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, Log lithostratigraphique séquentiel (V2lom, V2yam, V2lyad) de la Formation de Moguilivska (FM) reconstitué d'après les observations des affleurements des sites de Novodnistrovsky, Bendashevka et Popeluhi
, Annexe 1 Figure 2 Log lithostratigraphique : A -de la Formation Yarishevska (FY) établi sur la base des observations des Séquences V2bern et V2bron sur le site de la vallée Borshive
, FN), et de ses transitions avec les Séries Moguilive-Podilska et Kanilivska, établi sur la base des observations de la Séquences V2ka sur les sites de Lipchany et
, Logs litho-stratigraphiques des formations supérieures indifférenciées, ou « Upper Undifferentiated Formations » (UUF)
, En raison de ces difficultés, si la colonne stratigraphique établie représente une série condensée de bordure de bassin, elle permet cependant d'étudier de façon quasi continue la totalité des faciès et leur variablité dans le temps. La répartition des affleurements et les variations latérales de faciès rendent les corrélations difficiles à l'échelle de ce bassin, Les échantillons ont été prélevés près des localités de Novodnistrovsky (48°34'N, 27°26'E), Popeluhi (48°24'N, 28°96'E) et Bendashevka (48°39'N, 28°03'E) pour FM, dans vallée de Borshive, près de la ville Moguilive-Podilsky
, Les Méthodes d'analyses La lithologie
, Chaque affleurement a fait l'objet d'une description détaillée des relations stratigraphiques et structurales existant entre les différentes unités observées. Par ailleurs, dans ce contexte silicoclastique, l'ensemble des faciès et des figures sédimentaires qui leur sont attachées ont été étudiés avec soin afin de pouvoir reconstituer les paléo-conditions de dépôts et les paléo-environnements qui, Les études lithostratigraphique et faciologique ont été menées au cours de trois missions de terrain
, Les conditions d'analyses sont : vide 10 -5 Pa, courant de sonde 1,0 nA, distance de travail 17 mm, taille du spot 0,1 µm, temps de comptage 100 s. Les minéraux servant à l'étalonnage des éléments majeurs sont : albite (NaAlSi 3 O 8 ), orthose (KAlSi 3 O 8 ), forstérite (Mg 2 SiO 4 ), diopside (CaMgSi 2 O 6 ), pyrite, Les données chimiques sont acquises à l'aide du logiciel Quantax afin d'obtenir soit des cartes de répartition élémentaire soit des compositions chimiques pondérales (pourcentage massique élémentaire ou en oxyde) déterminées après corrections ZAF
, La minéralogie totale a été réalisée à partir de l'échantillon broyé à l'aide d'un broyeur SODEMI à anneaux en acier chromé. Les échantillons les plus durs, comme les grès silicifiés, sont préalablement débités à la scie diamantée en petits cubes de 0 ,5 cm de côté. La poudre obtenue a une finesse de 1 à 2 µm soit inférieure à 50 µm, taille minimale préconisée pour la diffractométrie de rayons X (Klug & Alexander, 1974). La poudre est placée sur un support évidé en minimisant au maximum les effets d'orientation afin d, Minéralogie Préparations L'étude minéralogique a porté tant sur la totalité des composants minéraux que sur les constituants de la fraction argileuse
, L'identification des phyllosilicates présents dans les échantillons repose sur l'analyse de leurs réflexions (00l) dont l'intensité diffractante en poudre est souvent insuffisante pour une détermination correcte. Aussi est-il nécessaire de travailler sur préparations orientées
, Le premier type est directement réalisé à partir d'un aliquot de poudre mis en suspension puis déposé sur une lame de verre. L'objectif est alors de caractériser l'ensemble du cortège des phyllosilicates, sans préjuger de la dimension de ces particules ni de leur origine. En outre, les proportions de ces différentes phases ainsi obtenues ont été utilisées pour l
, L'objectif étant alors d'obtenir une fraction enrichie en phyllosilicates hydratés i.e. en minéraux argileux, symptomatiques des mécanismes d'altération et/ou de diagenèse survenant au cours des épisodes géologiques. L'extraction de cette dernière est réalisée après avoir dispersé 10 g de matériau désagrégé (mais non broyé) mis en contact avec 300 mL d'eau osmosée (18 M?m .cm -1 ) et sonifié (300W pendant 2 min) à l'aide d'un sonificateur Bioblock VibroCell 750. Pour les matériaux très durs, 20 à 30g des cubes préalablement sciés sont mis à imbiber dans l'eau osmosée pendant 1 nuit à l'étuve 50°C avant d'être plongés dans l'azote liquide puis remis en contact eau et sonifié modérément dans un bain ultrason Elmasonic S60. Après plusieurs cycles de ce traitement, la congélation instantanée de l'eau porale aboutit à l'éclatement progressif des joints de grains et à la libération des phyllosilicates intergranulaires, Le second type de préparations orientées a porté sur la fraction argileuse, p.319
, Après contrôle visuel de la stabilité de la suspension obtenue après une nuit à 20°C, la fraction < 2 µm est extraite par sédimentation en pot Beckman de 750 mL à l'aide d'une centrifugeuse JOUAN GR 422 fonctionnant à 20°C et 1000 tr/min pendant 120 s. Le surnageant recueilli par siphonage sur 10 cm de profondeur est, mécanique sur une roue à renversement pendant 4 heures
, 15 mg d'argile sont remis en suspension dans 1,5 mL d'eau osmosée puis déposés sur une lame de verre et laissé sécher à l'air. La préparation orientée ainsi confectionnée permet d'étudier la position des réflexions (00l) de chacune des espèces phyllosilicatées lors des traitements usuels de séchage, glycolage, 1980.
, Pour cela les 15 mg d'argile ont été mis cinq fois en contact avec 5 mL d'une solution de CaCl 2 1N (ou M/2) puis lavés à l'eau osmosée pour éliminer les chlorures (dont l'absence est contrôlée par un test AgNO 3 ). En procédant ainsi le domaine interfoliaire des minéraux gonflants est saturé en ion calcium (Ca 2+ ), Les échantillons destinés à faire l'objet d'une simulation numérique ont été saturés au calcium
, Son système optique est constitué une fente anti-divergence de 0,11°2?, d'une fente antidiffusion de 0,11°2?, de systèmes de Soller de 4 radians d'espacement de fentes et d'un filtre K ? au nickel. Les conditions d'analyse sont 40 kV et 40 mA. Les paramètres d'acquisition sont de 1s par pas de 0.025 °2?, sur des domaines angulaires de 2-65 °2? et 2-35 °2?, en modes poudre et orienté respectivement, Les diffractogrammes de rayons X ont été obtenus à l'aide d'un diffractomètre Bruker D8 Advance A25, équipé d'une source au cuivre ((? CuK? = 1,5418 Å) et piloté par le logiciel Diffract Suite©, vol.8, 2009.
, Le traitement des diffractogrammes et la recherche des phases en mode poudre ont été faits à partir du logiciel ANalytical HighScore en relation avec le module minéralogique PdF3 de la base de donnée internationale ICDD JCPDS. En ce qui concerne la fraction argileuse, les phyllosilicates et les minéraux argileux (phyllosilicates hydratés) en particulier ont fait l'objet d'analyses complémentaires notamment pour les phases interstratifiées
, Dans le cas des minéraux interstratifiés, l'ensemble des réflexions dans le domaine angulaire 2-15°2? a été déconvolué à l'aide du logiciel libre Fytik afin de déterminer pour chaque réflexion le nombre minimal de ses composantes, et pour chacune d'elle ses caractéristiques propres à savoir : position angulaire (°2?), intensité (cps), surface totale (cps.°2?) et largeur à mi
, illite, smectite?) et de leurs proportions respectives dans l'interstratification. Les hypothèses émises permettent ainsi de fixer des contraintes physiques pour la simulation des diffractogrammes calculés de ces phases. La simulation, L'ensemble de ces données permet de formuler un certain nombre d'hypothèses sur les constituants primaires (chlorite
, Géochimie Les éléments majeurs, traces et les terres rares des 55 prélèvements ont été analysés par spectrométrie d'émission plasma à couplage inductif (ICP) au service d'analyse des roches et des minéraux (SARM) du Centre de Recherches Pétrographiques et Géochimiques (CRPG) de Nancy
, Avant analyse, les échantillons font l'objet d'un broyage et d'un microbroyage en mortiers agate afin d'éviter toute micropollution. Les poudres obtenues sont fondues dans un mélange de LiBO 2 puis minéralisées dans une solution de HNO 3 . Les éléments majeurs (Si, ) sont dosés par ICP-OES (Inductively Coupled Plasma Optical Emission Spectroscopy) Thermo Icap
, à torche radiale et restitués en pourcentages massiques d'oxydes. Les éléments mineurs, traces et terres rares sont mesurées par ICP-MS (Inductively Coupled Plasma Mass Spectrometry) Thermo
,
, Les ellipses d'erreur pour chaque point sont représentées au niveau 2? et intègrent des incertitudes internes et externes. Les points de données ont été regroupés pour calculer une date et une erreur 2? associée. Le matériau de référence 91500 zircon -1065 Ma (65) -a été analysé avec les échantillons pour surveiller de manière indépendante la précision externe et la précision des mesures, Datation Les données isotopiques U-Th-Pb de la bentonite B4 ont été mesurées par spectrométrie de masse à couplage inductif par ablation laser (LA-ICP-MS) au Laboratoire Magmas & Volcans, 2001.
, Les conditions de recuit sont de 900°C pendant 48 heures, tandis que l'abrasion chimique a été réalisée en plaçant chaque zircon isolé dans une capsule Savillex pré-nettoyée avec HF + trace HNO 3 à 210°C pendant 13 heures dans des bombes Parr. Après l'étape de dissolution partielle, chaque zircon a été de nouveau transféré dans un flacon Savilex de 3 ml à bouchon vissé. Le reste a été complètement pipeté et les zircons restants ont été rincés dans de l'eau ultra-pure puis fluxés pendant plusieurs heures dans HCl 6N sur une plaque chauffante à une température d'environ 80°C. Après élimination de l'acide, les fragments de zircon ont de nouveau été rincés plusieurs fois dans de l'eau ultra-pure et du HNO 3 7N dans un bain à ultrasons. Chaque grain de zircon a été dissout dans une capsule Savillex pré-nettoyée, additionnée d'environ 5 mg de la solution traceur EARTHTIME 202 Pb-205 Pb-233 U-235 U, Sr SRM987 et Pb SRM982 et SRM983. Le temps pour le MEB a été déterminé comme étant constant à 22,5 ns jusqu'à 1,3 Mcps et à un rendement Faraday / SEM compris entre 93 et 94%. Le fractionnement isotopique du plomb et de l'uranium a été corrigé en utilisant les rapports 202 Pb/ 205 Pb (0,9992391 ± 0,0265%, 1?) et 233 U/ 235 U (0,99506 ± 0,01%, 1?) de la solution à double pointe. Les facteurs de fractionnement moyens de Pb et U déterminés étaient, 2005.
, Tous les rapports 206 Pb/ 238 U et 207 Pb/ 206 Pb ont été corrigés pour le déséquilibre initial en 230 Th/ 238 U en utilisant Th/U [magma] en supposant que Th/U du magma = 3,5. La précision des données mesurées a été évaluée par une analyse répétée de la solution synthétique 100Ma, Tous les Pb communs dans les analyses de zircon ont été attribués au blanc procédural avec la composition isotopique de plomb suivante: 206 Pb/ 204 Pb = 17,62 ± 2,09, p.206, 2004.
, Toutes les données sont rapportées avec des erreurs internes seulement, y compris des statistiques de comptage, des incertitudes dans la correction de la discrimination de masse et l'incertitude dans la composition de Pb commune. La valeur MSWD de la moyenne pondérée de l'échantillon se situe dans la plage des valeurs acceptables, Pb/ 238 U meilleures que 0,05%. Toutes les incertitudes rapportées sont au niveau de 2 sigma, 2006.