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Analysis of hydrogen in olivine by SIMS: Evaluation of standards and protocol

Mosenfelder, Jed L. and Le Voyer, Marion and Rossman, George R. and Guan, Yunbin and Bell, David R. and Eiler, John M. and Asimow, Paul D. (2001) Analysis of hydrogen in olivine by SIMS: Evaluation of standards and protocol. American Mineralogist, 96 (11-12). pp. 1725-1741. ISSN 0003-004X. https://resolver.caltech.edu/CaltechAUTHORS:20130415-102910989

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Abstract

We measured hydrogen concentrations in 12 olivines using secondary ion mass spectrometry (SIMS and NanoSIMS), cross-calibrated against Fourier transform infrared (FTIR) spectroscopy and nuclear reaction analysis (NRA). Five of these samples are routinely used for calibration in other laboratories. We assess the suitability of these olivines as standards based on over 300 SIMS analyses, comprising 22 separate calibrations. Seven olivines with 0–125 ppm H_(2)O give highly reproducible results; in contrast to previous studies, the data are fit to well-constrained calibration lines with high correlation coefficients (r^2 = 0.98–1). However, four kimberlitic megacrysts with 140–245 ppm H2O sometimes yield ^(16)O^(1)H/^(30)Si ratios that have low internal precision and can vary by up to a factor of two even in sequential analyses. A possible cause of this behavior is the presence of sub-microscopic inclusions of hydrous minerals, such as serpentine. In most cases, however, we link the anomalous results to the presence of sub-micrometer to micrometer-scale pores (as small as 100 nm), which we imaged using SEM and NanoSIMS. These pores are interpreted to be fluid inclusions containing liquid H_(2)O, other volatiles (including fluorine), and/or hydrous phase precipitates. Ionization of the contents of the pores contributes variably to the measured ^(16)O^(1)H, resulting in analyses with erratic depth profiles and corresponding high uncertainties (up to 16%, 2σ_mean). After filtering of these analyses using a simple criterion based on the error predicted by Poisson counting statistics, all the data fit well together. Our results imply that the Bell et al. (2003) calibration can be applied accurately to all olivines with IR bands from ~3400–3700 cm^(−1), without the need for band-specific IR absorption coefficients.


Item Type:Article
Related URLs:
URLURL TypeDescription
http://dx.doi.org/10.2138/am.2011.3810DOIArticle
http://ammin.geoscienceworld.org/content/96/11-12/1725PublisherArticle
http://ammin.geoscienceworld.org/content/96/11-12/1725/suppl/DC1PublisherSupporting Information
ORCID:
AuthorORCID
Rossman, George R.0000-0002-4571-6884
Guan, Yunbin0000-0002-7636-3735
Asimow, Paul D.0000-0001-6025-8925
Additional Information:© 2011 Mineralogical Society of America. Manuscript received February 17, 2011; Manuscript accepted July 5, 2011; Manuscript handled by Florian Heidelbach. Financial support for this research was provided by the Gordon and Betty Moore Foundation, the White Rose Foundation, and by NSF grant EAR-0947956 to George Rossman. We thank Erik Hauri, Jeremy Boyce, and Richard Hervig for helpful discussions; Chi Ma for assistance with the electron microprobe and SEM; and Jörg Hermann and an anonymous reviewer for helpful suggestions that improved the manuscript.
Funders:
Funding AgencyGrant Number
Gordon and Betty Moore FoundationUNSPECIFIED
White Rose FoundationUNSPECIFIED
NSFEAR-0947956
Subject Keywords:Secondary ion mass spectrometry; spectroscopy; infrared; water; mantle; olivine; calibration
Issue or Number:11-12
Record Number:CaltechAUTHORS:20130415-102910989
Persistent URL:https://resolver.caltech.edu/CaltechAUTHORS:20130415-102910989
Usage Policy:No commercial reproduction, distribution, display or performance rights in this work are provided.
ID Code:37937
Collection:CaltechAUTHORS
Deposited By: Jason Perez
Deposited On:15 Apr 2013 21:18
Last Modified:27 Nov 2019 00:06

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