NanoSIMS as an analytical tool for measuring oxygen and hydrogen isotopes in clay minerals from palaeosols: Analytical procedure and preliminary results

Atomic spectrometry update – a review of advances in environmental analysis

“…Certied U particles were used 26 in a comparison of AMS, SIMS and TIMS for the determination of isotope ratios in individual U particles, an application important for nuclear provenance and safeguarding purposes. The relative errors in the determination of 234 U/ 235 U and 234 U/ 236 U in NBL CRM U200 (uranium isotopic standard) by AMS were <10 and <20%, respectively, whereas the results obtained by ssion track-TIMS and SIMS were within ±5% and ±10% of the certied values, respectively, for both techniques. The relative error and external precision of 234 U/ 238 U and 235 U/ 238 U in the analysis of NBL CRM U850 (uranium (U 3 O 8 ) isotopic standard, 85% U-235) by AMS, SEM-TIMS or SIMS were <10% and <5%, respectively.…”

“…The relative error and external precision of 234 U/ 238 U and 235 U/ 238 U in the analysis of NBL CRM U850 (uranium (U 3 O 8 ) isotopic standard, 85% U-235) by AMS, SEM-TIMS or SIMS were <10% and <5%, respectively. The average values of the relative error and external precision for 236 U/ 238 U were both <5% for AMS analysis but <10% for SEM-TIMS or SIMS analyses. The EDXRFS and SF-ICP-MS analyses in an inter-laboratory comparison of PM 2.5 lters from the IMPROVE air monitoring network gave 27 results that agreed within ±20%.…”

“…For a carbonatitic dolomite with variable Fe# but homogeneous O isotopes, this online method gave a homogeneous d 18 O value of 7.94 ± 0.34& (2SD, n = 40), comparable with that (7.94 ± 0.20&, 2SD) obtained from bulk analysis. In an application of NanoSIMS to the measurement of H and O isotopes in clay minerals in palaeosols, preparation of the samples as thin sections was preferable 236 because their resin contents were lower than those of thick polished sections. The high spatial resolution of NanoSIMS enabled the isotopic ratios to be measured in selected positions within the samples so that only the clay minerals of interest could be targeted.…”

“…Microwave-assisted digestion according to Method EN 16174 was preferred to digestion under reux (Method EN 13346), and ICP-AES was preferred to ICP-MS or spectrophotometric determination because this combination gave highest P recoveries and best precision. on rapid alkali-fusion methods for determining anthropogenic 236 U in soil that could provide results quickly following nuclear incidents. Automatic ow-analysis systems and potential application to multi-nuclide analysis were also addressed.…”