Pasquale Acquafredda

Eldfellite, NaFe(SO4)2, a new fumarolic mineral from Eldfell volcano, Iceland

Abstract A new mineral, eldfellite, was found among fumarolic encrustations collected in 1990 on the Eldfell volcano, Heimaey Island, Iceland. Associated minerals are ralstonite, anhydrite, gypsum, bassanite, hematite, opal and tamarugite, as well as a presumably new mineral with the composition Na3Fe(SO4)3. Along with opal and tamarugite, eldfellite forms soft and fragile aggregates built of thin, platy crystals of micrometre size. The mineral is yellowish-green to greenish-white, with a white streak. The calculated density is 3.062 g/cm3. Eldfellite is monoclinic, C2/m, a 8.043(4) Å, b 5.139(2) Å, c 7.115(4) Å, β 92.13(2)°, Vuc 293.9(2) Å3, Z = 2 and is isostructural with yavapaiite[KFe(SO4)2]. The strongest lines in the powder diffraction diagram are [d (Å), I (relative to 10)]: 3.72, 8; 3.64, 5; 3.43, 5; 2.77, 10; 2.72, 6; 2.57, 3; 2.370, 6; 1.650, 3. The chemical analysis and the X-ray diffraction data of eldfellite correspond to those of the synthetic compound NaFe(SO4)2.

Methodology of a combined approach: analytical techniques to identify the technology and raw materials used in thin-walled pottery from Herculaneum and Pompeii

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.

Heklaite, KNaSiF6, a new fumarolic mineral from Hekla volcano, Iceland

Abstract Heklaite, with the ideal formula KNaSiF6, was found among fumarolic encrustations collected in 1992 on the Hekla volcano, Iceland. Heklaite forms a fine-grained mass of micron- to sub-micron-sized crystals intimately associated with malladrite, hieratite and ralstonite. The mineral is colourless, transparent, non-fluorescent, has a vitreous lustre and a white streak. The calculated density is 2.69 g cm-3. An SEM-EDS quantitative chemical analysis shows the following range of concentrations (wt.%): Na 11.61-12.74 (average 11.98), K 17.02-18.97 (average 18.29), Si 13.48-14.17 (average 13.91), F 54.88-56.19 (average 55.66). The empirical chemical formula, calculated on the basis of 9 a.p.f.u., is Na1.07K0.96Si1.01F5.97. X-ray powder diffraction indicates that heklaite is orthorhombic, space group Pnma, with the following unit-cell parameters: a = 9.3387(7) Å, b = 5.5032(4) Å, c = 9.7957(8) Å, V = 503.43(7) Å3, Z = 4. The eight strongest reflections in the powder diffraction pattern [d in Å (I/I0) (hkl)] are: 4.33 (53) (102); 4.26 (56) (111); 3.40 (49) (112); 3.37 (47) (202); 3.34 (100) (211); 2.251 (27) (303); 2.050 (52) (123); 2.016 (29) (321). On the basis of chemical analyses and X-ray data, heklaite corresponds to the synthetic compound KNaSiF6. The name is for the type locality, the Hekla volcano, Iceland.

Jakobssonite, CaAlF5, a new mineral from fumaroles at the Eldfell and Hekla volcanoes, Iceland

Abstract 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 μm 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)S 0.84Al1.06F4.09(OH)1.01. Jakobssonite is monoclinic, space group C2/c, with a = 8.601(1), b = 6.2903(6), c = 7.2190(7) Å, β = 114.61(1)o, V = 355.09(8) Å3 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 CaMIII F5 compounds. The eight strongest lines in the powder diffraction diagram [d in Å (I) (hkl)] are as follows: 4.91 (18) (110), 3.92 (76) (200), 3.15 (68) (020), 3.13 (100) (11̅2̅), 2.27 (22) (22̅2̅), 1.957 (21) (400), 1.814 (20) (13̅2̅), 1.805 (22) (204̅). 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.

On the technical properties of the Carovigno stone from Apulia (Italy): physical characterization and decay effects by means of experimental ageing tests

Apulia (southern Italy) is typified by widespread outcrops of rocks exploited in the last centuries in historical architectures and religious constructions, as building and decorative stone. Today, as in the past, these stones represent an important source for region economy and prestige, due to their uses for modern works, restoration of local medieval churches and also exporting abroad. Among these, a noteworthy and still poorly known material is the Carovigno stone. In this paper, firstly an overall view on the, mineralogical and petrophysical features of the stone was reached through a multianalytical approach based on several investigation procedures and techniques, including ultrasonic test, X-ray diffractometry, scanning electron microscopy, optical microscopy, mercury intrusion porosimetry. In order to simulate decay phenomena, the Carovigno stone samples were processed to three different ageing tests: cycles of thermal treatments at different high temperatures, cycles of heating–cooling and cycles of exposure to decahydrate sodium sulphate and sodium chloride saline solutions. During and after each ageing processes, mineralogical transformations and petrophysical changes were evaluated. Results suggested that the Carovigno stone is a fine-grained calcarenite, pure or nearly pure, characterized by high porosity and, consequently, very notable thermal stress resistance. Conversely, the type and amount of porosity causes stone predisposition to salt crystallization decay.

Synergic analytical strategy to follow the technological evolution of Campanian medieval glazed pottery

Three classes of medieval lead-tin-glazed ceramics (protomajolica, transition enamel pottery and white enamel pottery), from the archaeological site of Castello del Monte in Montella (Avellino, southern Italy), were investigated. Inductively coupled plasma–mass spectrometry (ICP-MS), optical and scanning electron microscopy with energy-dispersive X-ray spectroscopy (OM and SEM-EDS) and X-ray powder diffraction (XRPD) were carried out on ceramic bodies, coatings and decorations in order to outline the technological features and define the nature of glazes and pigments. The aim of this work, in addition to delineating the features of production, is to confirm the archaeological hypothesis that transition enamel pottery produced between the fourteenth and fifteenth centuries, although having much in common with the protomajolica, is in fact a version of white enamel pottery, characterised by morphological and ornamental diversity. Our results show that both ceramic bodies and coatings feature different structural and compositional characteristics, linking the three ceramic classes and making it possible to confirm the archaeological hypothesis that transition enamel pottery can be defined as a ceramic class with transitional features between protomajolica and white enamel pottery.

Fumarolic Minerals: An Overview of Active European Volcanoes

The fumarolic mineralogy of the Icelandic active volcanoes, the Tyrrhenian volcanic belt (Italy) and the Aegean active arc (Greece) is investigated, and literature data surveyed in order to define the characteristics of the European fumarolic systems. They show broad diversity of mineral associations, with Vesuvius and Vulcano being also among the world localities richest in mineral species. Volcanic systems, which show recession over a longer period, show fumarolic development from the hightemperature alkaline halide/sulphate, calcic sulphate or sulphidic parageneses, synchronous with or immediately following the eruptions, through mediumtemperature ammonium minerals, metal chlorides, or fluoride associations to the late low-temperature paragenesis dominated by sulphur, gypsum, alunogen, and other hydrous sulphates. The situation can be different in the systems that are not recessing but show fluctuations in activity, illustrated by the example of Vulcano where the high-temperature association appears intermittently. A full survey of the mineral groups and species is given in respect to their importance and appearance in fumarolic associations.