Ultralow HO content analysis with a large-geometry secondary ion mass spectrometer
Large-geometry secondary ion mass spectrometry (LG-SIMS) is routinely used to determine the elemental and isotopic compositions, thanks to its high sensitivity and in situ micro-analysis capability. Its large volumes of transfer and coupling column, however, might bring low vacuum and high backgroun...
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Veröffentlicht in: | Journal of analytical atomic spectrometry 2024-04, Vol.39 (4), p.17-176 |
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Zusammenfassung: | Large-geometry secondary ion mass spectrometry (LG-SIMS) is routinely used to determine the elemental and isotopic compositions, thanks to its high sensitivity and
in situ
micro-analysis capability. Its large volumes of transfer and coupling column, however, might bring low vacuum and high background of volatile elements (esp. H), which hampers its application in ultralow H
2
O content measurement. In this study, we report a modified analytical procedure to accurately analyze samples with ultralow-level H
2
O content by using a LG-SIMS of type CAMECA IMS 1280-HR. Based on four new water content working reference materials of quartz glasses with H
2
O contents ranging from
ca.
0 to 39 ppm, the estimated detection limit of LG-SIMS is 0.15 ppm for H
2
O. This ultralow detection limit is achieved mainly by the intrinsic high sensitivity of the instrument and the conjunctive usage of a stabilized temperature-controlled cooling trap device and a novel tin-bismuth alloy mount preparation technology, which are able to maintain a vacuum pressure at 1.7 × 10
−9
mbar in the analysis chamber. Based on these new improvements, our approach can potentially become a routine choice for analyses of H
2
O content and oxygen-hydrogen isotopes for (extra)terrestrial materials with ultralow-level water content.
An improved LG-SIMS (CAMECA IMS 1280-HR) procedure for achieving sub-ppm LOD for water analysis by updating the cooling trap. |
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ISSN: | 0267-9477 1364-5544 |
DOI: | 10.1039/d3ja00422h |