Abstract
A variety of experimental techniques have been proposed to measure the composition of aqueous fluids in high-pressure experiments. In particular, the “diamond trap method,” where the fluid is sampled in the pore space of diamond powder and analyzed by laser-ablation ICP-MS after the experiment, has become a popular tool. Here, we carried out several tests to assess the reliability of this method. (1) We prepared several capsules loaded with fluid of known composition and analyzed the fluid by laser-ablation ICP-MS, either (a) after drying the diamond trap at ambient condition; (b) after freezing and subsequent freeze-drying; and (c) after freezing and by analyzing a frozen state. Of these methods, the analysis in the frozen state (c) was most accurate, while the results from the other two methods were poorly reproducible, and the averages sometimes deviated from the expected composition by more than a factor of 2. (2) We tested the reliability of the diamond trap method by using it to measure mineral solubilities in some well-studied systems at high pressure and high temperature in piston-cylinder runs. In the systems quartz-H2O, forsterite-enstatite-H2O, and albite-H2O, the results from analyzing the diamond trap in a frozen state by laser-ablation ICP-MS generally agreed well with the expected compositions according to literature data. However, in the systems corundum-H2O and rutile-H2O, the data from the analysis of the diamond trap were poorly reproducible and appeared to indicate much higher solubilities than expected. We attribute this not to some unreliability of the analytical method, but instead to the fact that in these systems, minor temperature gradients along the capsule may induce the dissolution and re-precipitation of material during the run, which causes a contamination of the diamond trap by solid phases. (3) We carried out several tests on the reliability of the diamond trap to measure fluid compositions and trace element partition coefficients in the eclogite-fluid system at 4 GPa and 800 °C using piston-cylinder experiments. The good agreement between “forward” and “reversed” experiments—with trace elements initially either doped in the solid starting material or the fluid—as well as the independence of partition coefficients on bulk concentrations suggests that the data obtained are reliable in most cases. We also show that the rate of quenching/cooling has little effect on the analytical results, that temperature oscillations during the run can be used to enhance grain growth, and that well-equilibrated samples can be obtained in conventional piston-cylinder runs. Overall, our results suggest that the diamond trap method combined with laser-ablation ICP-MS in frozen state yields reliable results accurate within a factor of two in most cases; however, the precipitation of accessory minerals in the diamond trap during the run may severely affect the data in some systems and may lead to a gross overestimation of fluid concentrations.
Acknowledgments and Funding
We thank M.P. Juriček for helping with some of the experiments. Constructive reviews by R.J. Bakker and an anonymous referee helped to improve the manuscript. This study was supported by the DFG International Research Training Group “Deep Volatile Cycles” (GRK 2156/1).
References cited
Aerts, M., Hack, A.C., Reusser, E., and Ulmer, P. (2010) Assessment of the diamond-trap method for studying high-pressure fluids and melts and an improved freezing stage design for laser ablation ICP-MS analysis. American Mineralogist, 95, 1523–1526.10.2138/am.2010.3356Search in Google Scholar
Anderson, G.M., and Burnham, C.W. (1965) Solubility of quartz in supercritical water. American Journal of Science, 263, 494–511.10.2475/ajs.263.6.494Search in Google Scholar
Antignano, A., and Manning, C.E. (2008) Rutile solubility in H2O, H2O-SiO2 and H2O-NaAlSi3O8 fluids at 0.7–2.0 GPa and 700–1000 °C: Implications for mobility of nominally insoluble elements. Chemical Geology, 255, 283–293.10.1016/j.chemgeo.2008.07.001Search in Google Scholar
Audétat, A., and Keppler, H. (2005) Solubility of rutile in subduction zone fluids, as determined by experiments in the hydrothermal diamond anvil cell. Earth and Planetary Science Letters, 232, 393–402.10.1016/j.epsl.2005.01.028Search in Google Scholar
Ayers, J.C., and Watson, E.B. (1993) Rutile solubility and mobility in supercritical aqueous fluids. Contributions to Mineralogy and Petrology, 114, 321–330.10.1007/BF01046535Search in Google Scholar
Bali, E., Audetat, A., and Keppler, H. (2011) The mobility of U and Th in subduction zone fluids: an indicator of oxygen fugacity and fluid salinity. Contributions to Mineralogy and Petrology, 161, 597–613.10.1007/s00410-010-0552-9Search in Google Scholar
Bali, E., Keppler, H., and Audetat, A. (2012) The mobility of W and Mo in subduction zone fluids and the Mo-W-Th-U systematics of island arc magmas. Earth and Planetary Science Letters, 351, 195–207.10.1016/j.epsl.2012.07.032Search in Google Scholar
Bernini, D., Audetat, A., Dolejs, D., and Keppler, H. (2013) Zircon solubility in aqueous fluids at high temperatures and pressures. Geochimica et Cosmochimica Acta, 119, 178–187.10.1016/j.gca.2013.05.018Search in Google Scholar
da Silva, M.M., Holtz, F., and Namur, O. (2017) Crystallization experiments in rhyolitic systems: The effect of temperature cycling and starting material on crystal size distribution. American Mineralogist, 102, 2284–2294.10.2138/am-2017-5981Search in Google Scholar
Fournier, R.O., and Potter, R.W. (1982) An equation correlating the solubility of quartz in water from 25 °C to 900 °C at pressures up to 10,000 bars. Geochimica et Cosmochimica Acta, 46, 1969–1973.10.1016/0016-7037(82)90135-1Search in Google Scholar
Jochum, K.P., Weis, U., Stoll, B., Kuzmin, D., Yang, Q.C., Raczek, I., Jacob, D.E., Stracke, A., Birbaum, K., Frick, D.A., Gunther, D., and Enzweiler, J. (2011) Determination of reference values for NIST SRM 610–617 glasses following ISO guidelines. Geostandards and Geoanalytical Research, 35, 397–429.10.1111/j.1751-908X.2011.00120.xSearch in Google Scholar
Johnson, M.C., and Plank, T. (1999) Dehydration and melting experiments constrain the fate of subducted sediments. Geochemistry, Geophysics, Geosystems, 1, 1007.10.1029/1999GC000014Search in Google Scholar
Kawamoto, T., Yoshikawa, M., Kumagai, Y., Mirabueno, M.H.T., Okuno, M., and Kobayashi, T. (2013) Mantle wedge infiltrated with saline fluids from dehydration and decarbonation of subducting slab. Proceedings of the National Academy of Sciences, 110, 9663–9668.10.1073/pnas.1302040110Search in Google Scholar
Kelley, K.A., and Cottrell, E. (2009) Water and the oxidation state of subduction zone magmas. Science, 325, 605–607.10.1126/science.1174156Search in Google Scholar
Keppler, H. (2017) Fluids and trace element transport in subduction zones. American Mineralogist, 102, 5–20.10.2138/am-2017-5716Search in Google Scholar
Kessel, R., Ulmer, P., Pettke, T., Schmidt, M.W., and Thompson, A.B. (2004) A novel approach to determine high-pressure high-temperature fluid and melt compositions using diamond-trap experiments. American Mineralogist, 89, 1078–1086.10.2138/am-2004-0720Search in Google Scholar
Kessel, R., Schmidt, M.W., Ulmer, P., and Pettke, T. (2005a) Trace element signature of subduction-zone fluids, melts and supercritical liquids at 120–180 km depth. Nature, 437, 724–727.10.1038/nature03971Search in Google Scholar
Kessel, R., Ulmer, P., Pettke, T., Schmidt, M.W., and Thompson, A.B. (2005b) The water-basalt system at 4 to 6 GPa: Phase relations and second critical endpoint in a K-free eclogite at 700 to 1400 °C. Earth and Planetary Science Letters, 237, 873–892.10.1016/j.epsl.2005.06.018Search in Google Scholar
Manning, C.E. (1994) The solubility of quartz in H2O in the lower crust and upper mantle. Geochimica et Cosmochimica Acta, 58, 4831–4839.10.1016/0016-7037(94)90214-3Search in Google Scholar
Manning, C.E. (2004) The chemistry of subduction zone fluids. Earth and Planetary Science Letters, 223, 1–16.10.1016/j.epsl.2004.04.030Search in Google Scholar
Newton, R.C., and Manning, C.E. (2002) Solubility of enstatite + forsterite in H2O at deep crust/upper mantle conditions: 4 to 15 kbar and 700 to 900 °C. Geochimica et Cosmochimica Acta, 66, 4165–4176.10.1016/S0016-7037(02)00998-5Search in Google Scholar
Potter, J.M., Pohl, D.C., and Rimstidt, J.D. (1987) Fluid flow systems for kinetic and solubility studies. In G.C. Ulmer and H.L. Barnes, Eds., Hydrothermal Experimental Techniques, p. 240–260. Wiley.Search in Google Scholar
Ragnarsdóttir, K.V., and Walther, J.V. (1985) Experimental determination of corundum solubilities in pure water between 400–700 °C and 1–3 kbar. Geochimica et Cosmochimica Acta, 49, 2109–2115.10.1016/0016-7037(85)90068-7Search in Google Scholar
Rustioni, G., Audétat, A., and Keppler, H. (2019) Experimental evidence for fluid-induced melting in subduction zones. Geochemical Perspectives Letters, 11, 49–54.10.7185/geochemlet.1925Search in Google Scholar
Ryabchikov, I.D., and Boettcher, A.L. (1980) Experimental evidence at high pressure for potassic metasomatism in the mantle of the Earth. American Mineralogist, 65, 915–919.Search in Google Scholar
Ryabchikov, I.D., Orlova, G.P., Kalenchuk, G.Y., Ganeyev, I.I., Udovkina, N.G., and Nosik, L.P. (1989) Reactions of spinel lherzolite with H2O-CO2 fluids at 20 kbar and 900 °C. Geochemistry International, 26, 56–62.Search in Google Scholar
Schmidt, M.W., and Ulmer, P. (2004) A rocking multianvil: elimination of chemical segregation in fluid-saturated high-pressure experiments. Geochimica et Cosmochimica Acta, 68, 1889–1899.10.1016/j.gca.2003.10.031Search in Google Scholar
Shen, A.H., and Keppler, H. (1997) Direct observation of complete miscibility the albite-H2O system. Nature, 385, 710–712.10.1038/385710a0Search in Google Scholar
Seo, J.H., Guillong, M., Aerts, M., Zajacz, Z., and Heinrich, C.A. (2011) Microanalysis of S, Cl, and Br in fluid inclusions by LA-ICP-MS. Chemical Geology, 284, 35–44.10.1016/j.chemgeo.2011.02.003Search in Google Scholar
Stalder, R., Foley, S.F., Brey, G.P., and Horn, I. (1998) Mineral aqueous fluid partitioning of trace elements at 900–1200 °C and 3.0–5.7 GPa: New experimental data for garnet, clinopyroxene, and rutile, and implications for mantle metasomatism. Geochimica et Cosmochimica Acta, 62 (10), 1781–1801.10.1016/S0016-7037(98)00101-XSearch in Google Scholar
Tatsumi, Y. (1989) Migration of fluid phases and genesis of basalt magmas in subduction zones. Journal of Geophysical Research, 94, 4697–4707.10.1029/JB094iB04p04697Search in Google Scholar
Tropper, P., and Manning, C.E. (2005) Very low solubility of rutile in H2O at high pressure and temperature, and its implications for Ti mobility in subduction zones. American Mineralogist, 90, 502–505.10.2138/am.2005.1806Search in Google Scholar
Tropper, P., and Manning, C.E. (2007) The solubility of corundum in H2O at high pressure and temperature and its implications for Al mobility in the deep crust and upper mantle. Chemical Geology, 240, 54–60.10.1016/j.chemgeo.2007.01.012Search in Google Scholar
Tsay, A., Zajacz, Z., and Sanchez-Valle, C. (2014) Efficient mobilization and fractionation of rare-earth elements by aqueous fluids upon slab dehydration. Earth and Planetary Science Letters, 398, 101–112.10.1016/j.epsl.2014.04.042Search in Google Scholar
Walther, J.V. (1997) Experimental determination and interpretation of the solubility of corundum in H2O between 350 and 600 °C from 0.5 to 2.2 kbar. Geochimica et Cosmochimica Acta, 61, 4955–4964.10.1016/S0016-7037(97)00282-2Search in Google Scholar
Weiss, Y., McNeill, J., Pearson, D.G., Nowell, G.M., and Ottley, C.J. (2015) Highly saline fluids from a subducting slab as the source for fluid-rich diamonds. Nature, 524, 339–342.10.1038/nature14857Search in Google Scholar PubMed
Wilke, M., Schmidt, C., Dubrail, J., Appel, K., Borchert, M., Kvashnina, K., and Manning, C.E. (2012) Zircon solubility and zirconium complexation in H2O+Na2O+SiO2±Al2O3 fluids at high pressure and temperature. Earth and Planetary Science Letters, 349, 15–25.10.1016/j.epsl.2012.06.054Search in Google Scholar
Zarei, A., Klumbach, S., and Keppler, H. (2018) The relative Raman scattering cross sections of H2O and D2O, with implications for in situ studies of isotope fractionation. ACS Earth and Space Chemistry, 2, 925–934.10.1021/acsearthspacechem.8b00078Search in Google Scholar
© 2021 Walter de Gruyter GmbH, Berlin/Boston
Articles in the same Issue
- P-V-T equation of state of hydrous phase A up to 10.5 GPa
- Elastic properties and structures of pyrope glass under high pressures
- Effects of pH and Ca exchange on the structure and redox state of synthetic Na-birnessite
- A systematic assessment of the diamond trap method for measuring fluid compositions in high-pressure experiments
- Origin, properties, and structure of breyite: The second most abundant mineral inclusion in super-deep diamonds
- Why Tolbachik diamonds cannot be natural
- Deciphering the enigmatic origin of Guyana’s diamonds
- Precipitation of low-temperature disordered dolomite induced by extracellular polymeric substances of methanogenic Archaea Methanosarcina barkeri: Implications for sedimentary dolomite formation
- Atomic-scale characterization of commensurate and incommensurate vacancy superstructures in natural pyrrhotites
- Three-dimensional and microstructural fingerprinting of gold nanoparticles at fluid-mineral interfaces
- Seaborgite, LiNa6K2(UO2)(SO4)5(SO3OH)(H2O), the first uranyl mineral containing lithium
- Reheating and magma mixing recorded by zircon and quartz from high-silica rhyolite in the Coqen region, southern Tibet
- Crystal chemistry and thermal behavior of Fe-carpholite from the Pollino Massif, southern Italy
- New insights into the control of visible gold fineness and deposition: A case study of the Sanshandao gold deposit, Jiaodong, China
- A comment on “An evolutionary system of mineralogy: Proposal for a classification of planetary materials based on natural kind clustering”
- Reply to “A comment on ‘An evolutionary system of mineralogy: Proposal for a classification of planetary materials based on natural kind clustering’”
- New Mineral Names
Articles in the same Issue
- P-V-T equation of state of hydrous phase A up to 10.5 GPa
- Elastic properties and structures of pyrope glass under high pressures
- Effects of pH and Ca exchange on the structure and redox state of synthetic Na-birnessite
- A systematic assessment of the diamond trap method for measuring fluid compositions in high-pressure experiments
- Origin, properties, and structure of breyite: The second most abundant mineral inclusion in super-deep diamonds
- Why Tolbachik diamonds cannot be natural
- Deciphering the enigmatic origin of Guyana’s diamonds
- Precipitation of low-temperature disordered dolomite induced by extracellular polymeric substances of methanogenic Archaea Methanosarcina barkeri: Implications for sedimentary dolomite formation
- Atomic-scale characterization of commensurate and incommensurate vacancy superstructures in natural pyrrhotites
- Three-dimensional and microstructural fingerprinting of gold nanoparticles at fluid-mineral interfaces
- Seaborgite, LiNa6K2(UO2)(SO4)5(SO3OH)(H2O), the first uranyl mineral containing lithium
- Reheating and magma mixing recorded by zircon and quartz from high-silica rhyolite in the Coqen region, southern Tibet
- Crystal chemistry and thermal behavior of Fe-carpholite from the Pollino Massif, southern Italy
- New insights into the control of visible gold fineness and deposition: A case study of the Sanshandao gold deposit, Jiaodong, China
- A comment on “An evolutionary system of mineralogy: Proposal for a classification of planetary materials based on natural kind clustering”
- Reply to “A comment on ‘An evolutionary system of mineralogy: Proposal for a classification of planetary materials based on natural kind clustering’”
- New Mineral Names