. The results of this study suggest that five of the six plutons under consideration are likely to contain uranium mineralization. These plutons are probably a potential source rock for uranium in the region.

Byrudite (IMA 2013-045, Raade et al., 2013), with simplified formula (Be,〈)(V3+,Ti)3O6, occurs in emerald-bearing syenitic pegmatites of Permian age at Byrud farm, Eidsvoll, Akershus, South Norway. It has a norbergite-type structure, Pnma, with a = 9.982(1), b = 8.502(1), c = 4.5480(6) Å, V = 385.97(9) Å3, Z = 4. The structure was refined to R1 = 0.045 for 1413 unique reflections. Twinning occurs on {210}. The occupancy of the tetrahedral Be site refined to 0.84(1). The presence of Be was verified by secondary ion mass spectrometry but could not be quantified. Electron-microprobe analyses of the crystal used for structure determination gave the empirical formula (Be0.84〈0.16) (V1.323+Ti1.25Cr0.29Fe0.09Al0.07)Σ3.02O6. There is a strong inverse correlation between V and Cr. The ideal endmember formula is BeV23+TiO6. The mineral is black and opaque with a metallic lustre. Reflectance data in air are reported from 400 to 700 nm. The Commission on Ore Mineralogy required wavelengths are [R1, R2(λ in nm)]:16.6,17.5(470), 16.7,17.9(546), 16.8,18.3(589) and 16.8,18.6(650). The Mohs hardness is ∼7, based on indentation measurements. The mineral is brittle with an uneven fracture; cleavage is not present. D(calc.) = 4.35 g cm–3 for the empirical formula with 0.84 Be a.p.f.u. The strongest reflections of the calculated powder X-ray diffraction pattern are [d in Å (Irel)(hkl)]: 3.721(72)(111), 2.965(100)(121), 2.561(50)(311), 2.464(41)(230), 2.167(24)(231), 1.681(34)(402), 1.671(66)(232), 1.435(23)(630).

Dendoraite-(NH4), (NH4)2NaAl(C2O4)(PO3OH)2(H2O)2, is a new mineral species from the Rowley mine, Maricopa County, Arizona, USA. It occurs in an unusual bat-guano-related, post-mining assemblage of phases that include a variety of vanadates, phosphates, oxalates and chlorides, some containing NH4+. Other secondary minerals found in association with dendoraite-(NH4) are antipinite, fluorite, mimetite, mottramite, relianceite-(K), rowleyite, salammoniac, struvite, vanadinite, willemite, wulfenite and at least one other new mineral. Crystals of dendoraite-(NH4) are colourless blades up to ~0.1 mm in length. The streak is white and lustre is vitreous, Mohs hardness is 2½, tenacity is brittle and fracture is splintery. The calculated density is 2.122 g⋅cm–3. Dendoraite-(NH4) is optically biaxial (–) with α = 1.490(5), β = 1.540(5) and γ = 1.541(5) (white light); 2Vcalc = 15.7°; and orientation X = b. Electron microprobe analysis gave the empirical formula [(NH4)1.48K0.52]Σ2.00Na0.96(Al0.96Fe3+0.03)Σ0.99(C2O4)[PO2.97(OH)1.03]2(H2O)2, with the C, N and H contents constrained by the crystal structure. Dendoraite-(NH4) is monoclinic, P21/n, with a = 10.695(6), b = 6.285(4), c = 19.227(12) Å, β = 90.933(10)°, V = 1292(2) Å3, and Z = 4. The structural unit in the crystal structure of dendoraite-(NH4) (R1 = 0.0467 for 1322 Io > 2σI reflections) is a double-strand chain of corner-sharing AlO6 octahedra and PO3OH tetrahedra decorated by additional PO3OH tetrahedra and C2O4 groups. Topologically, this is the same chain found in the structure of thebaite-(NH4). The decorated chains connect to one another through links to NaO7(H2O) polyhedra to form a [Na(H2O)Al(C2O4)(PO3OH)2]2– sheet, which connect to one another through bonds to (NH4)/K and through hydrogen bonds.

Ancient metamorphic processes are recorded by the formation of metallic-Pb nanospheres in zircon, a product of internal Pb mobilisation and thermally driven concentration. Here, metallic-Pb nanospheres formed within an ore deposit are characterised for the first time using high-angle annular dark field scanning transmission electron microscopy and energy-dispersive X-ray spectroscopy element-distribution mapping. Exceptional examples from the migmatite-hosted Archean–Paleoproterozoic Challenger Au deposit (Central Gawler Craton, South Australia) support widespread metallic-Pb nanosphere formation in zircon from rocks experiencing granulite-facies metamorphism. We also report new trace-element associations found with metallic-Pb nanospheres and a new mode of occurrence, in which Sc ‘haloes’ form adjacent to metallic-Pb nanospheres within the crystalline zircon lattice. This differs to previously characterised examples of metallic-Pb nanospheres associated with amorphous Si-rich glasses and unidentified Al–Ti, or Fe-bearing phases. Multiple modes of metallic-Pb nanosphere occurrences and trace-element associations suggests multiple modes of formation, probably dependant on zircon composition and metamorphic conditions. Identification of metallic-Pb nanospheres in a growing range of geological settings further highlights the mobility of Pb in zircon and the importance of detailed, nanoscale mineral characterisation, in order to constrain accurate geochronological histories for rocks within high-temperature geological environments.

Three samples of halurgite were re-examined: two from the Chelkar salt dome in the North Caspian Region, Western Kazakhstan (the type locality and including the type specimen), and one from a new locality in the Satimola salt dome located in the same region. The crystal structure of halurgite has been solved for the first time on the specimen from Chelkar with the empirical formula Mg3.94[B8.03O13.03(OH)1.97]2·7.16H2O; refinement began with single-crystal X-ray diffraction data and was subsequently refined on a powder sample using the Rietveld method (Rp = 0.0232, Rwp = 0.0354 and Robs = 0.0558). The idealised crystal chemical formula of halurgite is Mg4[B8O13(OH)2]2·7H2O. The mineral is monoclinic, P2/c, a = 13.201(2), b = 7.5622(10), c = 13.185(2) Å, β = 91.834(14)°, V = 1315.6(4) Å3 and Z = 2. The crystal structure is unique. Eight B polyhedra form a fundamental building block [B8O16(OH)2], which is a six-membered borate ring (built by two pairs of B tetrahedra and two B triangles) with two additional triangular BO2(OH) groups. Each [B8O16(OH)2] ring is linked to six adjacent analogous rings to form a [B8O13(OH)2]∞ layer. These layers are connected via MgO6 and Mg(OH)2(H2O)4 octahedra into a microporous heteropolyhedral pseudo-framework. The crystal structure of halurgite can also be described in terms of an approach developed for heterophyllosilicates containing three-layer HOH modules, where HOH refers to an octahedral layer O sandwiched between two heteropolyhedral layers H. In halurgite the HOH module consists of two heteropolyhedral (BO3 triangles + BO4 tetrahedra) borate H layers [B8O13(OH)2]∞ and a central interrupted O layer composed of MgO6 octahedra, whereas a more voluminous Mg(OH)2(H2O)4 octahedral complex and additional H2O molecules are located between HOH modules. Halurgite and four related synthetic H-free borates M2Cd3B16O28 and M2Ca3B16O28 (M = Rb or Cs) can be considered microporous heterophylloborates.

Gatedalite, Zr(Mn22+Mn43+)SiO12, is a new mineral of the braunite group. It is found in hausmannite-impregnated skarn together with jacobsite, Mn-bearing calcite, tephroite, Mn-bearing phlogopite, långbanite, pinakiolite and oxyplumboroméite at the Långban Mn-Fe oxide deposit, Värmland, central Sweden. The mineral occurs as very rare, small (≤60 μm), grey, submetallic, irregularly rounded anhedral grains. Gatedalite has a calculated density of 4.783 g/cm3. It is opaque and weakly anisotropic with reflectivity in air varying between 17.1 and 20.8% in the visible spectral range. Gatedalite is tetragonal, space group I41/acd, with the unit-cell parameters a = 9.4668(6) Å, c = 18.8701(14) Å, V = 1691.1(2) Å3 and Z = 8. The crystal structure was refined to an R1 index of 5.09% using 1339 unique reflections collected with MoKαX-ray radiation. The five strongest powder X-ray diffraction lines [d in Å, (I), (hkl)] are: 2.730(100)(224), 2.367(12)(040), 1.6735(12)(440), 1.6707(29)(048) and 1.4267(16)(264). Electron microprobe analyses in combination with single-crystal structure refinement resulted in the empirical formula: (Zr0.494+Mn0.402+Mg0.07Ca0.02Zn0.01Ce0.013+)Σ1.00(Mn4.443+Fe0.593+Mn0.572+Mg0.41Al0.01)Σ6.02Si0.99O12. Gatedalite is a member of the braunite group (general formula AB6SiO12). It is related to braunite (Mn2+Mn63+SiO12) through the net cation exchange (Zr4+ + Mn2+) → 2Mn3+, which results from the substitutions Zr4+ → Mn2+ at the 8-fold coordinated site (A in the general formula) coupled with a 2Mn2+ → 2Mn3+ substitution at the 6-fold coordinated sites (B in the general formula).

Myrmekites occurring in monzodiorite from the Meichuan pluton in the Dabie ultrahigh-pressure metamorphic belt were investigated. The petrographic evidence demonstrates a metasomatic origin for myrmekite formation at the scale of individual alkali feldspar grains, and that the myrmekitic quartz and plagioclase matrix are generated simultaneously replacing precursor feldspar. Energy-dispersive X-ray spectroscopy and electron microprobe analysis indicate a low anorthite content in the narrow rim of host plagioclase near the myrmekite–alkali-feldspar interface. The Ca2+, Na+ proportion of hydrothermal fluids replacing precursor alkali feldspar is 1:5.4, calculated from the anorthite content of the inner part of the host plagioclase and the neighbouring alkali feldspar. Electron back-scattered diffraction was used to identify the crystallographic orientation of the myrmekitic quartz, plagioclase matrix and the precursor alkali feldspar. The crystallographic orientation relationships (110)Kfs//(11$\bar{2}\bar{1}$)Qtz, (20$\bar{1}$)Kfs//(11$\bar{2}$1)Qtz and [11$\bar{2}3]$Qtz//[001]Kfs between myrmekitic quartz and adjacent alkali feldspar were obtained from statistical analysis. No clear crystallographic orientation relationship between quartz and plagioclase was found. The growth of myrmekitic quartz is constrained by the precursor alkali feldspar rather than the simultaneously crystallised plagioclase. This research is helpful for understanding the intergrowth mechanism during metasomatism.

The three-dimensional distribution of melt in partially molten synthetic samples compositionally corresponding to diopside (90 wt.%)–anorthite (10 wt.%) and doped with PbO, WO3, MoO3, or Cs2O to enhance contrast was studied by X-ray computed tomography (CT) with synchrotron radiation. The heavy elements were strongly concentrated in the melt and contributed to an increase of the X-ray linear attenuation coefficient (LAC) of it. PbO was found to be compatible with silicate melt (>20 wt.% in solution) and incompatible with diopside crystals. Other oxides WO3 (∼10 wt.%), MoO3 (∼5 wt.%) and Cs2O (< 5 wt.%) are also soluble only in the melt. Such doping is useful not only for LAC control in X-ray CT measurements, but also for systematic control of the structure (wetting properties, distribution and connectivity) of partial melt. This technique gives basic information for discussion of the 3D distribution of partial melt having different wetting properties. As PbO was most effective in visualization of the diopside–anorthite partially molten system, CT images of the PbO-bearing sample were used for further 3D investigation of distribution. A distribution of dihedral angles at solid-melt-solid triple junctions ranging from 22 to 55° was observed with the 3D data. This range in angle distribution was probably caused by anisotropy of crystals and the result supports the argument that there is some limitation in a theoretical framework of stereology which estimates the 3D structure based on 2D observations. Investigators have begun to apply X-ray CT to the study of the 3D distribution of partial melts in rocks using synchrotron radiation. Our study on the effect of doping is one approach for developing a technique to investigate 3D melt distribution.

Annivite-(Zn), Cu6(Cu4Zn2)Σ6Bi4S13, is a new IMA-approved mineral species from the Geister vein, Jáchymov ore district, Czech Republic. It occurs as anhedral grains, up to 50 μm in size, and growth zones, up to 100 μm in thickness, hosted by oscillatory zoned annivite-(Zn)/tennantite-(Zn) grains, and associated with Bi-rich tennantite-(Zn), tennantite-(Fe), tetrahedrite-(Zn), the not-yet approved ‘annivite-(Fe)’, bismuth, emplectite, wittichenite and supergene bismite, walpurgite and metazeunerite. In reflected light, annivite-(Zn) is isotropic, pale grey with a brownish shade and very rare pale brown internal reflections. Reflectance data for the four COM wavelengths in air are [λ (nm): R (%)]: 470: 32.3; 546: 32.0; 589: 32.0; 650: 31.6. Electron microprobe analysis gave (in wt.% – average of 5 spot analyses): Cu 36.29, Ag 0.14, Fe 0.08, Zn 7.11, Pb 0.19, As 6.07, Sb 4.50, Bi 21.08, S 23.68, total 99.14. On the basis of ΣMe =16 atoms per formula unit, the empirical formula of annivite-(Zn) is Cu10.13Ag0.02Zn1.93Fe0.03Pb0.02Bi1.79As1.43Sb0.66S13.10. Annivite-(Zn) is cubic, I$\bar 4$3m, with unit-cell parameters a = 10.3545(6) Å, V = 1110.16(19) Å3 and Z = 2. Its crystal structure was refined by single-crystal X-ray diffraction data to a final R1 = 0.0493 on the basis of 278 unique reflections with Fo > 4σ(Fo) and 23 refined parameters. Annivite-(Zn) is isotypic with other tetrahedrite-group minerals. Its crystal chemistry is discussed, and previous findings of Bi-rich tetrahedrite-group minerals are briefly reviewed, along with the description of a second finding of annivite-(Zn) from the abandoned Mauritius tin mine, Hřebečná, Krušné hory Mountains, Czech Republic.

Heflikite, the first Sc-dominant epidote-supergroup mineral, was discovered in two occurrences. The holotype was found in a granitic pegmatite associated with rodingite-like calc-silicate rocks and metasomatised granitic bodies exposed in a serpentinite quarry at Jordanów Śląski near Sobótka, Lower Silesia, SW Poland. The cotype comes from the Heftetjern pegmatite, Tørdal region, Norway. The holotype is composed of (in wt.%): 35.69 SiO2, 0.22 TiO2, 21.98 Al2O3, 6.12 Sc2O3, 0.07 V2O3, 1.10 Fe2O3, 0.11 Y2O3, 1.55 La2O3, 4.05 Ce2O3, 0.31 Pr2O3, 1.53 Nd2O3, 0.40 Sm2O3, 0.11 EuO, 0.56 Gd2O3, 0.14 MnO, 3.56 FeO, 0.16 MgO, 19.16 CaO and 1.78 H2O(+)calc.; total 98.60. The cotype contains: 34.92 SiO2, 0.44 TiO2, 0.82 SnO2, 19.13 Al2O3, 4.79 Sc2O3, 1.96 Fe2O3, 2.55 La2O3, 7.39 Ce2O3, 0.48 Pr2O3, 0.67 Nd2O3, 0.12 EuO, 0.61 Gd2O3, 0.13 MnO, 5.97 FeO, 17.66 CaO and 1.73 H2O(+)calc.; total 99.37. The compositions correspond to the following empirical formulae: (Ca1.729Ce0.125La0.048Nd0.046Gd0.016Sm0.012Pr0.010Y0.005Eu2+0.003)Σ1.994[(Al2.182Sc0.449Fe3+0.070V3+0.005)Σ2.706(Fe2+0.251Mg0.020Mn0.010)Σ0.281Ti0.014]Σ3.001(Si3.006O11)O(OH) and (Ca1.644Ce0.235La0.082Nd0.021Gd0.018Pr0.015Eu2+0.004)Σ1.019[(Al1.958Sc0.362Fe3+0.128)Σ2.448(Fe2+0.434Mn0.009)Σ0.443(Ti0.029Sn0.029)Σ0.058]Σ2.949(Si3.033O11)O(OH), respectively, and to the ideal formula Ca2(Al2Sc)(Si2O7)(SiO4)O(OH). The crystal structure of the holotype was refined in the monoclinic system with an R1 index of 8.62%. The crystal-structure refinement indicates exclusively Si occupied T sites, Al occupied M1 and M2 sites, and a Ca occupied A1 site. The M3 site is filled predominantly by trivalent cations, mainly Sc3+, with divalent cations (mainly Fe2+) as minor occupants. The A2 site is filled mostly by Ca with minor amounts of rare earth elements (REE). The holotype heflikite crystallised from metasomatic fluids that infiltrated a contact between the granitic pegmatite and the surrounding rodingite-type calc-silicate rocks and serpentinites. The fluids that introduced Sc into the pegmatite could have been either hydrothermal or related to low-grade regional metamorphism that postdated the formation of the pegmatite. The cotype heflikite formed during the late-stage hydrothermal crystallisation of the Sc-enriched granitic pegmatite.