AustriaAbstractThe new mineral adranosite-(Fe), ideally (NH4)4NaFe2(SO4)4Cl(OH)2, is the Fe3+-analogue of adranosite. It was found on a pyroclastic breccia in two different fumaroles at “La Fossa” crater of Vulcano, Aeolian Islands, Italy, and corresponds to an anthropogenic product previously observed in a burning coal dump at the Anna mine, near Aachen, Germany. The mineral is tetragonal, space group I41/acd (no. 142), with a = 18.261(2), c = 11.562(1) Å, V = 3855.5(7) Å3 (single-crystal data), and Z = 8. The six strongest reflections in the X-ray powder diffraction pattern are [dobs in Å(I)(hkl)]: 9.134(100)(020), 4.569(83)(040), 3.047(79)(152), 6.462(36)(220), 3.232(29)(251), and 2.891(11)(004). The average chemical composition of the holotype is (wt.%): Na2O 5.01, Fe2O3 15.77, Al2O3 5.11, K2O 0.82, (NH4)2O 15.76, SO3 50.96, Cl 3.71, H2O 2.75, –O≡Cl –0.84, total 99.05; the corresponding empirical formula is: [(NH4)3.89K0.11]Σ4.00Na1.04[Fe1.27Al0.64]Σ1.91S4.10O16.40Cl0.67(OH)1.96. Adranosite-(Fe) forms aggregates of pale yellow acicular crystals up to 1 mm in length, the most common forms most probably being {100}, {110}, and {111}. The measured density is 2.18(1) g/cm3, and the calculated density is 2.195 g/cm3. Adranosite-(Fe) is uniaxial (–) with ω = 1.58(1), ε = 1.57(1) (l = 589 nm). Using single-crystal X-ray diffraction data from the holotype, the structure was refined to a final R(F) = 0.0415 for 670 independent observed reflections [I > 2σ(I)]. Adranosite-(Fe) is isostructural with its Al-analogue adranosite and contains NaO4Cl2 square tetragonal bipyramids, linked through their opposite Cl corners and helicoidal chains with composition [FeO4(OH)2SO4]n, both extending along [001]. The framework resulting from the sharing of the sulfate ions between the different chains displays cages in which the nine-coordinated hydrogen-bonded NH4+ ions are hosted.

Photodetectors based on polycrystalline diamond (PCD) films are of great interest to many researchers for the attractive electronic, mechanical, optical and thermal properties. PCD films are grown using the Microwave Plasma Enhanced Chemical Vapor Deposition (MWPECVD) method. First, we characterized films by means of structural and morphological analysis (Raman spectroscopy and scanning electron microscopy), then we evaporated a pattern of coplanar interdigitated Cr/Au contacts with an inter-electrode spacing of 100 mu m in order to perform the electrical characterization. We carried out measurements of dark current and impedance spectroscopy to investigate the film properties and conduction mechanisms of films and the effects of post-growth treatments. Finally we developed a charge sensing pre-amplifier to read-out the signal produced by UV photons in the detector. (C) 2009 Elsevier B.V. All rights reserved.

A group of enamelled and gilded glass objects, coming from Melfi Castle (PZ - Italy) from an area dated to the period between the end of the 12th and the last quarter of the 13th century, offered the opportunity to closely investigate this technology with the aim of understanding the raw materials and the procedures employed to realize the objects and their precious decorations. Optical microscopy, scanning electron microscopy coupled with energy dispersive X-ray spectroscopy, Raman spectroscopy, laser ablation-inductively coupled plasma-mass spectrometry and X-Ray photoelectron spectroscopy were used to observe and analyze the glass, the enamels, the gildings and their mutual relations. The bulk of the objects resulted a soda-lime glass, while the enamels are lead-based 'soft' enamels or soda-lime glass; the palette of pigments employed to obtain their colours included iron III oxide and minium for red, lazurite and/or cobalt for blue, lead-tin-antimony pyrochlore solid solution oxide (yellow) plus cobalt for green, manganese oxides for black and calcium phosphate for white. Results obtained for gilding, in particular stratigraphy and morphology, suggest the use of the so called 'liquid gold'.

This paper presents the preliminary results of the recent excavations of the Early Neolithic site of Portonovo - Fosso Fontanaccia on the Conero promontory in the Marche. Here 16 domed ovens were found cut into the hillslope. Two of the ovens contain three burials, while the remains of a cremated female were found in an open area. This article presents the main features of the structures and burials, together with the preliminary results of anthropological, anthracological and archaeometrical analyses. The study of pottery and lithic production are in progress, as well as micromorphological, archaeozoological and palaeobotanical analyses.

The new mineral jakobssonite, ideally CaAlF5, was first found in crusts collected in 1988 from a fumarole on the Eldfell volcano, Heimaey Island, Iceland. It was subsequently found in similar crusts collected in 1991 from a fumarole on the Hekla volcano, Iceland. It is associated with leonardsenite (IMA2011-059), ralstonite, heklaite, anhydrite, gypsum, jarosite, hematite, opal and several fluoride minerals that have not been fully characterized. Jakobssonite occurs as soft white fragile crusts of acicular crystals <50 mm long. Its calculated density is 2.89 g cm-3. Chemical analyses by energy-dispersive spectrometry on a scanning electron microscope produced a mean elemental composition as follows: Ca, 18.99; Al, 18.55; Mg, 1.33; Na, 0.33; F, 50.20; O, 10.39; total 99.79 wt.%. The empirical chemical formula, calculated on the basis of 7 atoms per formula unit with all of the oxygen as OH, is (Ca0.73Mg0.09Na0.02)S0.84Al1.06F4.09(OH)1.01. Jakobssonite is monoclinic, space group C2/c, with a = 8.601(1), b = 6.2903(6), c = 7.2190(7) A ˚ , b = 114.61(1)o, V = 355.09(8) A ˚3 and Z = 4. The crystal structure contains chains of [AlF6] octahedra which run parallel to the c axis. These chains are interconnected by chains of [CaF7] pentagonal bipyramids. Jakobssonite is isostructural with several other CaMIIIF5 compounds. The eight strongest lines in the powder diffraction diagram [d in A ˚ (I) (hkl)] are as follows: 4.91 (18) (110), 3.92 (76) (200), 3.15 (68) (020), 3.13 (100) (11¯2¯ ), 2.27 (22) (22¯2¯ ), 1.957 (21) (400), 1.814 (20) (13¯2¯ ), 1.805 (22) (204¯ ). The chemical and crystal-structure analyses of jakobssonite are similar to synthetic CaAlF5 with minor substitutions of light elements (e.g. Na) or vacancies for Ca, and OH for F.

Leonardsenite (IMA2011-059), with ideal formula MgAlF5(H2O)2, is a new fumarole mineral from Eldfell volcano, Iceland. It has also been found in volcanic encrustations from the Hekla crater, Iceland. The mineral forms a soft and friable mass of white crystals up to 20 μm in length. The streak is white and the luster is earthy. The calculated density is 2.31 g cm–3. Leonardsenite is orthorhombic, space group Imma; the lattice parameters, obtained from Rietveld refinement of the XRPD data, are: a 7.055(1) Å, b 10.117(2) Å, c 6.813(1) Å, V 486.3(1) Å3, and Z = 4. The eight strongest reflections in the X-ray powder diffraction pattern are [d in Å (I) (hkl)]: 5.66 (100) (011), 4.92 (29) (101), 3.53 (27) (200), 3.03 (31) (031), 3.00 (38) (211), 2.30 (16) (231), 1.77 (19) (400), 1.76 (24) (242). Chemical analyses by energy-dispersive spectrometry using a scanning electron microscope produced a mean elemental composition as follows (wt.%): Mg 14.66, Al 16.16, F 52.98, O 15.88, H 1.78, total 101.46. The corresponding empirical formula, calculated on the basis of 2 cations pfu, is Mg1.00Al1.00[F4.64(OH)0.36]Σ5.00(H2O)1.29. On the basis of chemical analyses and X-ray diffraction data, leonardsenite corresponds to the synthetic compound MgAlF5(H2O)2. The crystal structure of leonardsenite contains infinite chains of [AlF6] octahedra along the c-axis which are connected via common fluorine atoms to isolated [MgF4(H2O)2] octahedra. Leonardsenite is the first aluminum fluoride hydrated mineral of the inverse weberite group with general formula MIIMIIIF5(H2O)2. Leonardsenite belongs to the group of fluorides with interesting optical and catalytic properties. The name of this new species honors Erik Leonardsen (1934–), the former leader of the X-Ray Diffraction Laboratory of the Geological Institute, University of Copenhagen. The mineral and its name have been approved by the IMA-CNMNC (IMA2011-059).

This study focuses on defining compositional and structural characteristics, identifying raw materials and production technology, and validating the archaeological hypothesis of a local production of thin-walled pottery (2nd cent. BC–3rd cent. AD) in the Vesuvian area. Samples investigated were analysed using OM, SEM-EDS, XRD and LA-ICPMS supported by a statistical multivariate treatment of the compositional data of the ceramic bodies. The results obtained show how an integrated approach of analytical techniques can provide answers to archaeological questions and also give a valuable insight into the exchange of raw materials and/or finished products between sites. The paper also discloses how a combined analytical methodology represents a positive step in answering the one question which remains unsolved concerning the entire ceramic production in the Vesuvian area: the provenance of the clayey raw materials used. Indeed, the massive pottery production in the Bay of Naples down the ages contrasts with the unavailability of the necessary clayey local resources.

Mastic incrustation sculptureswere used to decorate different types of objects by filling themarble incisionswith an impasto containing materials such as crushed pottery, glass or rock fragments, possibly in combination with organic substances, and was employed both in Byzantine and Occidental areas. From the 11th century onwards these sculptures are applied in important churches such as San Marco in Venice (Italy), but, despite their widespread use and conservation problems, the composition of these amalgams has never been thoroughly studied. Here we present the results of the examination of the mastic encrustations present on the medieval marble panels and precious cathedra in the San Nicola church of Bari (Italy). The matrixwas analysedwith Fourier transform infrared spectroscopy and pyrolysis gas chromatography-mass spectrometry. Organic binders were found and, in particular, the occurrence of heated Pinaceae resin, as well as of beeswaxwas assessed. The inclusions, including different types of rock, carbon black and opaque glass fragments,were characterised with opticalmicroscopy, scanning electronmicroscopy, and powderX-ray diffraction.Micro-Raman spectroscopywas carried out on both inclusions and matrix.

Sono stati sottoposti a determinazione di provenienza, in modo non distruttivo, gli unici tre reperti in ossidiana rinvenuti a Selva dei Muli (FR). Le analisi degli elementi maggiori mediante SEM-EDS e la determinazione delle intensità dei raggi X di alcuni elementi in traccia mediante FRX ha permesso di stabilire la fonte di approvvigionamento di due campioni di ossidiana da Lipari e di un terzo da Palmarola.

The X-ray fluorescence technique using peak intensity ratios of trace elements is one of the faster, less expensive and less invasive methods for obsidian sourcing. Moreover, XRF peak intensity ratios are particularly useful when the artifact is slightly altered, particularly affecting the alkali cations, or when its surfaces are covered with a fine film of carbonate deposits formed while the sample was buried. The limitation of this technique results from the dimensions of the obsidian samples: very small obsidian samples, nowadays about 1 cm in size, are difficult to measure given the very few X-rays emitted by their surface. An aluminium holder closed with a very thin Mylar© polyester film was prepared and the specimen, positioned at the centre of the surface of the Mylar film, was placed in the XRF spectrometer. The use of recent technology XRF apparatus equipped with a 4 kW Rh anode X-ray tube coupled with an accurate measurement of refined X-ray characteristic lines, that exclude the X-ray background contribution, of five trace elements (Rb, Sr, Y, Zr, Nb), made it possible to determine the source geological outcrop of archaeological obsidian samples as little as 7 mm and as light as 40 mg. A database of peak intensity ratios, background and interference free, of five trace elements was produced for obsidian samples from Monte Arci, Palmarola, Lipari, Pantelleria, Gyali and Melos. This database may be used by other laboratories provided the X-ray intensity of the trace elements Rb, Sr, Y, Zr, Nb are measured as net intensities, that is purified from the contribution of the background and from interelemental interferences. A comparison between data obtained with two spectrometers, of different generation and differently calibrated, confirmed the possibility of obtaining a database that can be shared with other laboratories. The proposed XRF method was tested on Neolithic obsidians from four Apulian sites (Ripa Tetta at Lucera, Palestra ex G.I.L. at Foggia, Pulo di Molfetta and Grotta di Santa Barbara at Polignano a Mare), whose source outcrops had been also determined by SEM-EDS.

Biological samples from 4 patients affected by carcinoma were investigated by SEM-EDS from a mineralogical point of view in order to ascertain presence of solid particles that could have caused their disease. Many dusty particles, in particular the silicatic ones, were foud; in particular there were recognized minerals as talc, biotite, amphiboles, pyroxene, olivine, wollastonite, feldspars, zircon, apatite, barite, and xenotime. Rare acicular fibre, likely amosite and chrysotile were observed only in the histological specimen of the patient that underwent surgery for colorectal cancer. These silicates, that are the causes of various and widespread pulmonary cancer, like the mesothelioma, seems to be strictly related also to colon carcinoma.

The two unique Early Neolithic obsidian bladelets found among the numerous ovens identified at the site of Portonovo (AN) were analysed. Non-destructive chemical analyses of the glass, by SEM-EDS and XRF, allowed the source rock region to be identified as the island of Lipari. As the bladelets are very fragile and thin, and present a pumice texture, the surfaces of the samples were protected with very thin aluminium foil before they were prepared and analysed with SEM-EDS. A sample holder closed at the bottom with a Mylar © film was used to allow the tiny specimens to be analysed by XRF. The provenance is then discussed in the context of the literature on obsidian provenance in Early to Late Neolithic sites in the middle Adriatic regions of the Marche and Abruzzo.

Viene proposto un modello di sonda orizzontale con tubo a U, di lunghezza finita in regime stazionario, usando il Metodo delle Sorgenti. Col Metodo delle Immagini si studia l’effetto della piccola profondità della sonda. Il modello permette di calcolare la differenza di temperatura del fluido tra entrata e uscita. Si discute l’influenza della resistenza di contatto nel caso di una sonda interrata in una trincea e quello di una sonda interrata mediante una perforazione orizzontale. HORIZONTAL STEADY STATE GEOTHERMAL PROBE OF FINITE LENGTH We propose a model of an U pipe of finite length in steady state regime by means of the Source Method. Moreover, we study the influence of the semi-infinite soil by the Images Method. The influence of the thermal contact resistance for the probe sited whitin a trench and that posed by the horizontal drilling is discussed.

The founding of lapis lazuli to give blue colour to glass and glazes is more and more coming out from the most recent studies of pottery and glassware of different epochs and provenances. The recent discovery in the south of Italy (Frederick II, Melfi castle) of enamelled glass pieces including blue enamels questioned the real nature of the blue colour raw materials because the castle is built over and not far from outcrops of two volcanic rocks – haüynophire and phonolite – that contain haüyne, mineral belonging to sodalite group as lazurite, that can be blue or become blue after heating. Raman microscopy and scanning electron microscopy coupled with energy dispersive X-ray spectroscopy were tested in order to identify the rock used as raw material and to understand if the chromophore-bearing mineral in the artefacts could be other than lazurite. To do this, the two volcanic rocks, lapis lazuli and archaeological glass with blue enamels, were studied. In particular, temperature-dependent Raman measurements and Raman mappings both on single lazurite and haüyne crystals and on the rocks and the enamels were carried out also in order to investigate the colouration mechanism of haüyne. The results obtained allowed to make hypotheses about the transformations occurring in haüyne with heating and about the procedures of distinguishing the raw materials.

Technological transformationsin the pottery production in the first half of the 4th millennium BC: archeometric data from Scanzano Cave, Masseria Stevanato and Parco San Nicola - This paper presents the results of characterisation analyses of 28 samples of Neolithic and Copper Age pottery from the site of Scanzano Cave and Masseria Stevanato (Bari) and Parco San Nicola (Rutigliano). Archaeometric analyses were performed at the Dipartimento di Scienze della Terra e Geoambientali of the University of Bari “Aldo Moro”. The samples are almost petrographically inhomogeneous and different potter fabrics can be distinguished from their composition and grain-size distribution. The existing relationships between the various sites and ceramic classes, their chronology and fabric are discussed. The analysis of mineral phases allowed distinguishing the various contributions to the NPIs between those of safe origin by Vulture volcanism, such as K-feldspars barium-rich and Ti-augitic pyroxenes and garnets, and those who have certainly source rocks of the Apennine slopes, such as pyrope or almandine rich garnets.