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Laboratory of Experimental Mineralogy and Petrology

The laboratory is in the Florence Unit of the IGG.
Laboratory simulation of the P/T conditions present in the Earth's crust and upper mantle is important because it allows us to better understand some of the key geological processes, such as the generation and evolution of magma, the formation and growth of minerals, and the interaction between fluids and rocks in various geological contexts, such as geothermal areas or the Earth's mantle (metasomatism).

The Laboratory

Mineralogy, Petrology, and Experimental Geochemistry allow us to simulate the typical processes of these geodynamic environments in the laboratory through experiments conducted both with natural materials and simplified synthetic systems, using solid and/or fluid phases. These experiments may also be of interest to the field of Materials Science, as they enable the synthesis of materials with high technological and economic potential.

Left: Garnets and clinopyroxenes synthesized with the piston-cylinder from a mixture of oxides and carbonates at 2.5 GPa and 1400°C. Right: Gold capsule used in hydrothermal autoclave experiments.
Left: Growth edge formed during an experiment in a clinopyroxene from a lava from Etna (1180 °C, 0.1 MPa). Right: Welding of an “S” thermocouple using an arc welder with a graphite electrode.

Instruments

The laboratory is equipped with:

  • Chamber furnaces (Carbolite ELF 10/14, CSF 1200 and CWF 1200) reaching 1200°C and horizontal tubular furnace (Carbolite STF 15/50/450) up to 1500°C equipped with a quenching device;
  • Deltech DT-31(T< 1700°C) vertical furnace specially modified to a) achieve rapid cooling (quenching) of the sample and b) control the oxygen fugacity during the experiment by means of a gas mixture (CO and CO2) flowed through the furnace;
  • Parr Mod. 5500 stirred microreactor specifically designed for fluid/rock interaction experiments (use: P < 20 MPa, T< 350°C);
  • Externally heated autoclave (Leco Corp., model HR-2B-2) to simulate upper crust PT conditions (P< 0.4 GPa, T < 900°C).
  • Piston cylinder (Psika) to simulate upper mantle PT conditions (P<3 GPa, T<1700°C).
  • Buchi Novoclave reactor (200 ml capacity) operating at up to 500 bar and 400 °C, equipped with a magnetic stirrer. Special valves allow for in situ gas and/or liquid samples to be taken during experiments.
  • Various service equipment: analytical balance (0.0001 g), arc welder, binocular microscope, dryer, IR lamp, etc.).
From left to right: Quenching tray in the vertical furnace; Cylinder piston; Stirred microreactor.

Staff and Contacts

Dr. Andrea Orlando, (CNR Researcher – Manager)
Dr. Daniele Borrini (DST Researcher UniFI – Manager)

Phones

+39 055 2757510 (Dr. Andrea Orlando)
+39 055 2757560 (Laboratory)


E-mail:

andrea.orlando@cnr.it
daniele.borrini@unifi.it

Methods and Applications

The methods vary depending on the instrumentation used and the experiment being performed. The experiments have applications in igneous and metamorphic petrology, geothermal science, mineralogy, materials science, archaeometry, etc.


Vertical Oven:
The sample can be suspended from a Pt wire loop, which is in turn attached to two electrodes. At the end of the experiment, the current flowing through the electrodes causes the sample to fall into the quenching tank. Oxygen fugacity during the experiment can be monitored and measured externally.

Vertical furnace (left), and glass samples on loops obtained at the end of an experiment on a lava at 1500°C (right).

Stirred Microreactor

Solid and fluid material in a 25 ml container, stirring by magnetic stirrer, possibility of sampling the fluid during the experiment

Hydrothermal Autoclave:
The sample, placed in a gold capsule, is inserted into a reactor heated by an external oven. Temperature is controlled and measured by K-type thermocouples. The oven allows for a controlled temperature gradient to be established along the reactor.

Hydrothermal autoclave (left) and detail of the reactor with the oven (right).

Piston-Cylinder
The sample in a Pt capsule is placed together with other material (assembly) in a tungsten carbide cylinder and is compressed by a 0.5-inch piston that is pushed into the chamber by a 75-ton press. The Pt medium is solid (NaCl), and the temperature is measured by an S thermocouple.

Piston Assembly – Cylinder with the capsule in the central part (in white).
Some constituents of the assembly.

Scientific Projects and Interests

The laboratory has been actively used in several scientific projects, including:

  • PNRA-PEA 2004 to simulate the infiltration of alkali silicate melts into lherzolitic rocks, similar to what occurs in nature in the Mt. Melbourne volcanic province (Antarctica)
  • COFIN 2004 in which experiments allowed to determine the growth rate of minerals in silicate melts
  • Spontaneous free-topic research focused on the geothermal system of Mount Amiata, an interesting natural analogue for the study of mineral carbonation processes due to water-gas-rock interaction.
  • Zebu Project (Zero Emission Use of Methane-Poor Biogas by Mineral Carbonation), financed through the POR FESR 2007 – 2013, regional call (Tuscany Region) 2008, in which mineral carbonation in serpentinite rocks was studied
  • PRIN “Geochemistry and Fluid Dynamics in high pCO2systems ” in which water-gas-rock interactions were studied in high pCO2 conditions
  • Informal IGG-UniPr-Inaf-UniFi project on the synthesis of plagioclases containing Fe2+ to better interpret the reflectance spectra of celestial bodies
  • Aithale project of archaeometric scope, in which laboratory experiments had the aim of replicating the reduction processes of Elban hematite used in ancient times
  • Integrated Methods for Advanced Geothermal Exploration (IMAGE) project with tourmaline synthesis and fluid inclusions
  • Project H2020 GEMEx, Cooperation in Geothermal energy research Europe-Mexico for development of Enhanced Geothermal Systems and Superhot Geothermal Systems
  • H2020 GECO Project. GEothermal Emission Control
Tourmalines synthesized within the IMAGE project (left) and mineral carbonation evidenced by XRD spectra in experiments performed at different solid/fluid ratios at 30 MPa and 300°C (right).
SEM image of a siderite crystal from a phyllite from Mt Amiata whose decomposition at 300°C forms magnetite, CO, CO2, H2 and hydrocarbons (left), and planes of synthetic fluid inclusions formed at 400°C on pre-fractured quartz crystals (right).

Publications

  • Orlando A., Conticelli S., Armienti P. & Borrini D. (2000) – “Experimental study on a basanite from McMurdo Volcanic Group, Antarctica: inference on its mantle source”. Antarctic Science, 12, 105-116.
  • Orlando A., Thibault Y. & Edgar A.D. (2000) – “Experimental study of the K2ZrSi3O9 (wadeite)-K2TiSi3O9 and K2(Zr,Ti)Si3O9-phlogopite systems at 2-3 GPa”. Contrib. Mineral. Petrol., 139, 136-145.
  • Orlando A. & Borrini D. (2001) – “Solubility of Ti in andradite under upper mantle conditions: preliminary results”. Periodico di Mineralogia, 70, 99-110.
  • Orlando A. & Borrini D. (2003)- “Synthesis of pyrope – grossular garnets: an experimental study at P=2.5 GPa”. Mineral. and Petrol., 78, 37-51.
  • Orlando A. & Borrini D. (2006): “High temperature gas-mixing furnace: experimental set up and applications to Earth Sciences”. Periodico di Mineralogia, 75, 233-240.
  • Orlando A., Abebe T., Manetti P., Santo A.P. & Corti G. (2006)- “ Petrology of mantle xenoliths from Megado and Dilo, Kenya Rift, Southern Ethiopia. Ofioliti, 31, 67-83.
  • Perinelli C., Orlando A., Conte A.M., Armienti P., Borrini D., Faccini B. & Misiti V. (2008)- “Metasomatism induced by alcaline magma in the upper mantle of northern Victoria Land (Antartcica): an experimental approach”. From: Coltorti M. & Grègoire M. (eds) Metasomatism in Oceanic and Continental Lithospheric Mantle, Geological Society, London, Special publications, 293, 279-302.
  • Orlando A., D’Orazio M., Armienti P. & Borrini D. (2008)- “Experimental determination of plagioclase and clinopyroxene crystal growth rates in an anhydrous trachybasalt from Mt Etna (Italy)”. European Journal of Mineralogy, 20, 653-664.
  • Orlando A., Conte A.M., Borrini D., Perinelli C., Gianelli G. & Tassi F. (2010)- “Experimental investigation of CO2-rich fluids production in a geothermal area: the Mt Amiata (Tuscany, Italy) case study”. Chemical Geology, 274, 177-186.
  • Orlando A., Borrini D. & Marini L. (2011)- “Dissolution and carbonation of a serpentinite: Inferences from acid attack and high P–T experiments performed in aqueous solutions at variable salinity”. Applied Geochemistry, 26, 1569-1583.
  • Orlando A., Lelli M. & Marini L. (2012)- “Production of amorphous hydrated impure magnesium carbonate through ex situ carbonation”. Applied Geochemistry, 27, 2500-2510.
  • Manca R., Pagliantini L., Pecchioni E., Santo A.P., Cambi F., Chiarantini L., Corretti A., Costagliola P., Orlando A. & Benvenuti M. (2016)- “The island of Elba (Tuscany, Italy) at the crossroads of ancient trade routes: an archaeometric investigation of dolia defossa from the archaeological site of San Giovanni. Mineralogy and Petrology, 110, 693-711, DOI 10.1007/s00710-016-0438-2.
  • Benvenuti M., Orlando A., Borrini D, Chiarantini L., Costagliola P., Mazzotta C. & Rimondi V. (2016)-“ Experimental smelting of iron ores from Elba Island (Tuscany, Italy): results and implications for the reconstruction of ancient metallurgical processes and iron provenance. Journal of Archaeological Science, 70, 1-14.
  • Hernández-Rodríguez A., Montegrossi G., Orlando A., Huet B., Virgili G., Vaselli O., Agnelli M., Venturi S. & Marini L. (2017)- “Experimental analysis of the reaction rate of hydrated Class G cement powder at 11 bar PCO2 and ambient temperature. Procedia Earth and Planetary Science, 17, 889-892.
  • Orlando A., Ruggieri G., Chiarantini L., Montegrossi G. & Rimondi V. (2017) – “Experimental investigation of Biotite-rich schist reacting with B-bearing fluids at upper crustal conditions and correlated tourmaline formation”. Minerals, 7, 155, 1-23, DOI:10.3390/min7090155.
  • Carli C., Orlando A., Borrini D., Serventi G., Pratesi G., Sgavetti M. (2018) – “Synthetic plagioclases as support for future “in-situ” missions: iron’s influence on VNIR reflectance”. 2018 5th IEEE International Workshop on Metrology for AeroSpace (MetroAeroSpace), Volume 2018, 140-145.
  • Hernàndez-Rodrìguez A., Orlando A., Montegrossi G., Huet B., Virgili B., Vaselli O. (2021) – “ Experimental analysis on the carbonation rate of Portland cement at room temperature and CO2 partial pressure from 1 to 51 bar”. Cement and Concrete Composites, 124- 104271, 11 pp.
  • Ercoli R., Orlando A., Borrini D., Tassi F., Bicocchi G., Renzulli A. (2021) – “Hydrogen-rich gas produced by the chemical neutralization of reactive by-products from the screening processes of the secondary Aluminum industry”. Sustainability, 13, 12261, 17pp, https://doi.org/10.3390/su132112261.