Analytical Methods

Analytical Methods for H in Minerals

Updated 3-Jul-2023 by GR Rossman

1950s

Bigeleisen K, Perlman ML, Prosse HC (1952) Conversion of Hydrogenic Materials to Hydrogen for Isotopic Analysis. Analytical Chemistry 24, 1356-1357.
Nakamoto K, Margoshes M, Rujndle RE (1955) Stretching Frequencies as a Function of Distances in Hydrogen Bonds. Journal of the American Chemical Society 77, 6480-6486.

1960s

Bellamy LJ, Owen AJ (1969) A simple relationship between the infra-red stretching frequencies and the hydrogen bond distances in crystals. Spectrochimica Acta, Part A (Molecular Spectroscopy) 25A, 329-33.

1970s

Leich DA, Tombrello TA (1973) A technique for measuring hydrogen concentrations versus depth in solid samples. Nuclear Instruments and Methods 108, 67-71.
Hinthorne JR, Andersen CA (1975) Microanalysis for fluorine and hydrogen in silicates with the ion microprobe mass analyzer. American Mineralogist 60, 143-147.
Lanford WA, Trautvetter HP, Ziegler JF, Keller J (1976) New precision technique for measiuring the concentration versus depth of hydrogen in solids. Applied Physics Letters 28, 566-568.
Ligeon E, Guivarch A (1974) A new utilisation of ¹¹B ion beams: hydrogen analysis by ¹H(¹¹B,α)α,α nuclear reaction. Radiation Effects 22, 101-105.
Tsong IST, McLaren AC, Hobbs B (1976) Determnatino of hydrogen in silicates using the ion beam spectrochemical analyzer: applilcation to hydrolytic weaking. American Mineralogist 61, 921-926.

1980s

McLaren AC, Payling R (1980) The determination of hydrogen concentration in silicates using ion-beam spectrochemical analysis (IBSCA). Physics and Chemistry of Minerals 5, 315-326.
Moze O, Hicks TJ, McLaren, AC (1980) Determination of the hydrogen content of synthetic quartz by neutron polarization analysis. Physics and Chemistry of Minerals, 5(4), 309-14.
Paterson MS (1982) The determination of hydroxyl by infrared absorption in quartz, silicate glasses and similar materials. Bull Mineral 105, 20-29.
Aines RD, Rossman GR (1984) The hydrous component in garnets. Pyraspites. American Mineralogist , 69, 1116-1126.
Mikkenda W (1986) Stretching frerquency versus bond distance correlation of O-D(H)...Y (Y=N,O,S,Se,Cl,Br, I) hydrogen bonds in solid dydrates. Journal of Molecular Structure 147, 1-15.
Xiong F, Rauch F, Shi C, Zhou Z, Livi RP, Tombrello TA (1987) Hydrogen depth profiling in solids: a comparison of several resonant nuclear reaction techniques. Nuclear Instruments and Methods in Physics Research B27, 432-441.
Rossman GR, Rauch F, Livi R, Tombrello TA, Shi CR, Zhou ZY (1988) Nuclear analysis of hydrogen in almandine, pyrope, and spessartite garnets. Neues Jahrbuch für Mineralogie, Monatshefte 1988, 172-178.
Yesinowski JP, Eckert H, Rossman GR (1988) High-speed proton MAS-NMR of minerals. Journal of the American Chemical Society 110, 1367-1375.
Yurimoto H, Kurosawa M, Sueno S (1989) Hydrogen analysis in quartz crystals and quartz glasses by secondary ion mass spectrometry. Geochimica et Cosmochimica Acta 53:751-755.

1990s

Rossman GR (1990) Hydrogen in "anhydrous" minerals. Nuclear Instruments and Methods in Research B45, 41-44.
Kurosawa M, Yurimoto H, Matsumoto K, Sueno S (1992) Hydrogen analysis of mantle olivine by secondary ion mass spectrometry. In: Syono, Manghnani MH (eds) High-Pressure Research in Mineral Physics: Application to Earth and Planetary Sciences. pp. 283–287. Terra Pub-Am Geophys Union, Tokyo/Washington DC.
Kurosawa M, Yurimoto H, Matsumoto K, Sueno S (1992) Quantitative analysis of H, Ca and Ni in olivine by secondary ion mass spectrometry. Annual Report of the Institute of Geosciences University of Tsukuba 18, 83–89.
Fujimoto K, Fukutani K, Tsunoda M, Yamashita H, Kobayashi K (1993) Hydrogen depth profiling using ¹H(¹⁵N,alpha-gamma)¹²C resonant nuclear reaction on water-treated olivine surfaces and characterization of hydrogen species. Geochemical Journal 27, 155-162.
Bell DR, Ihinger PD, Rossman GR (1995) Quantitative analysis of hydroxyl in garnet and pyroxene. American Mineralogist 80, 465-474.
Sie SH, Suter GF, Chekhmir A, Green TH (1995) Microbeam recoil detection for the study of hydration of minerals. Nuclear Instruments and Methods in Physics Research Section B: Beam Interactions with Materials and Atoms 104, 261-265.
Libowitzky E, Rossman GR (1996) Principles of quantitative absorbance measurements in anisotropic crystals. Physics and Chemistry of Minerals 23, 319 -327.
Mikenda W, Steinböck S (1996) Stretching frequency vs. bond distance correlation of hydrogen bonds in solid hydrates: a generalized correlation function. Jourmal of Molecular Structure 384, 159–163.
Sweeney RJ, Prozesky VM, Springhorn KA (1997) Use of the elastic recoil detection analysis (ERDA) microbeam technique for the quantitative determination of hydrogen in materials and hydrogen partitioning between olivine and melt at high pressures - Geochimica et Cosmochimica Acta 61, 101-113.
Libowitzky E, Rossman GR (1997) An IR absorption calibration for water in minerals - American Mineralogist 82, 1111–1115.
Nakashima Y, Nakashima S, Gross D, Weiss K, Yamauchi K (1998) NMR imaging of ¹H in hydrous minerals. Geothermics 27, 43-53.
Libowitzky E (1999) Correlation of O-H Stretching Frequencies and O-H···O Hydrogen Bond Lengths in Minerals. Monatshefte für Chemie 130, 1047-1059.

2000-2004

Keppler H, Rauch M (2000) Water solubility in nominally anhydrous minerals measured by FTIR and ¹H MAS NMR: the effect of sample preparation. Physics and Chemistry of Minerals 27. 371-376.
Dyar MD, Wiedenbeck M, Robertson D, Cross LR, Delaney JS, Ferguson K, Francis CA, Grew ES, Guidotti CV, Hervig RL, Hughes JM, Husler J, Leeman W, McGuire AV, Rhede D, Rothe H, Paul RL, Richards I, Yates M (2001) Reference Minera ls for the Microa na lysis of Light Elements. The Journal of Geostandards and Geoanalysis 25, 451-463.
Eiler JM, Kitchen N (2001) Hydrogen-isotope analysis of nanomole (picoliter) quantities of H₂O. Geochimica et Cosmochimica Acta 65, 4467– 4479.
Furuno K, Komatsubara T, Sasa K, Oshima H, Yamato Y, Ishii S, Kimura H, Kurosawa M (2003) Measurement of hydrogen concentration in thick mineral or rack samples. Nuclear Instruments and Methods in Physics Research B 210, 459-463.
Koga K, Hauri E, Hirschmann M, Bell D (2003) Hydrogen concentration analyses using SIMS and FTIR: Comparison and calibration for nominally anhydrous minerals. Geochemistry Geophysics Geosysems 4, 1019 doi:10.1029/2002GC000378
Sasa K, Furuno K, Yamato Y, Ohshima H, Ishii S, Komatsubara T, Kurosawa M (2003) The Tsukuba high-energy nuclear microprobe for hydrogen analysis of mineral samples. Nuclear Instruments and Methods in Physics Research B 210, 48-53.
Aubaud C, Hauri EH, Hirschmann MM (2004) Hydrogen partition coefficients between nominally anhydrous minerals and basaltic melts. Geophysical Resarch Letters 31, L20611.
Lathe C, Koch-Müller M, Wirth R, Westrenen WV, Mueller HJ, Schilling F, Lauterjung J (2004) The influence of OH in coesite on the kinetics of the coesite-quartz phase transition. American Mineralogist 90, 36-43.
Ryan CG (2004) Ion beam microanalysis in geoscience research. Nuclear Instruments and Methods in Physics Research B, 219-220, 534-549.
Wegdén M, Kristiansson P, Pastuovic Z, Skogby H, Auzelyte V, Elfman M, Malmqvist KG, Nilsson C, Pallon J, Shariff A (2004) Hydrogen analysis by p–p scattering in geological material. Nuclear Instruments and Methods in Physics Research B, 550-554.

2005-2009

Wegden M, Kristiansson P, Skogby H, Auzelyte V, Elfman M, Malmqvist KG, Nilsson C, Pallon J, Shariff A (2005) Hydrogen depth profiling by p–p scattering in nominally anhydrous minerals. Nuclear Instruments and Methods in Physics Research B 231, 524–529.
Asimow PD, Stein LC, Mosenfelder JL, Rossman GR (2006) Quantitative polarized FTIR analysis of trace OH in populations of randomly oriented mineral grains. American Mineralogist 91, 278-284.
Kohn SC (2006) Structural studies of OH in nominally anhdyrous minerals using NMR. Reviews in Mineralogy and Geochemistry 62, 53-66.
Libowitzky E, Beran A (2006) The structure of hydrous species in nominally anhydrous minerals: information from polarized IR spectroscopy. Reviews in Mineralalogy and Geochemistry 62, 29-52.
Rossman GR (2006) Analytical methods for measuring water in nominally anhydrous minerals. In: Keppler H and Smyth JR, eds, Water in Nominally Anhydrous Minerals. Reviews in Mineralogy and Geochemistry 62, 1-28.
Aubaud C, Withers AC, Hirschmann MM, Guan Y, Leshin LA, Mackwell SJ, Bell DR (2007) Intercalibration of FTIR and SIMS for hydrogen measurements in glasses andnominally anhydrous minerals. American Mineralogist 92, 811–828.
Ludwig T, Stalder R (2007) A new method to eliminate the influence of in situ contamination in SIMS analysis of hydrogen. Journal of Analytical Atomic Spectroscopy 22, 1415-1419
O'Leary JA, Rossman GR, Eiler J (2007) Hydrogen analysis in minerals by continuous-flow mass spectrometry. American Mineralogist 92, 1990-1997.
Wegden M, Kristiansson P, Skogby H, Auzelyte V, Elfman M, Malmqvist KG, Nilsson C, Pallon J, Shariff A (2005) Hydrogen depth profiling by p–p scattering in nominally anhydrous minerals. Nuclear Instruments and Methods in Physics Research B 231, 524–529.
Kovacs I, Hermann J, O'Neill HSC, Gerald JF, Sambridge M, Horvath G (2008) Quantitative absorbance spectroscopy with unpolarized light: Part II. Experimental evaluation and development of a protocol for quantitative analysis of mineral IR spectra. American Mineralogist 93, 765–778.
Sambridge M, Gerald JF, Kovacs K, O'Neill HSC, Hermann J (2008) Quantitative absorbance spectroscopy with unpolarized light: Part I. Physical and mathematical development. American Mineralogis 93, 751–764.
Bureau H, Raepsaet C, Khodja H, Carraro A, Aubaud C (2007) Determination of hydrogen content in geological samples using elastic recoil detection analysis (ERDA). Geochimica et Cosmochimica Acta 73, 3311–3322.
Xue X, Kamzaki M (2009) H Proton Distributions and Hydrogen Bonding in Crystalline and Glassy Hydrous Silicates and Related Inorganic Materials: Insights from High-Resolution Solid-State Nuclear Magnetic Resonance Spectroscopy. Journal of the American Ceramic Society 92, 2803-2830.

2010s

Prechtel F, Stalder R (2010) FTIR spectroscopy with a focal plane array detector: A novel tool to monitor the spatial OH-defect distribution in single crystals applied to synthetic enstatite. American Mineralogist 95, 888–891.
Withers AC (2013) On the use of unpolarized infrared spectroscopy for quantitative analysis of absorbing species in birefringent crystals. American Mineralogist 98, 689-697.
Stephant A, Remusat L, Thomen A, Robert F (2014) Reduction of OH contamination in quantification of water contents using NanoSIMS imaging. Chemical Geology 380, 20-26.
Withers A, Mosenfelder J, Bureau H, Raepsaet C, Hirchmann M (2014) Analysis of H in Natural and Experimental Nominally Anhydrous Minerals: A Comparison of Elastic Recoil Detection Analysis, Infrared and SIMS Measurements. AGU ERDA abstract V41A-4764.
Kumamoto KM, Warren JM, Hauri EH (2017) New SIMS reference materials for measuring water in upper mantle minerals. American Mineralogist 102, 537-547.
Shuai K, Yang X (2017) Quantitative analysis of H-species in anisotropic minerals by polarized infrared spectroscopy along three orthogonal directions. Contributions to Mineralogy and Petrology 172, 14.
Jackson A, Parker RL, Sambridge M, Constable C, Wolf AS (2018) The inverse problem of unpolarized infrared spectroscopy of geological materials: Estimation from noisy random sampling of a quadratic form. American Mineralogist 103, 1176–1184.
Qiu Y, Jiang H, Kovacs I, Xia QK, Yang X (2018) Quantitative analysis of H-species in anisotropic minerals by unpolarized infrared spectroscopy: An experimental evaluation. American Mineralogist 103, 1761–1769.
Weis FZ, Ros L, Reichart P, SKogby H, Kristlansson P, Dollinger G (2008) Hydrogen concentration analysis in clinopyroxene usingproton–proton scattering analysis. Physics and Chemistry of Minerals 45, 669-678.
Zhang WF, Xia XP, Eiichi T, Li L, Yang Q, Zhang YQ, Yang YN, Liu ML, Lai C (2019) Optimization of SIMS analytical parameters for water content measurement of olivine. Surface and Interface A,alysis 52, 224-233.