title: IR laser extraction technique applied to oxygen isotope analysis of small biogenic silica samples.
abstract: An IR-laser fluorination technique is reported here for analyzing the oxygen isotope composition (delta18O) of microscopic biogenic silica grains (phytoliths and diatoms). Performed after a controlled isotopic exchanged (CIE) procedure, the laser fluorination technique that allows one to visually check the success of the fluorination reaction is faster than the conventional fluorination technique and allows analyzing delta18O of small to minute samples (1.6-0.3 mg) as required for high-resolution paleoenvironmental reconstructions. The long-term reproducibility achieved with the IR laser-heating fluorination/O2 delta18O analysis is lower than or equal to +/-0.26 per thousand (1 SD; n = 99) for phytoliths and +/-0.17 per thousand (1 SD; n = 47) for diatoms. When several CIE are taken into account in the SD calculation, the resulting reproducibility is lower than or equal to +/-0.51 per thousand for phytoliths (1 SD; n = 99; CIE > 5) and +/-0.54 per thousand (1 SD; n = 47; CIE = 13) for diatoms. A minimum reproducibility of +/-0.5 per thousand leads to an estimated uncertainty on delta18Osilica close to +/-0.5 per thousand. Resulting uncertainties on reconstructed temperature and delta18Oforming water are, respectively, +/-2 degrees C and +/-0.5 per thousand and fit in the precisions required for intertropical paleoenvironmental reconstructions. Several methodological points such as optimal extraction protocols and the necessity or not of performing two CIE prior to oxygen extraction are assessed.
authors.affiliation: CEREGE, CNRS, Université Paul Cézanne Aix-Marseille III and IRD, Europôle de l'Arbois, BP 80, 13545, Aix en Provence Cedex 04, France.
authors.forename: Julien
authors.initials: J
authors.lastname: Crespin
authors.forename: Anne
authors.initials: A
authors.lastname: Alexandre
authors.forename: Florence
authors.initials: F
authors.lastname: Sylvestre
authors.forename: Corinne
authors.initials: C
authors.lastname: Sonzogni
authors.forename: Christine
authors.initials: C
authors.lastname: Paillès
authors.forename: Vincent
authors.initials: V
authors.lastname: Garreta
mesh_terms: D007259:Infrared Rays; D010103:Oxygen Isotopes / Q000032:analysis; D015203:Reproducibility of Results; D012822:Silicon Dioxide / Q000032:analysis*; D013696:Temperature
chemical_list: D010103:Oxygen Isotopes; D012822:Silicon Dioxide