Gibbs energies of formation of zircon (ZrSiO4), thorite (ThSiO4), and phenacite (Be2SiO4)

International Nuclear Information System (INIS)

Schuiling, R.D.; Vergouwen, L.; Rijst, H. van der

1976-01-01

Zircon, thorite, and phenacite are very refractory compounds which do not yield to solution calorimetry. In In order to obtain approximate Gibbs energies of formation for these minerals, their reactions with a number of silica-undersaturated compounds (silicates or oxides) were studied. Conversely baddeleyite (ZrO 2 ), thorianite (ThO 2 ), and bromellite (BeO) were reacted with the appropriate silicates. As the Gibbs energies of reaction of the undersaturated compounds with SiO 2 are known, the experiments yield the following data: Δ G 298 , 1 /sub bar/ 0 = -459.02 +- 1.04 kcal for zircon, -489.67 +- 1.04 for thorite, and -480.20 +- 1.01 for phenacite

On the rutile alpha-PbO"2-type phase boundary of TiO"2

DEFF Research Database (Denmark)

Olsen, J.S.; Gerward, Leif; Jiang, Jianzhong

1999-01-01

The high-pressure, high-temperature phase quilibria of TiO"2 have been studied with special emphasis on the rutile and alpha-PbO"2-type phases. It is found that the phase boundary, when plotted in a pressure-temperature diagram, changes from having a negative to having a positive slope...... with increasing temperature at about 6GPa and 850^oC. For nanophase material, the phase boundary is shifted towards lower pressure. The room-temperature bulk moduli are 210(120)GPa, 258(8)GPa and 290(20)GPa for rutile, the alpha-PbO"2-type phase and the baddeleyite-type phase, respectively....

Paleomagnetism and geochronological studies on a 450 km long 2216 Ma dyke from the Dharwar craton, southern India

Science.gov (United States)

Nagaraju, E.; Parashuramulu, V.; Kumar, Anil; Srinivas Sarma, D.

2018-01-01

Paleomagnetic and geochronological studies were carried out on a ∼ 450 km long (from 17 sites) N-S striking Paleoproterozoic dyke swarm exposed along a natural crustal cross section of about 10 km (increasing from North to South) in the Dharwar Craton, to study the characteristics of paleomagnetism and geochronology in vertical dimension. U-Pb/Pb-Pb dating on baddeleyite gives a crystallisation age of 2216.0 ± 0.9 Ma for long dyke AKLD. Paleomagnetic data from this well dated ∼ 2216 Ma dyke swarm in Dharwar Craton are of excellent quality. High coercivity and high blocking temperature components are carried by single domain magnetite and show dual polarity remanence directions. Combined normal and reverse polarity remanences on AKLD and other N-S dykes define the most reliable paleomagnetic pole for ∼ 2216 Ma at latitude 36°S and longitude 312°E (A95 = 7°). Though paleomagnetic data is unavailable on other N-S dykes below the Cuddapah basin, high precision geochronology suggest that they are of similar age within errors. Though there is a variation in the crustal depth of Dharwar craton from north to south, consistent Pb-Pb/U-Pb baddeleyite geochronology and paleomagnetic studies along the AKLD established its continuity and preservation along its entire strike length. The virtual geomagnetic poles of these sites confirm a stable remanence and are almost identical to the previously reported paleomagnetic pole and also supported by positive reversal test. Positive paleomagnetic reversal test on these dykes signify that the remanent magnetization is primary and formed during initial cooling of the intrusions. Updated apparent polar wander path of Dharwar craton indicates relatively low drift rate during 2.21-2.08 Ga interval. Magnetogranulometry and SEM studies show that remanent magnetization in this dyke was carried by single domain magnetite residing within silicate minerals.

Local environment of zirconium in nuclear gels studied by XAS

International Nuclear Information System (INIS)

Pelegrin, E.; Ildefonse, Ph.; Calas, G.; Ricol, St.; Flank, A.M.

1997-01-01

During lixiviation experiments, nuclear gels are formed and heavy metals are retained. In order to understand this retardation mechanisms, we performed an analysis of the local environment of Zr in parent glasses and derived alteration gels both at the Zr-L II,III , and Zr-K edges. Calibration of the method was conducted through the analysis of model compounds with known coordination number (CN): catapleite Na 2 ZrSi 3 O 9 ,2H 2 O (CN=6), baddeleyite ZrO 2 (CN=7) and zircon SiZrO 4 (CN=8). Nuclear glasses (R7T7, and a simplified nuclear glass V 1) and gels obtained at 90 deg C, with leaching times from 7 to 12 months and with solution renewal. were also investigated (GR7T7R and GV1). Zr-L II,III XANES spectra evidenced that zirconium is 6-fold coordinated in R7T7 and V1 nuclear glasses. For GR7T7R and GV1 gels, Zr local environment is significantly changed, and a mixture of CN (6 and 7J has been evidenced. Quantitative structural results were derived from EXAFS analysis at Zr-K edge. In parent glasses, derived Zr-O distance is 2.10±0.01 10 -10 m, and is in the range Zr-O distances for octahedral coordination in model compounds. In both gels studied, Zr-O distances increase significantly up to 2.15 ±0.01 10 -10 m. This distance is close to that known in baddeleyite (2,158 10 -10 m). A better understanding of the Zr retention mechanism has to be made by studying the second neighbors contributions. (authors)

Bixbyite-type phases in the system Ta-Zr-O-N

Energy Technology Data Exchange (ETDEWEB)

Luedtke, Tobias; Orthmann, Steven; Lerch, Martin [Technische Univ. Berlin (Germany). Inst. fuer Chemie

2017-06-01

Phase-pure tantalum/zirconium oxide nitrides and nitrides were synthesized by the ammonolysis of amorphous oxide precursors. The nitrogen-rich oxide nitrides with variable anion composition and the nitride TaZrN3 crystallize in the cubic bixbyite-type structure (space group Ia3). The nitrogen content of these compounds has a significant influence on the cell parameters, the atomic positions, and the optical band gap. The results extend the already well-studied Ta-Zr-O-N system by new oxide nitrides in addition to the already known baddeleyite- and anosovite-type phases. TaZrN{sub 3} can be considered as a thermodynamically stable ternary variant of metastable Ta{sub 2}N{sub 3}.

Purification of zirconium concentrates

International Nuclear Information System (INIS)

Brown, A.E.P.

1976-01-01

A commercial grade ZrO 2 and an ammonium uranate (yellow cake) are obtained from the caldasito ore processing. This ore is found in the Pocos de Caldas Plateau, State of Minas Gerais, Brazil. Caldasito is an uranigerous zirconium ore, a mixture of zircon and baddeleyite and contains 60% ZrO 2 and 0,3% U 3 O 8 . The chemical opening of the ore was made by alkaline fusion with NaOH at controlled temperature. The zirconium-uranium separation took place by a continuous liquid-liquid extraction in TBP-varsol-HNO 3 -H 2 O system. The raffinate containing zirconium + impurities (aluminium, iron and titanium) was purified by an ion exchange operation using a strong cationic resin [pt

Assessment of exposures to ionizing radiation in industries and activities implementing raw materials which naturally contain radionuclides and which are not used because of their radioactive properties. Assessment of the 25. of May 2005 Order related to these activities

International Nuclear Information System (INIS)

2009-12-01

This report proposes an assessment of the exposure of workers and of population to reinforced natural radioactivity associated to some particular professional activities, i.e. activities where raw materials which are used, are naturally radioactive, for example: coal combustion in thermal power plants, ore processing (tin, aluminium, copper, titanium, niobium, bismuth, thorium), production of refractory ceramics, production or use of thorium compounds, zircon or baddeleyite production, and so on. After a presentation of the French national regulation, the report gives an assessment of its application through different measurements or surveys, notably dosimetry performed on workers or population exposure measurements, or some waste management activities. It discusses the evolution opportunities of this regulation, either in the French framework or at the European level

Time resolution of geologic events on the Keweenaw Peninsula and implications for development of the Midcontinent Rift system

International Nuclear Information System (INIS)

Davis, D.W.; Paces, J.B.

1990-01-01

Three flood-type lava flows from the Keweenaw Peninsula in upper Michigan have been precisely dated, using U-Pb analyses of zircon and baddeleyite. Zircons were extracted from pegmatoid segregations within two basaltic flows. Ages from the Copper City Flow, near the base of the Portage Lake Volcanics, and the Greenstone Flow, near the top, are 1096.2±1.8 Ma and 1094.0±1.5 Ma, respectively (95% confidence errors). U-Pb analyses of baddeleyite from these samples are in general agreement with the zircon results although some fractions appear slightly older, possibly due to 222 Rn loss. The age of an andesite flow from the Lake Shore Traps, 1000 m above the Portage Lake Volcanics and within the Copper Harbour Conglomerate, is 1087.2±1.6 Ma from analyses of zircon. This gives an age for sedimentation within the Copper Harbor Conglomerate. These ages, along with stratigraphic data, indicate a subsidence rate of 1.3 -0.6 +1.8 mm/y during eruption of the Portage Lake Volcanics and 0.2±0.1 mm/y (1σ errors) for the transitional period from flood basalt eruption to clastic sedimentation. Magma eruption rates were at least 0.02-0.05 km 3 /y during emplacement of the Portage Lake Volcanics. Rates as high as 0.2-0.6 km 3 /y are inferred from regional stratigraphic data and currently available precise dates from throughout the Lake Superior basin. These values are comparable to the high rates of magma production estimated for Phanerozoic continental flood basalt provinces. Analyses of three detrital zircon grains from a sandstone at the base of the Copper Harbor Conglomerate give ages from 1101 to 1106 Ma. A fraction consisting of 29 detrital zircon grains has an age of 1104±2 Ma indicating that sediments within the Copper Harbor Conglomerate were probably derived almost entirely from lower Keweenawan rocks. (orig./WB)

Zirconium

Science.gov (United States)

Bedinger, G.M.

2013-01-01

Zirconium is the 20th most abundant element in the Earth’s crust. It occurs in a variety of rock types and geologic environments but most often in igneous rocks in the form of zircon (ZrSiO4). Zircon is recovered as a coproduct of the mining and processing of heavy mineral sands for the titanium minerals ilmenite and rutile. The sands are formed by the weathering and erosion of rock containing zircon and titanium heavy minerals and their subsequent concentration in sedimentary systems, particularly in coastal environments. A small quantity of zirconium, less than 10 kt/a (11,000 stpy), compared with total world production of 1.4 Mt (1.5 million st) in 2012, was derived from the mineral baddeleyite (ZrO2), produced from a single source in Kovdor, Russia.

REE-substituted Ca-free zirconolites

International Nuclear Information System (INIS)

Stefanovsky, S.V.; Chernyavskaya, N.E.; Ochkin, A.V.; Yudintsev, S.V.

2002-01-01

Previously we found zirconolite with composition (Gd 0.90 La 0.10 )(Zr 0.91 Ce 0.13 ) (Ti 1.20 Al 0.69 )O 7 in one of the ceramics designed for immobilization of REE-actinide HLW fraction. In this work we studied REEZrTiAlO 7 zirconolites with REE = La, Ce, Pr, Nd, Sm, Gd, Tb, and Y. To obtain the samples, the oxide mixtures were milled, compacted into pellets at 200 MPa and sintered at 1450 deg C or melted at 1550 deg C in air. To convert Ce (IV) to Ce (III), one test was performed in reducing conditions (carbon was introduced in batches). The ceramics were examined by X-ray diffraction (XRD) and by scanning and transmission electron microscopy (SEM, TEM). The XRD data revealed that the La-, Ce-, Pr-, and Nd-bearing samples were not single-phase ceramics. The La-bearing sample was composed of a major perovskite-type phase and a minor baddeleyite. The Ce-bearing samples consisted of major pyrochlore, cerianite-zirconia based cubic solid solution as a second in abundance phase, and minor zirconolite. The Pr-bearing ceramic contained major baddeleyite and a perovskite-type phase, and minor pyrochlore. In the Nd-, Sm-, Gd-, Tb-, and Y-bearing samples, zirconolite was predominant. Rare grains of REE-stabilized zirconia (fianite) were found by SEM in the Nd-, Sm, and Y-bearing ceramics. The Gd- and Tb-bearing samples were single phase. The average zirconolite formulas were Sm 1.06 Zr 1.07 Ti 1.00 Al 0.86 O 7 , Gd 1.01 Zr 1.05 Ti 0.98 Al 0.95 O 7 , Tb 0.93 Zr 1.09 Ti 1.08 Al 0.85 O 7 , and Y 1.05 Zr 1.03 Ti 1.03 Al 0.87 O 7 , hence, close to the specified zirconolite formula within the experimental error. XRD patterns of the Tb- and Y-bearing zirconolites are typical of zirconolite-2M variety. XRD patterns of the Nd-, Sm-, and Gd-bearing zirconolites differ from patterns typical of 2M, 3T, and 3O varieties known from reference data. The TEM study revealed a probable tetragonal symmetry of the zirconolite lattice on electron diffraction pattern

Partial pressures of oxygen, phosphorus and fluorine in some lunar lavas

Science.gov (United States)

Nash, W. P.; Hausel, W. D.

1973-01-01

Lunar sample 14310 is a feldspar-rich basalt which shows no evidence of shock deformation or recrystallization. Pyroxenes include Mg-rich orthopyroxene, pigeonite and augite; pyroxferroite occurs in the interstitial residuum. Plagioclase feldspars are zoned from An(96) to An(67), and variations in feldspar compositions do not necessarily indicate loss of Na during eruption of the lava. Opaque phases include ilmenite, ulvospinel, metallic iron, troilite, and schreibersite. Both whitlockite and apatite are present, and the interstitial residua contain baddeleyite, tranquillityite and barium-rich sanidine. Theoretical calculations provide estimates of partial pressures of oxygen, phosphorus, and fluorine in lunar magmas. In general, partial pressures of oxygen are restricted by the limiting assemblages of iron-wuestite and ilmenite-iron-rutile; phosphorus partial pressures are higher in lunar magmas than in terrestrial lavas. The occurrence of whitlockite indicates significantly lower fugacities of fluorine in lunar magmas than in terrestrial magmas.

U-Pb zircon geochronology and evolution of some Adirondack meta-igneous rocks

Science.gov (United States)

Mclelland, J. M.

1988-01-01

An update was presented of the recent U-Pb isotope geochronology and models for evolution of some of the meta-igneous rocks of the Adirondacks, New York. Uranium-lead zircon data from charnockites and mangerites and on baddeleyite from anorthosite suggest that the emplacement of these rocks into a stable crust took place in the range 1160 to 1130 Ma. Granulite facies metamorphism was approximately 1050 Ma as indicated by metamorphic zircon and sphene ages of the anorthosite and by development of magmatitic alaskitic gneiss. The concentric isotherms that are observed in this area are due to later doming. However, an older contact metamorphic aureole associated with anorthosite intrusion is observed where wollastonite develops in metacarbonates. Zenoliths found in the anorthosite indicate a metamorphic event prior to anorthosite emplacement. The most probable mechanism for anorthosite genesis is thought to be ponding of gabbroic magmas at the Moho. The emplacement of the anorogenic anorthosite-mangerite-charnockite suite was apparently bracketed by compressional orogenies.

U-Pb geochronology documents out-of-sequence emplacement of ultramafic layers in the Bushveld Igneous Complex of South Africa.

Science.gov (United States)

Mungall, James E; Kamo, Sandra L; McQuade, Stewart

2016-11-14

Layered intrusions represent part of the plumbing systems that deliver vast quantities of magma through the Earth's crust during the formation of large igneous provinces, which disrupt global ecosystems and host most of the Earth's endowment of Pt, Ni and Cr deposits. The Rustenburg Layered Suite of the enormous Bushveld Igneous Complex of South Africa has been presumed to have formed by deposition of crystals at the floor of a subterranean sea of magma several km deep and hundreds of km wide called a magma chamber. Here we show, using U-Pb isotopic dating of zircon and baddeleyite, that individual chromitite layers of the Rustenburg Layered Suite formed within a stack of discrete sheet-like intrusions emplaced and solidified as separate bodies beneath older layers. Our U-Pb ages and modelling necessitate reassessment of the genesis of layered intrusions and their ore deposits, and challenge even the venerable concept of the magma chamber itself.

The heavy-minerals plant at Palabora Mining Company

International Nuclear Information System (INIS)

Van der Spuy, R.C.M.

1982-01-01

The heavy-minerals plant at the Palabora Mining Company treats 25 to 30 kt of new feed daily. The U 3 O 8 value of the ore averages approximately 40 p.p.m. The circuit consists of four stages of upgrading on 68 Reichert cones, followed by a jig and 30 table decks. The paper describes how feed-distribution problems have been overcome and the methods used for monitoring and controlling the cone performance. The adaptation of a standard jig for the recovery of fine minerals is discussed, and a method of table agglomeration, for the recovery of coarse refractory copper sulphide is described. The tables consist of polyurethane-covered fibreglass decks, and their operation is controlled according to measurements of the uranothorianite content of the concentrates and middlings by means of a nuclear scintillation counter. The upgrading ratio of the uranium mineral by gravity concentration is 1000:1, baddeleyite (ZrO 2 ) being recovered as a byproduct [af

Rift magmatism on the Eurasia basin margin: U–Pb baddeleyite ages of alkaline dyke swarms in North Greenland

DEFF Research Database (Denmark)

Thórarinsson, Sigurjón B.; Söderlund, Ulf; Døssing, Arne

2015-01-01

The opening of the Arctic Ocean involved multiple stages of continental rifting and intrusion of extensive dyke swarms. To trace tectonomagmatic processes of the High Arctic, we present the first U–Pb ages for alkaline dyke swarms of North Greenland. Concordia ages of 80.8 ± 0.6 and 82.1 ± 1.5 Ma...... indicate that north–south and east–west dykes are coeval. The north–south dykes reflect initial east–west rifting that led to break-up along the Gakkel Ridge and formation of the Eurasia Basin. The east–west dykes reflect local variations in the stress field associated with reactivated Palaeozoic faults...

Kampelite, Ba3Mg1.5Sc4(PO4)6(OH)3·4H2O, a new very complex Ba-Sc phosphate mineral from the Kovdor phoscorite-carbonatite complex (Kola Peninsula, Russia)

Science.gov (United States)

Yakovenchuk, Victor N.; Ivanyuk, Gregory Yu.; Pakhomovsky, Yakov A.; Panikorovskii, Taras L.; Britvin, Sergei N.; Krivovichev, Sergey V.; Shilovskikh, Vladimir V.; Bocharov, Vladimir N.

2018-02-01

Kampelite, Ba3Mg1.5Sc4(PO4)6(OH)3·4H2O, is a new Ba-Sc phosphate from the Kovdor phoscorite-carbonatite complex (Kola Peninsula, Russia). It is orthorhombic, Pnma, a = 11.256(1), b = 8.512(1), c = 27.707(4) Å, V = 2654.6(3) Å3 and Z = 4 (from powder diffraction data) or a = 11.2261(9), b = 8.5039(6), c = 27.699(2) Å, V = 2644.3(3) Å3 (from single-crystal diffraction data). The mineral was found in a void within the calcite-magnetite phoscorite (enriched in hydroxylapatite and Sc-rich baddeleyite) inside the axial zone of the Kovdor phoscorite-carbonatite pipe. Kampelite forms radiated aggregates (up to 1.5 mm in diameter) of platy crystals grown on the surfaces of crystals of quintinite-2 H in close association with pyrite, bobierrite and quintinite-3 R. Kampelite is colourless, with a pearly lustre and a white streak. The cleavage is perfect on {001}, the fracture is smooth. Mohs hardness is about 1. In transmitted light, the mineral is colourless without pleochroism or dispersion. Kampelite is biaxial + (pseudouniaxial), α ≈ β = 1.607(2), γ = 1.612(2) (589 nm), and 2 V calc = 0°. The calculated and measured densities are 3.28 and 3.07(3) g·cm-3, respectively. The mean chemical composition determined by electron microprobe is: MgO 4.79, Al2O3 0.45, P2O5 31.66, K2O 0.34, Sc2O3 16.17, Mn2O3 1.62, Fe2O3 1.38, SrO 3.44, and BaO 29.81 wt%. The H2O content estimated from the crystal-structure refinement is 7.12 wt%, giving a total of 96.51 wt%. The empirical formula calculated on the basis of P = 6 apfu (atoms per formula unit) is (Ba2.62Sr0.45K0.10Ca0.06)Σ3.23Mg1.60Mn0.28(Sc3.15Fe3+ 0.23Al0.12)Σ3.50(PO4)6(OH)2.61·4.01H2O. The simplified formula is Ba3Mg1.5Sc4(PO4)6(OH)3·4H2O. The mineral easily dissolves in 10% cold HCl. The strongest X-ray powder-diffraction lines [listed as d in Å ( I) ( hkl)] are as follows: 15.80(100)(001), 13.86(45)(002), 3.184(18)(223), 3.129(19)(026), 2.756(16)(402), 2.688(24)(10 10). The crystal structure of kampelite was

U-Pb geochronology and paleomagnetism of the Neoproterozoic St Simeon dolerite dykes, Quebec: an eastern Laurentian perspective of Ediacaran Rodinia breakup

Science.gov (United States)

Pisarevsky, Sergei; Murphy, Brendan; Hamilton, Mike; Söderlund, Ulf; Hodych, Joseph

2013-04-01

The St Simeon (SS) mafic dykes (150 km NE of Quebec City) are now dated at 548 ± 1 Ma (U-Pb; baddeleyite). This age is similar to a published LA-ICPMS zircon age of 550 ± 7 Ma for the Mt. St-Anselme (MS) basalts, which supports previous inferences of (i) a genetic relationship between them, (ii) the pene-contemporaneity of OIB-type mafic magmatism in East Laurentia and (iii) the existence of two late Ediacaran plumes that attended the final breakup of Rodinia and opening of the Iapetus Ocean and Tornquist Sea. Both the SS dykes and the MS basalts were sampled for paleomagnetic study. The paleomagnetic pole for SS is similar to the previously published pole for coeval basalts (Skinner Cove, SC) from Newfoundland. Unlike SC, the St Simeon pole represents rocks which are unambiguously coherent tectonically with the Laurentian Craton. This new pole is also coeval with high quality poles from the Winter Coast (Baltica) and provides paleomagnetic constraints on the history of the final breakup of Rodinia and opening of Eastern Iapetus and Tornquist Sea.

Approach of automatic 3D geological mapping: the case of the Kovdor phoscorite-carbonatite complex, NW Russia.

Science.gov (United States)

Kalashnikov, A O; Ivanyuk, G Yu; Mikhailova, J A; Sokharev, V A

2017-07-31

We have developed an approach for automatic 3D geological mapping based on conversion of chemical composition of rocks to mineral composition by logical computation. It allows to calculate mineral composition based on bulk rock chemistry, interpolate the mineral composition in the same way as chemical composition, and, finally, build a 3D geological model. The approach was developed for the Kovdor phoscorite-carbonatite complex containing the Kovdor baddeleyite-apatite-magnetite deposit. We used 4 bulk rock chemistry analyses - Fe magn , P 2 O 5 , CO 2 and SiO 2 . We used four techniques for prediction of rock types - calculation of normative mineral compositions (norms), multiple regression, artificial neural network and developed by logical evaluation. The two latter became the best. As a result, we distinguished 14 types of phoscorites (forsterite-apatite-magnetite-carbonate rock), carbonatite and host rocks. The results show good convergence with our petrographical studies of the deposit, and recent manually built maps. The proposed approach can be used as a tool of a deposit genesis reconstruction and preliminary geometallurgical modelling.

Metal dioxides as analogue of SiO2 under strong compression studied by synchrotron XRD and simulations

Science.gov (United States)

Liu, H.; Liu, L. L.

2017-12-01

The phase transition sequence of SiO2 inducing by high pressure was theoretically predicted as coordination number (CN=6) structures (rutile, pyrite), CN=8 (Pnma) and CN=9 (P-62m) structures, but only the phases up to pyrite structure in SiO2 were observed experimentally up to now. The CN8 phase and CN9 phases of SiO2 were predicted to be stable at least 650 GPa, which is challenging to achieve in the static DAC experiment at present. In other metal dioxide systems, such as TiO2, the ambient rutile and anatase phases first transform to pyrite (CN6), then to the baddeleyite (CN7) phase, to a Pnma (CN8) phase and P-62m(CN9) phase. In this report, under strong compression at room temperature, several metal dioxides were studied experimentally and theoretically, to verify whether this theoretical predicted trend is common transition path under strong compression. This work was supported by Natural Science Foundation of China (11374075), Heilongjiang Province Science Fund for Distinguished Young Scholars (JC201005), Longjiang Scholar, the Fundamental Research Funds for the Central Universities (HIT. BRET1.2010002, HIT. IBRSEM.A.201403).

The structure of ZrO2 phases and deviltrification processes in a Ca-Zr-Si-O-based glass ceramic: a combined a-XRD and XAS study

International Nuclear Information System (INIS)

Meneghini, C.; Mobilio, S.

2004-01-01

The structure of Zr atomic environment in a CaO-ZrO 2 -Si 2 glass ceramic as a function of thermal treatments has been studied, combining X-ray absorption spectroscopy (XAS), X-ray diffraction (XRD) and anomalous XRD (a-XRD) techniques. The analysis of XRD patterns demonstrates that the devitrification process proceeds through the partial segregation of Zr-depleted phases (wollastonite-like) and Zr-rich phases (Zr oxides). The XAS and a-XRD measurements at the Zr K-edge have been exploited in order to obtain a closer insight into the atomic structure around the Zr atoms. In the as-quenched glass the Zr atom is sixfold coordinated to O atoms in an amorphous environment rich in Ca and Si. Thermal treatment firstly (T=1273-1323 K) causes partial segragation of Zr in the form of an oxide with a tetragonal zirconia (t-ZrO 2 ) crystalline structure. Raising the temperature (T=1373 K) causes the formation of ZrO 2 crystallites in the monoclinic crystallographic phase (baddeleyite, m-ZrO 2 ). Analysis of the XAS data shows that a considerable amount of Zr remains in an amorphous calcium silicate phase. (orig.)

Study on fused/cast AZS refractories for deployment in vitrification of radioactive waste effluents

Science.gov (United States)

Sengupta, Pranesh; Mishra, R. K.; Soudamini, N.; Sen, D.; Mazumder, S.; Kaushik, C. P.; Ajithkumar, T. G.; Banerjee, K.

2015-12-01

'Fused/cast Al2O3-ZrO2-SiO2 (FC-AZS)' is being considered as 'glass contact refractory' within ceramic melters, to be used for nuclear waste immobilization. Microstructural analyses reveal random distributions of baddeleyite (ZrO2) within aluminosilicate (Al2SiO5) matrix. 27Al and 29Si NMR data suggest that within aluminosilicate matrix Al occurs in both 4- and 6-fold co-ordinations whereas Si prefers a 4-fold environment. Polydispersity of pores has been studied with small-angle neutron scattering (SANS) technique. Corrosion rates of FC-AZS within 6 M HNO3, simulated wastes (500 h exposure), and borosilicate melt (975 °C, 800 h exposure) are found to be 0.38 × 103 μmy-1, 0.13 × 103 μmy-1 and 4.75 × 103 μmy-1 respectively. A comparison of chemical interaction data clearly suggests that FC-AZS exhibits better chemical durability than AZC refractory (Al2O3-ZrO2-Cr2O3, also used for similar purpose). Thermal cycling studies indicate that FC-AZS retains structural integrity (including compressive strength and density) even up to 20 cycles.

Magnetic studies and U Pb geochronology of the Uruguayan dyke swarm, Rio de la Plata craton, Uruguay: paleomagnetic and economic implications

Science.gov (United States)

Halls, Henry C.; Campal, Nestor; Davis, Don W.; Bossi, Jorge

2001-09-01

A U-Pb age on baddeleyite of 1790±5 Ma has been obtained from a single dyke of the Uruguayan tholeiitic dyke swarm from the Rio de la Plata craton. Palaeomagnetic results from this and 10 other dykes yield two components, one (A) has the following paleomagnetic parameters: declination=12°, inclination=-16°, α95=7°, latitude of paleopole=61°, longitude=-31°, dp=4°, dm=7°, paleolatitude=-8°, whereas another (B), about 20° steeper, has a direction closer to the present Earth's field direction in Uruguay. Neither magnetisation is considered primary, although the A component may represent a composite between B and a primary component. A field test for the primary nature of the remanences was inconclusive, and no primary pole positions of similar age from other South American cratons are available for comparison. The magnetic results demonstrate that darker-coloured andesite dykes that are sought for facing and monument stone (as 'black granite') can be easily differentiated from more andesi-basaltic, lighter coloured, less valuable dykes of the same swarm, using aeromagnetic data. The results suggest that a high resolution airborne magnetic survey could constitute an important exploration tool for the Uruguayan 'black granite' industry.

Antimony (V) oxide adsorbed on a silica-zirconia mixed oxide obtained by the sol-gel processing method: preparation and acid properties

International Nuclear Information System (INIS)

Zaitseva, Galina; Gushikem, Yoshitaka

2002-01-01

The preparation, degree of dispersion, thermal stability and Lewis and Broensted acidity of antimony (V) oxide adsorbed on Si O 2 /Zr O 2 mixed oxide, previously prepared by the sol-gel processing method, are described herein. The samples Si O 2 /Zr O 2 /Sb 2 O 5 , with compositions (in wt %): (a) Zr= 8.1 and Sb= 6.3; (b) Zr= 14.9 and Sb= 11.4, were prepared. Scanning electron microscopy images connected to a X-ray energy dispersive spectrometer showed that both metals, Zr and Sb, were highly dispersed in the matrices. The X-ray diffraction patterns of Si O 2 /Zr O 2 /Sb 2 O 5 heated at different temperatures showed that, up to 1023 K, the matrix was amorphous. At 1273 K a crystalline phase of Zr O 2 (baddeleyite) was observed and raising the temperature to 1573 K, crystalline phases of Si O 2 (cristobalite) and presumably of Zr O 2 /Sb 2 O 5 were observed. Using pyridine as a molecular probe, Broensted acid sites on the Si O 2 /Zr O 2 /Sb 2 O 5 matrix, heat treated up to 523 K, were shown to be very stable. (author)

Natural radioactivity concentration in raw materials used for manufacturing refractory products

International Nuclear Information System (INIS)

Fathivand, A. A.; Amidi, J.; Hafezi, S.

2007-01-01

Some Particular areas contain natural radionuclide at levels much higher than those usually present in earth's crust. The radiological impact of the use of zirconium ore in zirconium industry is due to internal exposure of the lung by alpha particles and external exposure of the body by the gamma rays. The result of gamma spectrometry measurement of the concentrations of the natural radionuclide in zirconium industry is described. Materials and Methods: Gamma spectrometry system with a shielded high pure germanium (HPGe) detector connected to multi channel analyzer (MCA) was used to determine concentrations of natural radionuclide in about 45 samples of imported zirconium minerals, tiles, stone ware and waste sludge's of Iranian ceramic industry. Results: The 238 U concentration in the samples, ranging from 3000 to 10000 Bq Kg -1 , is higher than the concentration of both 232 Th (500-1800 Bq Kg -1 ), and 40 K (50-800 Bq Kg -1 ). The measured specific activities in the mineral showed that specific activity of baddeleyite is higher than that of zircon. The results of ceramic tiles show that the tiles usually contain small amount of zirconium compound. Conclusion: Due to relatively high concentration level of uranium in imported zirconium samples, specific regulations is necessary for zirconium compound used in ceramic industry

Crystalline phase, microstructure, and aqueous stability of zirconolite-barium borosilicate glass-ceramics for immobilization of simulated sulfate bearing high-level liquid waste

Science.gov (United States)

Wu, Lang; Xiao, Jizong; Wang, Xin; Teng, Yuancheng; Li, Yuxiang; Liao, Qilong

2018-01-01

The crystalline phase, microstructure, and aqueous stability of zirconolite-barium borosilicate glass-ceramics with different content (0-30 wt %) of simulated sulfate bearing high-level liquid waste (HLLW) were evaluated. The sulfate phase segregation in vitrification process was also investigated. The results show that the glass-ceramics with 0-20 wt% of HLLW possess mainly zirconolite phase along with a small amount baddeleyite phase. The amount of perovskite crystals increases while the amount of zirconolite crystals decreases when the HLLW content increases from 20 to 30 wt%. For the samples with 20-30 wt% HLLW, yellow phase was observed during the vitrification process and it disappeared after melting at 1150 °C for 2 h. The viscosity of the sample with 16 wt% HLLW (HLLW-16) is about 27 dPa·s at 1150 °C. The addition of a certain amount (≤20 wt %) of HLLW has no significant change on the aqueous stability of glass-ceramic waste forms. After 28 days, the 90 °C PCT-type normalized leaching rates of Na, B, Si, and La of the sample HLLW-16 are 7.23 × 10-3, 1.57 × 10-3, 8.06 × 10-4, and 1.23 × 10-4 g·m-2·d-1, respectively.

Antimony (V Oxide Adsorbed on a Silica-Zirconia Mixed Oxide Obtained by the Sol-Gel Processing Method: Preparation and Acid Properties

Directory of Open Access Journals (Sweden)

Zaitseva Galina

2002-01-01

Full Text Available The preparation, degree of dispersion, thermal stability and Lewis and Brphinsted acidity of antimony (V oxide adsorbed on SiO2/ZrO2 mixed oxide, previously prepared by the sol-gel processing method, are described herein. The samples SiO2/ZrO2/Sb2O5, with compositions (in wt %: (a Zr= 8.1 and Sb= 6.3; (b Zr= 14.9 and Sb= 11.4, were prepared. Scanning electron microscopy images connected to a X-ray energy dispersive spectrometer showed that both metals, Zr and Sb, were highly dispersed in the matrices. The X-ray diffraction patterns of SiO2/ZrO2/Sb2O5 heated at different temperatures showed that, up to 1023 K, the matrix was amorphous. At 1273 K a crystalline phase of ZrO2 (baddeleyite was observed and raising the temperature to 1573 K, crystalline phases of SiO2 (cristobalite and presumably of ZrO2/Sb2O5 were observed. Using pyridine as a molecular probe, Brphinsted acid sites on the SiO2/ZrO2/Sb2O5 matrix, heat treated up to 523 K, were shown to be very stable.

Pressure effect on the Raman and photoluminescence spectra of Eu3+-doped Na2Ti6O13 nanorods

Science.gov (United States)

Zeng, Q. G.; Yang, G. T.; Chen, F.; Luo, J. Y.; Zhang, Z. M.; Leung, C. W.; Ding, Z. J.; Sheng, Y. Q.

2013-12-01

Eu3+-doped Na2Ti6O13 (Na2Ti6O13:Eu) nanorods with diameters of 30 nm and lengths 400 nm were synthesized by hydrothermal and heat treatment methods. Raman spectra at ambient conditions indicated a pure monoclinic phase (space group C2/m) of the nanorods. The relations between structural and optical properties of Na2Ti6O13:Eu nanorods under high pressures were obtained by photoluminescence and Raman spectra. Two structural transition points at 1.39 and 15.48 GPa were observed when the samples were pressurized. The first transition point was attributed to the crystalline structural distortion. The later transition point was the result of pressure-induced amorphization, and the high-density amorphous (HDA) phase formed after 15.48 GPa was structurally related to the monoclinic baddeleyite structured TiO2 (P21/c). However, the site symmetry of the local environment around the Eu3+ ions in Na2Ti6O13 increased with the rising pressure. These above results indicate the occurrence of short-range order for the local asymmetry around the Eu3+ ions and long-range disorder for the crystalline structure of Na2Ti6O13:Eu nanorods by applying pressure. After releasing the pressure from 22.74 GPa, the HDA phase is transformed to low-density amorphous form, which is attributed to be structurally related to the α-PbO2-type TiO2.

Extreme biomimetic approach for synthesis of nanocrystalline chitin-(Ti,Zr)O2 multiphase composites

International Nuclear Information System (INIS)

Wysokowski, Marcin; Motylenko, Mykhaylo; Rafaja, David; Koltsov, Iwona; Stöcker, Hartmut; Szalaty, Tadeusz J.; Bazhenov, Vasilii V.; Stelling, Allison L.; Beyer, Jan; Heitmann, Johannes; Jesionowski, Teofil; Petovic, Slavica; Đurović, Mirko; Ehrlich, Hermann

2017-01-01

This work presents an extreme biomimetics route for the modification of the surface of fibre-based scaffolds of poriferan origin by the creation of novel nanostructured multiphase biocomposites. The exceptional thermal stability of the nanostructured sponge chitin allowed for the formation of a novel nanocrystalline chitin-(Ti,Zr)O 2 composite with a well-defined nanoscale structure under hydrothermal conditions (160 °C). Using a combination of experimental techniques, including X-ray diffraction, scanning electron microscopy, high resolution transmission electron microscopy, EDX mapping and near-edge electron loss spectroscopy (ELNES) in TEM and thermogravimetry/differential scanning calorimetry coupled with mass spectrometry; we showed that this bioorganic scaffold facilitates selective crystallization of TiO 2 , predominantly in form of anatase, over the monoclinic zirconium dioxide (baddeleyite). The control of the crystal morphology through the chitin templates is also demonstrated. Obtained samples were characterized in terms of their photoluminescent properties and photocatalytic performance. These data confirm the high potential of the extreme biomimetics approach for developing a new generation of multiphase biopolymer-based nanostructured materials. - Highlights: • Extreme biomimetically prepared chitin-(Ti,Zr)O 2 and (Ti,Zr)O 2 composites. • Chitin-(Ti,Zr)O 2 composite contains anatase as the most inorganic component. • The mean crystallite size is (31.7 ± 0.3) nm for chitin-(Ti,Zr)O 2 composite. • The mean crystallite size is (2.4 ± 0.5) nm for (Ti,Zr)O 2 composite. • (Ti,Zr)O 2 composite is 2 times more effective photocatalyst than chitin-(Ti,Zr)O 2 .

Study on fused/cast AZS refractories for deployment in vitrification of radioactive waste effluents

Energy Technology Data Exchange (ETDEWEB)

Sengupta, Pranesh, E-mail: praneshsengupta@gmail.com [Materials Science Division, Bhabha Atomic Research Centre, Mumbai 400 085 (India); Mishra, R.K.; Soudamini, N. [Waste Management Division, Bhabha Atomic Research Centre, Mumbai 400 085 (India); Sen, D.; Mazumder, S. [Solid State Physics Division, Bhabha Atomic Research Centre, Mumbai 400 085 (India); Kaushik, C.P. [Waste Management Division, Bhabha Atomic Research Centre, Mumbai 400 085 (India); Ajithkumar, T.G. [Central NMR Facility, National Chemical Laboratory, Pune 411 008 (India); Banerjee, K. [Nuclear Recycle Group, Mumbai 400 085 (India)

2015-12-15

‘Fused/cast Al{sub 2}O{sub 3}–ZrO{sub 2}–SiO{sub 2} (FC-AZS)’ is being considered as ‘glass contact refractory’ within ceramic melters, to be used for nuclear waste immobilization. Microstructural analyses reveal random distributions of baddeleyite (ZrO{sub 2}) within aluminosilicate (Al{sub 2}SiO{sub 5}) matrix. {sup 27}Al and {sup 29}Si NMR data suggest that within aluminosilicate matrix Al occurs in both 4- and 6-fold co-ordinations whereas Si prefers a 4-fold environment. Polydispersity of pores has been studied with small-angle neutron scattering (SANS) technique. Corrosion rates of FC-AZS within 6 M HNO{sub 3}, simulated wastes (500 h exposure), and borosilicate melt (975 °C, 800 h exposure) are found to be 0.38 × 10{sup 3} μmy{sup −1}, 0.13 × 10{sup 3} μmy{sup −1} and 4.75 × 10{sup 3} μmy{sup −1} respectively. A comparison of chemical interaction data clearly suggests that FC-AZS exhibits better chemical durability than AZC refractory (Al{sub 2}O{sub 3}–ZrO{sub 2}–Cr{sub 2}O{sub 3}, also used for similar purpose). Thermal cycling studies indicate that FC-AZS retains structural integrity (including compressive strength and density) even up to 20 cycles. - Highlights: • Vitrification of nuclear waste using AZS refractory within ceramic melter. • Microstructure of AZS refractory. • Interaction of AZS with simulated high level waste and glass.

Extreme biomimetic approach for synthesis of nanocrystalline chitin-(Ti,Zr)O{sub 2} multiphase composites

Energy Technology Data Exchange (ETDEWEB)

Wysokowski, Marcin, E-mail: Marcin.Wysokowski@put.poznan.pl [Poznan University of Technology, Faculty of Chemical Technology, Institute of Chemical Technology and Engineering, Berdychowo 4, 60965, Poznan (Poland); Motylenko, Mykhaylo; Rafaja, David [TU Bergakademie Freiberg, Institute of Materials Science, Gustav-Zeuner-Str. 5, 09596, Freiberg (Germany); Koltsov, Iwona [Laboratory of Nanostructures, Institute of High Pressure Physics of The Polish Academy of Sciences, Sokołowska 29/37, 01-142, Warsaw (Poland); Stöcker, Hartmut [TU Bergakademie Freiberg, Institute of Experimental Physics, Leipziger str. 23, 09596, Freiberg (Germany); Szalaty, Tadeusz J. [Poznan University of Technology, Faculty of Chemical Technology, Institute of Chemical Technology and Engineering, Berdychowo 4, 60965, Poznan (Poland); Bazhenov, Vasilii V., E-mail: vasily.bazhenov@gmail.com [TU Bergakademie Freiberg, Institute of Experimental Physics, Leipziger str. 23, 09596, Freiberg (Germany); Stelling, Allison L. [Duke University, Department of Biochemistry, Durham, NC, 27708 (United States); Beyer, Jan; Heitmann, Johannes [TU Bergakademie Freiberg, Institute of Applied Physics, Leipziger str. 23, 09596, Freiberg (Germany); Jesionowski, Teofil [Poznan University of Technology, Faculty of Chemical Technology, Institute of Chemical Technology and Engineering, Berdychowo 4, 60965, Poznan (Poland); Petovic, Slavica; Đurović, Mirko [Institute of Marine Biology, Dobrota, 85330, Kotor (Montenegro); Ehrlich, Hermann [TU Bergakademie Freiberg, Institute of Experimental Physics, Leipziger str. 23, 09596, Freiberg (Germany)

2017-02-15

This work presents an extreme biomimetics route for the modification of the surface of fibre-based scaffolds of poriferan origin by the creation of novel nanostructured multiphase biocomposites. The exceptional thermal stability of the nanostructured sponge chitin allowed for the formation of a novel nanocrystalline chitin-(Ti,Zr)O{sub 2} composite with a well-defined nanoscale structure under hydrothermal conditions (160 °C). Using a combination of experimental techniques, including X-ray diffraction, scanning electron microscopy, high resolution transmission electron microscopy, EDX mapping and near-edge electron loss spectroscopy (ELNES) in TEM and thermogravimetry/differential scanning calorimetry coupled with mass spectrometry; we showed that this bioorganic scaffold facilitates selective crystallization of TiO{sub 2}, predominantly in form of anatase, over the monoclinic zirconium dioxide (baddeleyite). The control of the crystal morphology through the chitin templates is also demonstrated. Obtained samples were characterized in terms of their photoluminescent properties and photocatalytic performance. These data confirm the high potential of the extreme biomimetics approach for developing a new generation of multiphase biopolymer-based nanostructured materials. - Highlights: • Extreme biomimetically prepared chitin-(Ti,Zr)O{sub 2} and (Ti,Zr)O{sub 2} composites. • Chitin-(Ti,Zr)O{sub 2} composite contains anatase as the most inorganic component. • The mean crystallite size is (31.7 ± 0.3) nm for chitin-(Ti,Zr)O{sub 2} composite. • The mean crystallite size is (2.4 ± 0.5) nm for (Ti,Zr)O{sub 2} composite. • (Ti,Zr)O{sub 2} composite is 2 times more effective photocatalyst than chitin-(Ti,Zr)O{sub 2}.

Radioactivity and associated radiation hazards in ceramic raw materials and end products.

Science.gov (United States)

Viruthagiri, G; Rajamannan, B; Suresh Jawahar, K

2013-12-01

Studies have been planned to obtain activity and associated radiation hazards in ceramic raw materials (quartz, feldspar, clay, zircon, kaolin, grog, alumina bauxite, baddeleyite, masse, dolomite and red mud) and end products (ceramic brick, glazed ceramic wall and floor tiles) as the activity concentrations of uranium, thorium and potassium vary from material to material. The primordial radionuclides in ceramic raw materials and end products are one of the sources of radiation hazard in dwellings made of these materials. By the determination of the activity level in these materials, the indoor radiological hazard to human health can be assessed. This is an important precautionary measure whenever the dose rate is found to be above the recommended limits. The aim of this work was to measure the activity concentration of (226)Ra, (232)Th and (40)K in ceramic raw materials and end products. The activity of these materials has been measured using a gamma-ray spectrometry, which contains an NaI(Tl) detector connected to multichannel analyser (MCA). Radium equivalent activity, alpha-gamma indices and radiation hazard indices associated with the natural radionuclides are calculated to assess the radiological aspects of the use of the ceramic end products as decorative or covering materials in construction sector. Results obtained were examined in the light of the relevant international legislation and guidance and compared with the results of similar studies reported in different countries. The results suggest that the use of ceramic end product samples examined in the construction of dwellings, workplace and industrial buildings is unlikely to give rise to any significant radiation exposure to the occupants.

Radioactivity and associated radiation hazards in ceramic raw materials and end products

International Nuclear Information System (INIS)

Viruthagiri, G.; Rajamannan, B.; Suresh Jawahar, K.

2013-01-01

Studies have been planned to obtain activity and associated radiation hazards in ceramic raw materials (quartz, feldspar, clay, zircon, kaolin, grog, alumina bauxite, baddeleyite, masse, dolomite and red mud) and end products (ceramic brick, glazed ceramic wall and floor tiles) as the activity concentrations of uranium, thorium and potassium vary from material to material. The primordial radionuclides in ceramic raw materials and end products are one of the sources of radiation hazard in dwellings made of these materials. By the determination of the activity level in these materials, the indoor radiological hazard to human health can be assessed. This is an important precautionary measure whenever the dose rate is found to be above the recommended limits. The aim of this work was to measure the activity concentration of 226 Ra, 232 Th and 40 K in ceramic raw materials and end products. The activity of these materials has been measured using a gamma-ray spectrometry, which contains an NaI(Tl) detector connected to multichannel analyser (MCA). Radium equivalent activity, alpha-gamma indices and radiation hazard indices associated with the natural radionuclides are calculated to assess the radiological aspects of the use of the ceramic end products as decorative or covering materials in construction sector. Results obtained were examined in the light of the relevant international legislation and guidance and compared with the results of similar studies reported in different countries. The results suggest that the use of ceramic end product samples examined in the construction of dwellings, workplace and industrial buildings is unlikely to give rise to any significant radiation exposure to the occupants. (authors)

Zirconium and hafnium

Science.gov (United States)

Jones, James V.; Piatak, Nadine M.; Bedinger, George M.; Schulz, Klaus J.; DeYoung,, John H.; Seal, Robert R.; Bradley, Dwight C.

2017-12-19

Zirconium and hafnium are corrosion-resistant metals that are widely used in the chemical and nuclear industries. Most zirconium is consumed in the form of the main ore mineral zircon (ZrSiO4, or as zirconium oxide or other zirconium chemicals. Zirconium and hafnium are both refractory lithophile elements that have nearly identical charge, ionic radii, and ionic potentials. As a result, their geochemical behavior is generally similar. Both elements are classified as incompatible because they have physical and crystallochemical properties that exclude them from the crystal lattices of most rock-forming minerals. Zircon and another, less common, ore mineral, baddeleyite (ZrO2), form primarily as accessory minerals in igneous rocks. The presence and abundance of these ore minerals in igneous rocks are largely controlled by the element concentrations in the magma source and by the processes of melt generation and evolution. The world’s largest primary deposits of zirconium and hafnium are associated with alkaline igneous rocks, and, in one locality on the Kola Peninsula of Murmanskaya Oblast, Russia, baddeleyite is recovered as a byproduct of apatite and magnetite mining. Otherwise, there are few primary igneous deposits of zirconium- and hafnium-bearing minerals with economic value at present. The main ore deposits worldwide are heavy-mineral sands produced by the weathering and erosion of preexisting rocks and the concentration of zircon and other economically important heavy minerals, such as ilmenite and rutile (for titanium), chromite (for chromium), and monazite (for rare-earth elements) in sedimentary systems, particularly in coastal environments. In coastal deposits, heavy-mineral enrichment occurs where sediment is repeatedly reworked by wind, waves, currents, and tidal processes. The resulting heavy-mineral-sand deposits, called placers or paleoplacers, preferentially form at relatively low latitudes on passive continental margins and supply 100 percent of

The synthesis and certification of zirconia certified reference materials (CRM) as a processed result of zircon sand

International Nuclear Information System (INIS)

Samin; Supriyanto C; Sajima

2016-01-01

In order to support the pilot plant of zirconia production at PSTA-BATAN, synthesis and certification of zirconia certified reference materials (CRM) is absolutely needed. The synthesis and certification of zirconia CRM has been carried out from the row material of zirconium oxide chloride as a processed result of Kalimantan zircon sand. Zirconium oxide chloride dissolved in distilled water (1:10), added by ammonia at pH 10, it was formed a zirconium hydroxide precipitate. Zirconium hydroxide was heated at 110 °C and calcination at a temperature of 900 °C in order to obtain zirconia. Zirconia was dried at 110 °C, crushed and sieved to obtain a grain size of 200 mesh qualify. Zirconia powder was homogenized and then treated by homogenation test, stabilization test, characterization test and water content test. In the evaluation of the test data showed that candidate of CRM zirconia were homogeneous, stable, contain the monoklin of baddeleyite minerals and the water content obtained was less than 1%. It was concluded that zirconia powder are already physical qualified as CRM. Certificate of test results on parameters of zirconia CRM from 7 accredited laboratories using statistical methods obtained 9 oxides were ZrO_2 : (95.422 ± 0.027)%; HfO_2: (1.443 ± 0.004)%; SiO_2 : (0.535 ± 0.002)%; Al_2O_3 : (0.362 ± 0.012)%; Fe_2O_3 : (0.028 ± 0.003)%; TiO_2: (0.026 ± 0.001) %; Na_2O: (0.262 ± 0.026)%; Nd_2O_3 : (0.0367 ± 0.007)%; CeO_2: (0.131 ± 0.013)%. This certification was traceable to BCS-CRM No. 358 zirconia from BAS-France. (author)

δ18O and chemical composition of Libyan Desert Glass, country rocks, and sands: New considerations on target material

Science.gov (United States)

Longinelli, Antonio; Sighinolfi, Giampaolo; de Michele, Vincenzo; Selmo, Enricomaria

2011-02-01

Oxygen isotope and chemical measurements were carried out on 25 samples of Libyan Desert Glass (LDG), 21 samples of sandstone, and 3 of sand from the same area. The δ18O of LDG samples range from 9.0‰ to 11.9‰ (Vienna Standard Mean Ocean Water [VSMOW]); some correlations between isotope data and typological features of the LDG samples are pointed out. The initial δ18O of a bulk parent material may be slightly increased by fusion due to the loss of isotopically light pore water with no isotope exchange with oxygen containing minerals. Accordingly, the δ18O of the bulk parent material of LDG may have been about 9.0 ± 1‰ (VSMOW). The measured bulk sandstone and sand samples have δ18O values ranging from 12.6‰ to 19.5‰ and are consequently ruled out as parent materials, matching the results of previous studies. However, separated quartz fractions have δ18O values compatible with the LDG values suggesting that the modern surface sand inherited quartz from the target material. This hypothesis fits previous findings of lechatelierite and baddeleyite in these materials. As the age of the parent material reported in previous studies is Pan-African, we measured the δ18O values of bulk rock and quartz from intrusives of Pan-African age and the results obtained were compatible with the LDG values. The main element abundances (Fe, Mg, Ca, K, Na) in our LDG samples conform to previous estimates; Fe, Mg, and K tend to be higher in heterogeneous samples with dark layers. The hypothesis of a low-altitude airburst involving silica-rich surface materials deriving from weathered intrusives of Pan-African age, partially melted and blown over a huge surface by supersonic winds matches the results obtained.

Zirconium - an imported mineral commodity

International Nuclear Information System (INIS)

1983-10-01

This report examines Canada's position in regard to the principal zirconium materials: zircon; fusion-cast zirconium-bearing refractory products; zirconium-bearing chemicals; and zirconium metal, master alloys, and alloys. None of these is produced in Canada except fused alumina-zirconia and certain magnesium-zirconium alloys and zirconium-bearing steels. Most of the 3 000-4 000 tonnes of the various forms of zircon believed to be consumed in Canada each year is for foundry applications. Other minerals, notably chromite, olivine and silica sand are also used for these purposes and, if necessary, could be substituted for zircon. Zirconium's key role in Canada is in CANDU nuclear power reactors, where zirconium alloys are essential in the cladding for fuel bundles and in capital equipment such as pressure tubes, calandria tubes and reactivity control mechanisms. If zirconium alloys were to become unavailable, the Canadian nuclear power industry would collapse. As a contingency measure, Ontario Hydro maintains at least nine months' stocks of nuclear fuel bundles. Canada's vulnerability to short-term disruptions to supplies of nuclear fuel is diminished further by the availability of more expensive electricity from non-nuclear sources and, given time, from mothballed thermal plants. Zirconium minerals are present in many countries, notably Australia, the Republic of South Africa and the United States. Australia is Canada's principal source of zircon imports; South Africa is its sole source of baddeleyite. At this time, there are no shortages of either material. Canada has untapped zirconium resources in the Athabasca Oil Sands (zircon) and at Strange Lake along the ill-defined border between Quebec and Newfoundland (gittinsite). Adequate metal and alloy production facilities exist in France, Japan and the United States. No action by the federal government in regard to zirconium supplies is called for at this time

An Integrated Geochronological, Petrological, Geochemical and Paleomagnetic Study of Paleoproterozoic and Mesoproterozoic Mafic Dyke Swarms in the Nain Craton, Labrador

Science.gov (United States)

Sahin, Tugce

The Nain craton comprises the western, Labrador segment of the larger North Atlantic craton (NAC) which exposes Early through Late Archean gneisses. The NAC is bounded on all sides by Paleoproterozoic collisional orogens that involved either considerable structural reworking (Torngat-Nagssugtoqidian-Lewisian) or the accretion of juvenile arc magmas (Ketilidian-Makkovik). The NAC remains poorly understood compared to other Archean crustal blocks now dispersed globally. Compounding this problem is a lack of reliable paleomagnetic poles for NAC units that predate its assembly into the supercontinent Laurentia by ca. 1800 Ma, which could be used to test neighboring relationships with other cratonic fragments. In order to understand the history of the NAC as part of a possible, larger supercontinent, the record of mafic dyke swarms affecting the craton, particularly those that postdate the Late Archean terrane assembly, were examined in this study. Diabase or gabbroic dyke swarms are invaluable in such studies because their geometries offer possible locus points, they often have a punctuated emplacement and precisely datable crystallization histories, and they have cooling histories and oxide mineralogy amenable to recovering robust paleopoles. Coastal Labrador exposes a number of mafic dykes, some of which are demonstrably Paleoproterozoic (e.g. 2235 Ma Kikkertavak dykes; 2121 Ma Tikkigatsiagak dykes) or Mesoproterozoic (e.g. 1280-1270 Ma Nain and Harp dykes) in age (U-Pb; baddeleyite or zircon). The southern half of the Nain craton (Hopedale block) in particular preserves a rich array of mafic dykes. Dyke cross-cutting relationships are numerous and relatively well exposed, permitting multiple opportunities for paleomagnetic field tests (e.g. baked contact). The results presented here allow understanding of the tectonic evolution of the NAC with implications for strengthened Labrador-Greenland correlations, and testing possible Paleoproterozoic supercontinent

The P3 kimberlite and P4 lamproite, Wajrakarur kimberlite field, India: mineralogy, and major and minor element compositions of olivines as records of their phenocrystic vs xenocrystic origin

Science.gov (United States)

Shaikh, Azhar M.; Kumar, Satya P.; Patel, Suresh C.; Thakur, Satyajeet S.; Ravi, Subramanian; Behera, Duryadhan

2018-03-01

Distinctly different groundmass mineralogy characterise the hypabyssal facies, Mesoproterozoic diamondiferous P3 and P4 intrusions from the Wajrakarur Kimberlite Field, southern India. P3 is an archetypal kimberlite with macrocrysts of olivine and phlogopite set in a groundmass dominated by phlogopite and monticellite with subordinate amounts of serpentine, spinel, perovskite, apatite, calcite and rare baddeleyite. P4 contains mega- and macrocrysts of olivine set in a groundmass dominated by clinopyroxene and phlogopite with subordinate amounts of serpentine, spinel, perovskite, apatite, and occasional gittinsite, and is mineralogically interpreted as an olivine lamproite. Three distinct populations of olivine, phlogopite and clinopyroxene are recognized based on their microtextural and compositional characteristics. The first population includes glimmerite and phlogopite-clinopyroxene nodules, and Mg-rich olivine macrocrysts (Fo 90-93) which are interpreted to be derived from disaggregated mantle xenoliths. The second population comprises macrocrysts of phlogopite and Fe-rich olivine (Fo 81-89) from P3, megacrysts and macrocrysts of Fe-rich olivine (Fo 85-87) from P4 and a rare olivine-clinopyroxene nodule from P4 which are suggested to have a genetic link with the precursor melt of the respective intrusions. The third population represents clearly magmatic minerals such as euhedral phenocrysts of Fe-rich olivine (Fo 85-90) crystallised at mantle depths, and olivine overgrowth rims formed contemporaneously with groundmass minerals at crustal levels. Close spatial association and contemporaneous emplacement of P3 kimberlite and P4 lamproite is explained by a unifying petrogenetic model which involves the interaction of a silica-poor carbonatite melt with differently metasomatised wall rocks in the lithospheric mantle. It is proposed that the metasomatised wall rock for lamproite contained abundant MARID-type and phlogopite-rich metasomatic veins, while that for

Initial Evaluation of Processing Methods for an Epsilon Metal Waste Form

International Nuclear Information System (INIS)

Crum, Jarrod V.; Strachan, Denis M.; Zumhoff, Mac R.

2012-01-01

to have a high melting point as well, perhaps exceeding 1500 C. The purpose of the work reported here is to find a potential commercial process with which (var e psilon)-metal plus other components of UDS can be consolidated into a solid with minimum surface area and high strength Here, we report the results from the preliminary evaluation of spark-plasma sintering (SPS), hot-isostatic pressing (HIP), and microwave sintering (MS). Since bulk (var e psilon)-metal is not available and companies could not handle radioactive materials, we prepared mixtures of the five individual metal powders (Mo, Ru, Rh, Pd, and Re) and baddeleyite (ZrO 2 ) to send the vendors of SPS, HIP, and MS. The processed samples were then evaluated at the Pacific Northwest National Laboratory (PNNL) for bulk density and phase assemblage with X-ray diffraction (XRD) and phase composition with scanning electron microscopy (SEM). Physical strength was evaluated qualitatively. Results of these scoping tests showed that fully dense cermet (ceramic-metal composite) materials with up to 35 mass% of ZrO 2 were produced with SPS and HIP. Bulk density of the SPS samples ranged from 87 to 98% of theoretical density, while HIP samples ranged from 96 to 100% of theoretical density. Microwave sintered samples containing ZrO 2 had low densities of 55 to 60% of theoretical density. Structurally, the cermet samples showed that the individual metals alloyed in to (var e psilon)-phase - hexagonal-close-packed (HCP) alloy (4-95 mass %), the α-phase - face-centered-cubic (FCC) alloy structure (3-86 mass %), while ZrO 2 remained in the monoclinic structure of baddeleyite. Elementally, the samples appeared to have nearly uniform composition, but with some areas rich in Mo and Re, the two components with the highest melting points. The homogeneity in distribution of the elements in the alloy is significantly improved in the presence of ZrO 2 . However, ZrO 2 does not appear to react with the alloy, nor was Zr found in

Mineralogy and geochemistry of triassic carbonatites in the Matcha alkaline intrusive complex (Turkestan-Alai Ridge, Kyrgyz Southern Tien Shan), SW Central Asian orogenic belt

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Vrublevskii, V. V.; Morova, A. A.; Bukharova, O. V.; Konovalenko, S. I.

2018-03-01

Postorogenic intrusions of essexites and alkaline and nepheline syenites in the Turkestan-Alai segment of the Kyrgyz Southern Tien Shan coexist with dikes and veins of carbonatites dated at ∼220 Ma by the Ar-Ar and Rb-Sr age methods. They are mainly composed of calcite and dolomite (60-85%), as well as sodic amphibole, phlogopite, clinopyroxene, microcline, albite, apatite, and magnetite, with accessory niobate, ilmenite, Nb-rutile, titanite, zircon, baddeleyite, monazite-(Ce), barite, and sulfides. The rocks share mineralogical and geochemical similarity with carbonatites that originated by liquid immiscibility at high temperatures above 500 °C. Alkaline silicate and salt-carbonate melts are derived from sources with mainly negative bulk εNd(t) ∼ from -11 to 0 and high initial 87Sr/86Sr ratios (∼0.7061-0.7095) which may be due to mixing of PREMA and EM-type mantle material. Pb isotopic ratios in accessory pyrrhotite (206Pb/204Pb = 18.38; 207Pb/204Pb = 15.64; 208Pb/204Pb = 38.41) exhibit an EM2 trend. The intrusions bear signatures of significant crustal contamination as a result of magma genesis by syntexis and hybridism. Concordant isotope composition changes of δ13C (-6.5 to -1.9‰), δ18O (9.2-23‰), δD (-58 to -41‰), and δ34S (12.6-12.8‰) in minerals and rocks indicate inputs of crustal material at the stage of melting and effect of hot fluids released during dehydration of metamorphosed oceanic basalts or sediments. The observed HFSE patterns of the oldest alkaline gabbro may be due to interaction of the primary mafic magma with IAB-type material. The isotope similarity of alkaline rocks with spatially proximal basalts of the Tarim large igneous province does not contradict the evolution of the Turkestan-Alai Triassic magmatism as the "last echo" of the Tarim mantle plume.

Paraná flood basalt volcanism primarily limited to 1 Myr beginning at 135 Ma: New 40Ar/39Ar ages for rocks from Rio Grande do Sul, and critical evaluation of published radiometric data

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Baksi, Ajoy K.

2018-04-01

40Ar/39Ar step heating analyses were carried out on seven rocks (five basalts, an andesite and a rhyolite) from the southern Paraná Province ( 28°S-30°S); they yield plateau/isochron ages of 135-134 Ma, in good agreement with published step heating data on rocks from the same area. Critical review of laser spot isochron ages for rocks from the Province, ranging from 140 to 130 Ma, are shown to be unreliable estimates of crystallization ages, as the rocks were substantially altered; step heating results on three of these rocks thought to yield good plateau ages, are shown to be incorrect, as a result of a technicality in dating procedures followed. U-Pb ages on zircon and baddeleyite separated from a variety of rock types ( 30°S-23°S) fall in the range 135 to 134 Ma. All reliable 40Ar/39Ar and U-Pb ages indicate volcanism was sharply focused, initiated at 135 Ma, and 1 Myr in duration; no variation of age with either latitude or longitude is noted, Scrutiny of published 40Ar/39Ar ages on the Florianopolis dykes shows they cannot be used as reliable crystallization ages. U-Pb work shows that this dyke swarm was formed coevally with the main part of the Parana province. Most of the published 40Ar/39Ar ages on the Ponta Grossa dyke swarm are unreliable; a few ages appear reliable and suggest the magmatic event in this area, may have postdated the main Paraná pulse by 1-2 Myr. A single 40Ar/39Ar age from a high-Nb basalt in the southernmost part ( 34°S) of the Paraná at 135 Ma, highlights the need for further radiometric work on other areas of this flood basalt province. The Paraná Province postdates the time of the Jurassic-Cretaceous bound­ary by 10 Myr.

Silurian extension in the Upper Connecticut Valley, United States and the origin of middle Paleozoic basins in the Québec embayment

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Rankin, D.W.; Coish, R.A.; Tucker, R.D.; Peng, Z.X.; Wilson, S.A.; Rouff, A.A.

2007-01-01

Pre-Silurian strata of the Bronson Hill arch (BHA) in the Upper Connecticut Valley, NH-VT are host to the latest Ludlow Comerford Intrusive Suite consisting, east to west, of a mafic dike swarm with sheeted dikes, and an intrusive complex. The rocks are mostly mafic but with compositions ranging from gabbro to leucocratic tonalite. The suite is truncated on the west by the Monroe fault, a late Acadian thrust that carries rocks of the BHA westward over Silurian-Devonian strata of the Connecticut Valley-Gaspe?? trough (CVGT). Dikes intrude folded strata with a pre-intrusion metamorphic fabric (Taconian?) but they experienced Acadian deformation. Twenty fractions of zircon and baddeleyite from three sample sites of gabbrodiorite spanning nearly 40 km yield a weighted 207Pb/206Pb age of 419 ?? 1 Ma. Greenschist-facies dikes, sampled over a strike distance of 35 km, were tholeiitic basalts formed by partial melting of asthenospheric mantle, with little or no influence from mantle or crustal lithosphere. The dike chemistry is similar to mid-ocean ridge, within-plate, and back-arc basin basalts. Parent magmas originated in the asthenosphere and were erupted through severely thinned lithosphere adjacent to the CVGT. Extensive middle Paleozoic basins in the internides of the Appalachian orogen are restricted to the Que??bec embayment of the Laurentian rifted margin, and include the CVGT and the Central Maine trough (CMT), separated from the BHA by a Silurian tectonic hinge. The NE-trending Comerford intrusions parallel the CVGT, CMT, and the tectonic hinge, and indicate NW-SE extension. During post-Taconian convergence, the irregular margins of composite Laurentia and Avalon permitted continued collision in Newfoundland (St. Lawrence promontory) and coeval extension in the Que??bec embayment. Extension may be related to hinge retreat of the northwest directed Brunswick subduction complex and rise of the asthenosphere following slab break-off. An alternative hypothesis is

Understanding Magmatic Timescales and Magma Dynamics in Proterozoic Anorthosites: a Geochronological Investigation of the Kunene Complex (Angola)

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Brower, A. M.; Corfu, F.; Bybee, G. M.; Lehmann, J.; Owen-Smith, T.

2016-12-01

The Kunene Anorthosite Complex, located in south west Angola, is one of the largest massif-type anorthosite intrusions on Earth, with an areal extent of at least 18 000 km2. Previous studies considered the Complex to consist of a series of coalesced plutons. However, the ages and relative emplacement sequence of these plutons are unknown. Understanding the relative timing of the pluton emplacement is crucial for understanding how these enigmatic magmas form and how they rise through the crust. Here we present new high precision U-Pb ID-TIMS ages (n=10) on zircons and baddeleyites for many of the coalesced plutons across the 300-km-long anorthositic complex. These new geochronological results reveal subtle variations in crystallization age between the coalesced plutons. There is no gradual age progression between plutons, but distinct groupings of ages (Fig.1). Age clusters of 1379.8 ± 2 Ma (n=5) occur north of the Red Granite NE-SW-striking intrusions, whereas in the south there is an older age grouping of 1390.4 ± 2.3 (n=3). Two additional ages of 1400.5 ± 1.3 in the centre and 1438.4 ± 1.1 Ma in the south east have been obtained. These results indicate that the Kunene anorthosites were emplaced over 60 Ma and may suggest long-lived magmatic systems and/or slowly ascending plutons. We also find a link between pluton composition and age. In general, leuconoritic domains are older than the leucotroctolitic domains. This may imply that the first pulses of magma received a greater degree of contamination, forcing the broadly basaltic magma to produce orthopyroxene as the main mafic phase. The later pulses receive less contamination as they ascend through the already partially melted crust, producing olivine as the mafic phase and deforming the older domains. This study reiterates the multiphase petrogenesis of Proterozoic anorthosites and sheds light on the assembly of crystal-rich magmas as they ascend through the crust.

40Ar/39Ar geochronology of terrestrial pyroxene

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Ware, Bryant; Jourdan, Fred

2018-06-01

Geochronological techniques such as U/Pb in zircon and baddeleyite and 40Ar/39Ar on a vast range of minerals, including sanidine, plagioclase, and biotite, provide means to date an array of different geologic processes. Many of these minerals, however, are not always present in a given rock, or can be altered by secondary processes (e.g. plagioclase in mafic rocks) limiting our ability to derive an isotopic age. Pyroxene is a primary rock forming mineral for both mafic and ultramafic rocks and is resistant to alteration process but attempts to date this phase with 40Ar/39Ar has been met with little success so far. In this study, we analyzed pyroxene crystals from two different Large Igneous Provinces using a multi-collector noble gas mass spectrometer (ARGUS VI) since those machines have been shown to significantly improve analytical precision compared to the previous single-collector instruments. We obtain geologically meaningful and relatively precise 40Ar/39Ar plateau ages ranging from 184.6 ± 3.9 to 182.4 ± 0.8 Ma (2σ uncertainties of ±1.8-0.4%) and 506.3 ± 3.4 Ma for Tasmanian and Kalkarindji dolerites, respectively. Those data are indistinguishable from new and/or published U-Pb and 40Ar/39Ar plagioclase ages showing that 40Ar/39Ar dating of pyroxene is a suitable geochronological tool. Scrutinizing the analytical results of the pyroxene analyses as well as comparing them to the analytical result from plagioclase of the same samples indicate pure pyroxene was dated. Numerical models of argon diffusion in plagioclase and pyroxene support these observations. However, we found that the viability of 40Ar/39Ar dating approach of pyroxene can be affected by irradiation-induced recoil redistribution between thin pyroxene exsolution lamellae and the main pyroxene crystal, hence requiring careful petrographic observations before analysis. Finally, diffusion modeling show that 40Ar/39Ar of pyroxene can be used as a powerful tool to date the formation age of mafic

Protoliths of enigmatic Archaean gneisses established from zircon inclusion studies: Case study of the Caozhuang quartzite, E. Hebei, China

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Allen P. Nutman

2014-07-01

Full Text Available A diverse suite of Archaean gneisses at Huangbaiyu village in the North China Craton, includes rare fuchsite-bearing (Cr-muscovite siliceous rocks – known as the Caozhuang quartzite. The Caozhuang quartzite is strongly deformed and locally mylonitic, with silica penetration and pegmatite veining common. It contains abundant 3880–3600 Ma and some Palaeoarchaean zircons. Because of its siliceous nature, the presence of fuchsite and its complex zircon age distribution, it has until now been accepted as a (mature quartzite. However, the Caozhuang quartzite sample studied here is feldspathic. The shape and cathodoluminescence petrography of the Caozhuang quartzite zircons show they resemble those found in immature detrital sedimentary rocks of local provenance or in Eoarchaean polyphase orthogneisses, and not those in mature quartzites. The Caozhuang quartzite intra-zircon mineral inclusions are dominated by quartz, with lesser biotite, apatite (7% and alkali-feldspar, and most inclusions are morphologically simple. A Neoarchaean orthogneiss from near Huangbaiyu displays morphologically simple inclusions with much more apatite (73%, as is typical for fresh calc-alkaline granitoids elsewhere. Zircons were also examined from a mature conglomerate quartzite clast and an immature feldspathic sandstone of the overlying weakly metamorphosed Mesoproterozoic Changcheng System. These zircons have oscillatory zoning, showing they were sourced from igneous rocks. The quartzite clast zircons contain only rare apatite inclusions (<1%, with domains with apatite habit now occupied by intergrowths of muscovite + quartz ± Fe-oxides ± baddeleyite. We interpret that these were once voids after apatite inclusions that had dissolved during Mesoproterozoic weathering, which were then filled with clays ± silica and then weakly metamorphosed. Zircons in the immature feldspathic sandstone show a greater amount of preserved apatite (11%, but with petrographic

Mantle reservoirs (EM-1, OIB, E-MORB and N-MORB), long duration and polystages history for PGE-bearing paleoproterozoic layered intrusions in the N-E part of Fennoscandian Shield.

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Bayanova, Tamara; Nerovich, Ludmila; Serov, Pavel; Kunakkuzin, Evgeniy; Elizarov, Dmitriy

2015-04-01

Paleoproterozoic layered PGE -bearing intrusions located in the N-E part of the Fennoscandian Shield and have a total are about 2000 km2. Long multidisciplinary studies using isotope Nd-Sr, U-Pb and 3He/4He systematics permit create a big bank of geochemistry data for different part of the intrusions: barren and main Cu-Ni-Cr-Ti-V and PGE phases, dykes complexes and host rocks. Based on U-Pb isotope data (on baddeleyite and zircon) and Sm-Nd mineral isochrones (on rock-forming and sulphides minerals) there is distinguished long magmatic duration from 2.53 to 2.40 Ga. Using precise U-Pb and Sm-Nd data for different part of the intrusions there are established four main impulses: 2.53, 2.50, 2.45, and 2.40 Ga of magmatic (LIP) activities for gabbronorite, anothosite et.set. rocks. The primary reservoir for all precious and multimetal massifs are considered as enriched mantle EM-1 using ɛNd- ISr system with negative ɛNd values and low ISr data for whole rocks of the intrusions. Dyke complexes are presented as three groups: high Ti-ferrodolerites, low Ti and low Fe-gabbronorites. Complex isotope (U-Pb, Sm-Nd) and geochemistry (REE, ɛNd, ISr) data investigations reflect OIB, E-MORB and N-MORB reservoirs for its origin (Nerovich et all., 2014). Isotope 3He/4He and 3He concentrations for accessory minerals ( ilmenite, magnetite et. set ) from the layered paleoproterozoic intrusions reflect significant lower mantle component and upper mantle contribution. According to the model of binary mixing (Jahn et all, 2000) there were calculated mantle and core component into plume magmatic reservoir connected with the origin of the PGE paleoproterozoic intrusions. The mantle contributions lie in the interval from 85 to 93% and core component are very less. All investigations are devoted to memory of academician RAS, professor F.Mitrofanov (Russia), he was a leader of scientific school for geology, geochemistry and metallogenesis of ore deposits. The studies are

CONCH: A Visual Basic program for interactive processing of ion-microprobe analytical data

Science.gov (United States)

Nelson, David R.

2006-11-01

A Visual Basic program for flexible, interactive processing of ion-microprobe data acquired for quantitative trace element, 26Al- 26Mg, 53Mn- 53Cr, 60Fe- 60Ni and U-Th-Pb geochronology applications is described. Default but editable run-tables enable software identification of secondary ion species analyzed and for characterization of the standard used. Counts obtained for each species may be displayed in plots against analysis time and edited interactively. Count outliers can be automatically identified via a set of editable count-rejection criteria and displayed for assessment. Standard analyses are distinguished from Unknowns by matching of the analysis label with a string specified in the Set-up dialog, and processed separately. A generalized routine writes background-corrected count rates, ratios and uncertainties, plus weighted means and uncertainties for Standards and Unknowns, to a spreadsheet that may be saved as a text-delimited file. Specialized routines process trace-element concentration, 26Al- 26Mg, 53Mn- 53Cr, 60Fe- 60Ni, and Th-U disequilibrium analysis types, and U-Th-Pb isotopic data obtained for zircon, titanite, perovskite, monazite, xenotime and baddeleyite. Correction to measured Pb-isotopic, Pb/U and Pb/Th ratios for the presence of common Pb may be made using measured 204Pb counts, or the 207Pb or 208Pb counts following subtraction from these of the radiogenic component. Common-Pb corrections may be made automatically, using a (user-specified) common-Pb isotopic composition appropriate for that on the sample surface, or for that incorporated within the mineral at the time of its crystallization, depending on whether the 204Pb count rate determined for the Unknown is substantially higher than the average 204Pb count rate for all session standards. Pb/U inter-element fractionation corrections are determined using an interactive log e-log e plot of common-Pb corrected 206Pb/ 238U ratios against any nominated fractionation-sensitive species pair

Compositional variations of zirconolite from the Evate apatite deposit (Mozambique) as an indicator of magmatic-hydrothermal conditions during post-orogenic collapse of Gondwana

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Hurai, Vratislav; Huraiová, Monika; Gajdošová, Michaela; Konečný, Patrik; Slobodník, Marek; Siegfried, Pete R.

2018-06-01

Zirconolite is documented from the Evate apatite-magnetite-carbonate deposit in the circular Monapo Klippe (eastern Mozambique)—a relic of Neoproterozoic nappe thrusted over the Mesoproterozoic basement of the Nampula block. Zirconolite enriched in rare earth elements—REE = Y + Lu+ΣLa-Yb (up to 24.11 wt% REE2O3, 0.596 apfu REE) creates thin rims around spinel and magnetite grains, whereas zirconolite enriched in U and Th (up to 18.88 wt% ThO2 + UO2, 0.293 apfu Th + U) replace the Late Ediacaran ( 590 Ma) zircon and baddeleyite along contacts with pyrrhotite and magnetite. Both types of zirconolite contain locally increased Nb and Ta concentrations (up to 7.58 wt% Nb2O5 + Ta2O5, 0.202 apfu Nb + Ta). Typical substitutions in zirconolite from Evate involve REE + U,Th → Ca, and M 2++ M 5+→Ti + M 3+ ( M 2+ = Fe2++Mg, M 3+ = Fe3+, M 5+ = Nb5++Ta5+). In addition, REE-zirconolite is typical of the REE + M 2+ → Ca + M 3+ substitution ( M 2+ = Mg, M 3+ = Fe3++Al3+). Hence, Fe3+ predominates over Fe2+ in all types of zirconolite, thus enabling the high REE content in Nb-poor zirconolites to be stored in locally dominant REEZrTiFe3+O7 component known so far only as a synthetic analogue of natural zirconolite. Other types of zirconolite from Evate are dominated by the common CaZrTi2O7 end member, but the aforementioned "synthetic" REEZrTiFe3+O7 accompanied by another `synthetic' (U,Th)ZrFe3 + 2O7 component are also abundant. The U,Pb,Th concentrations in U,Th-zirconolites plot discordantly to theoretical isochrons, thus indicating 440 ppm of non-radiogenic excess lead in earlier Nb-rich zirconolite contrasting with secondary Pb loss from later Nb-poor zirconolite. The non-radiogenic Pb-corrected age of the early zirconolite corresponded to 485 ± 9 Ma, within uncertainty limit identical with the 493 ± 10 Ma age of the associated uranothorianite. The variegated chemical composition of zirconolites reflects the complex history of the Evate deposit. Compositional and

Compositional variations of zirconolite from the Evate apatite deposit (Mozambique) as an indicator of magmatic-hydrothermal conditions during post-orogenic collapse of Gondwana

Science.gov (United States)

Hurai, Vratislav; Huraiová, Monika; Gajdošová, Michaela; Konečný, Patrik; Slobodník, Marek; Siegfried, Pete R.

2017-11-01

Zirconolite is documented from the Evate apatite-magnetite-carbonate deposit in the circular Monapo Klippe (eastern Mozambique)—a relic of Neoproterozoic nappe thrusted over the Mesoproterozoic basement of the Nampula block. Zirconolite enriched in rare earth elements—REE = Y + Lu+ΣLa-Yb (up to 24.11 wt% REE2O3, 0.596 apfu REE) creates thin rims around spinel and magnetite grains, whereas zirconolite enriched in U and Th (up to 18.88 wt% ThO2 + UO2, 0.293 apfu Th + U) replace the Late Ediacaran ( 590 Ma) zircon and baddeleyite along contacts with pyrrhotite and magnetite. Both types of zirconolite contain locally increased Nb and Ta concentrations (up to 7.58 wt% Nb2O5 + Ta2O5, 0.202 apfu Nb + Ta). Typical substitutions in zirconolite from Evate involve REE + U,Th → Ca, and M 2++M 5+→Ti + M 3+ (M 2+ = Fe2++Mg, M 3+ = Fe3+, M 5+ = Nb5++Ta5+). In addition, REE-zirconolite is typical of the REE + M 2+ → Ca + M 3+ substitution (M 2+ = Mg, M 3+ = Fe3++Al3+). Hence, Fe3+ predominates over Fe2+ in all types of zirconolite, thus enabling the high REE content in Nb-poor zirconolites to be stored in locally dominant REEZrTiFe3+O7 component known so far only as a synthetic analogue of natural zirconolite. Other types of zirconolite from Evate are dominated by the common CaZrTi2O7 end member, but the aforementioned "synthetic" REEZrTiFe3+O7 accompanied by another `synthetic' (U,Th)ZrFe3 + 2O7 component are also abundant. The U,Pb,Th concentrations in U,Th-zirconolites plot discordantly to theoretical isochrons, thus indicating 440 ppm of non-radiogenic excess lead in earlier Nb-rich zirconolite contrasting with secondary Pb loss from later Nb-poor zirconolite. The non-radiogenic Pb-corrected age of the early zirconolite corresponded to 485 ± 9 Ma, within uncertainty limit identical with the 493 ± 10 Ma age of the associated uranothorianite. The variegated chemical composition of zirconolites reflects the complex history of the Evate deposit. Compositional and

Laachite, (Ca,Mn){sub 2}Zr{sub 2}Nb{sub 2}TiFeO{sub 14}, a new zirconolite-related mineral from the Eifel volcanic region, Germany

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Chukanov, Nikita V. [Institute of Problems of Chemical Physics, Chernogolovka (Russian Federation); Krivovichev, Sergey V.; Pakhomova, Anna S. [St. Petersburg State Univ. (Russian Federation). Faculty of Crystallography; Pekov, Igor V.; Vigasina, Marina F. [Moscow State Univ. (Russian Federation). Faculty of Geology; Schaefer, Christof [Suedwestdeutsche Salzwerke AG, Heilbronn (Germany); Van, Konstantin V. [Russian Academy of Sciences, Chernogolovka (Russian Federation). Inst. of Experimental Mineralogy

2014-02-15

The new mineral laachite was discovered in a sanidinite specimen from the Laach Lake (Laacher See) volcano, Eifel region, Rheinland-Pfalz, Germany. Associated minerals are sanidine, allanite-(Ce), baddeleyite, hau¨yne, hedenbergite, intermediate members of the jacobsite-magnetite series, phlogopite, rhodonite, spessartine, tephroite, thorite, zircon, and a pyrochlore-group mineral. Laachite is deep brownish-red, has an adamantine lustre, and is translucent; the streak is brownish red. It forms longprismatic crystals up to 0.02 x 0.04 x 0.5 mm, which are present as random intergrowths and twins in cavities within sanidinite. The density calculated from the empirical formula is 5.417 g/cm{sup 3}. The mean refractive index calculated from the Gladstone-Dale relationship is 2.26. The Raman spectrum shows the absence of hydrogen-bearing groups. The chemical composition is (electron microprobe, mean of 5 analyses, wt. %): CaO 4.29, MnO 9.42, FeO 5.73, Y{sub 2}O{sub 3} 2.56, La{sub 2}O{sub 3} 2.00, Ce{sub 2}O{sub 3} 6.37, Nd{sub 2}O{sub 3} 2.22, Al{sub 2}O{sub 3} 0.99, ThO{sub 2} 7.75, TiO{sub 2} 10.98, ZrO{sub 2} 19.39, Nb{sub 2}O{sub 5} 27.82, total 99.52. The empirical formula based on 14 O atoms is: (Ca{sub 0.66}Mn{sub 0.37}Th{sub 0.25}Y{sub 0.20}La{sub 0.11}Ce{sub 0.34}Nd{sub 0.11})(Zr{sub 1.3} {sub 6}Mn{sub 0.64})(Nb{sub 1.81}Ti{sub 1.19})(Fe{sub 0.69}Al{sub 0.17}Mn{sub 0.14})O{sub 14.00}. The simplified formula, taking into account the structural data, is: (Ca,Mn){sub 2}(Zr,Mn){sub 2}Nb{sub 2}TiFeO{sub 14}. Laachite is monoclinic, space group C2/c, a = 7.3119(5), b = 14.1790(10), c = 10.1700(7)Aa, β = 90.072(2), V = 1054.38(1) Aa{sup 3}, Z = 4. The crystal structure was solved using single-crystal X-ray diffraction data. Laachite is a monoclinic analogue of zirconolite-3O, CaZrTi{sub 2}O{sub 7}, with Nb dominant over Ti in the octahedral sites Nb1 and Nb2 and Fe dominant in a site with four-fold coordination. The strongest lines of the powder X-ray diffraction

Evaluating crustal contributions to enriched shergottites from the petrology, trace elements, and Rb-Sr and Sm-Nd isotope systematics of Northwest Africa 856

Science.gov (United States)

Ferdous, J.; Brandon, A. D.; Peslier, A. H.; Pirotte, Z.

2017-08-01

The origin of the incompatible trace element (ITE) characteristics of enriched shergottites has been critical for examining two contradicting scenarios to explain how these Martian meteorites form. The first scenario is that it reflects ITE enrichment in an early-formed mantle reservoir whereas the second scenario attributes it to assimilation of ancient Martian crust (∼4-4.5 Ga) by ITE-depleted magmas. Strongly differentiated shergottite magmas may yield added constraints for determining which scenario can best explain this signature in enriched shergottites. The meteorite Northwest Africa (NWA) 856 is a basaltic shergottite that, unlike many enriched shergottites, lacks olivine and has undergone extensive differentiation from more primitive parent magma. In similarity to other basaltic shergottites, NWA 856 is comprised primarily of compositionally zoned clinopyroxenes (45% pigeonite and 23% augite), maskelynite (23%) and accessory minerals such as ulvöspinel, merrillite, Cl-apatite, ilmenite, pyrrhotite, baddeleyite and silica polymorph. The CI-chondrite normalized rare earth element (REE) abundance patterns for its maskelynite, phosphates, and its whole rock are flat with corresponding light-REE depletions in clinopyroxenes. The 87Rb-87Sr and 147Sm-143Nd internal isochron ages are 162 ± 14 (all errors are ±2σ) Ma and 162.7 ± 5.5 Ma, respectively, with an initial εNdI = -6.6 ± 0.2. The Rb-Sr isotope systematics are affected by terrestrial alteration resulting in larger scatter and a less precise internal isochron age. The whole rock composition is used in MELTS simulations to model equilibrium and fractional crystallization sequences to compare with the crystallization sequence from textural observations and to the mineral compositions. These models constrain the depth of initial crystallization to a pressure range of 0.4-0.5 GPa (equivalent to 34-42 km) in anhydrous conditions at the Fayalite-Magnetite-Quartz buffer, and consistently reproduce the

Zirconium and hafnium in the southeastern Atlantic States

Science.gov (United States)

Mertie, J.B.

1958-01-01

The principal source of zirconium and hafnium is zircon, though a minor source is baddeleyite, mined only in Brazil. Zircon is an accessory mineral in igneous, metamorphic, and sedimentary rocks, but rarely occurs in hardrock in minable quantities. The principal sources of zircon are therefore alluvial deposits, which are mined in many countries of five continents. The principal commercial deposits in the United States are in Florida, though others exist elsewhere in the southeastern Coastal Plain. The evidence indicates that conditions for the accumulation of workable deposits of heavy minerals were more favorable during the interglacial stages of the Pleistocene epoch than during Recent time. Therefore detrital ores of large volume and high tenor are more likely to be found in the terrace deposits than along the present beaches. Other concentrations of heavy minerals, however, are possible at favored sites close to the Fall Line where the Tuscaloosa formation rests upon the crystalline rocks of the Piedmont province. A score of heavy and semiheavy minerals occur in the detrital deposits of Florida, but the principal salable minerals are ilmenite, leucoxene, rutile, and zircon, though monazite and staurolite are saved at some mining plants. Commercial deposits of heavy minerals are generally required to have a tenor of 4 percent, though ores with a lower tenor can be mined at a profit if the content of monazite is notably high. The percentages of zircon in the concentrates ranges from 10 to 16 percent, and in eastern Florida from 13 to 15 percent. Thus the tenor in zircon of the ore-bearing sands ranges from 0.4 to 0.6 percent. The content of hafnium in zircon is immaterial for many uses, but for some purposes very high or very low tenors in hafnium are required. Alluvial zircon cannot be separated into such varieties, which, if needed, must be obtained from sources in bedrock. It thus becomes necessary to determine the Hf : Zr ratios in zircon from many kinds of

Bulk and Interface Thermodynamics of Calcia-, and Yttria-doped Zirconia Ceramics: Nanograined Phase Stability

Science.gov (United States)

Drazin, John Walter

Calcia-, and yttria- doped zirconia powders and samples are essential systems in academia and industry due to their observed bulk polymorphism. Pure zirconia manifests as Baddeleyite, a monoclinic structured mineral with 7-fold coordination. This bulk form of zirconia has little application due to its asymmetry. Therefore dopants are added to the grain in-order to induce phase transitions to either a tetragonal or cubic polymorph with the incorporation of oxygen vacancies due to the dopant charge mis-match with the zirconia matrix. The cubic polymorph has cubic symmetry such that these samples see applications in solid oxide fuel cells (SOFCs) due to the high oxygen vacancy concentrations and high ionic mobility at elevated temperatures. The tetragonal polymorph has slight asymmetry in the c-axis compared to the a-axis such that the tetragonal samples have increased fracture toughness due to an impact induced phase transformation to a cubic structure. These ceramic systems have been extensively studied in academia and used in various industries, but with the advent of nanotechnology one can wonder whether smaller grain samples will see improved characteristics similar to their bulk grain counterparts. However, there is a lack of data and knowledge of these systems in the nano grained region which provides us with an opportunity to advance the theory in these systems. The polymorphism seen in the bulk grains samples is also seen in the nano-grained samples, but at slightly distinct dopant concentrations. The current theory hypothesizes that a surface excess, gamma (J/m 2), can be added to the Gibbs Free energy equation to account for the additional free energy of the nano-grain atoms. However, these surface energies have been difficult to measure and therefore thermodynamic data on these nano-grained samples have been sparse. Therefore, in this work, I will use a well established water adsorption microcalorimetry apparatus to measure the water coverage isotherms