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A systematic assessment of the diamond trap method for measuring fluid compositions in high-pressure experiments

  • Greta Rustioni , Andreas Audétat and Hans Keppler EMAIL logo
Published/Copyright: December 31, 2020
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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

Received: 2020-01-29
Accepted: 2020-05-22
Published Online: 2020-12-31
Published in Print: 2021-01-27

© 2021 Walter de Gruyter GmbH, Berlin/Boston

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