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03 aiea presentation fakhi
03 aiea presentation fakhi
03 aiea presentation fakhi
03 aiea presentation fakhi
03 aiea presentation fakhi
03 aiea presentation fakhi
03 aiea presentation fakhi
03 aiea presentation fakhi
03 aiea presentation fakhi
03 aiea presentation fakhi
03 aiea presentation fakhi
03 aiea presentation fakhi
03 aiea presentation fakhi
03 aiea presentation fakhi
03 aiea presentation fakhi
03 aiea presentation fakhi
03 aiea presentation fakhi
03 aiea presentation fakhi
03 aiea presentation fakhi
03 aiea presentation fakhi
03 aiea presentation fakhi
03 aiea presentation fakhi
03 aiea presentation fakhi
03 aiea presentation fakhi
03 aiea presentation fakhi
03 aiea presentation fakhi
03 aiea presentation fakhi
03 aiea presentation fakhi
03 aiea presentation fakhi
03 aiea presentation fakhi
03 aiea presentation fakhi
03 aiea presentation fakhi
03 aiea presentation fakhi
03 aiea presentation fakhi
03 aiea presentation fakhi
03 aiea presentation fakhi
03 aiea presentation fakhi
03 aiea presentation fakhi
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03 aiea presentation fakhi

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  • -Le détecteur qui délivre les impulsions électriques à la suite de chaque détection de rayonnement Gamma. L’efficacité relative du détecteur utilisé dans ce travail, est de 30%, sa résolution est de 1,8 Kev. - Un générateur délivrant une haute tension au détecteur, qui est de 5000V positive. - Le préamplificateur qui a pour rôle la mise en forme du signal. - L’amplificateur , sa fonction est d’amplifier et de mettre en forme les signaux délivrés par le P.A. - ADC (Analogue Digital Converter), permet de convertir le signal analogique en provenance de l’amplificateur en un signal logique lisible par la carte d’acquisition. - MCA  est la carte d’acquisition d’enregistrement et d’affichage des spectres permettant leur dépouillement.
  • We have been applied Sequential extractions using extractants with progressively increasing extraction capacity . The sequential extractions, described in this diagram, were performed under oxic conditions in constantly agitated centrifuge tubes, with a sample size of 1 g. After each extraction stage, supernatant was separated from the residue by centrifugation for 15 min and then filtrated through a 0.45 µm membrane filter into polypropylene bottles for analysis. Residue was rinsed twice with deionised water, hand shaken and separated by centrifugation and filtration . Each filtrate acidified at pH < 1 with concentrated hydrochloric acid and stored at 4°C for uranium determination by ICP-MS. The residue obtained at the last stage of the sequential extractions were ground, ashed at 850°C during 2 h and completely dissolved by alkaline fusion.
  • Transcript

    • 1. Presented by: Pr.fakhi Said Directory of Radiochemistry research group Uranium in Moroccan sedimentary rocks: Metrology and Geochemistry tryS.FAKHI Said, E.Fait, R.Outayad, I. Voique, C. Galindo. A. Nourreddine, E.Khouya, H. Elhadi, M.Aadjour, H. Hannach, M.Benmansour, A.Abderahim.M. Mouflih Projects: PICS 52, PICSS 802, AECID A/026017/09 and the UMR: CNESTEN and Projects: PICS 52, PICSS 802, AECID A/026017/09 and the UMR: CNESTEN andUHIIMC, Projet of marocain academie (oïl shales valorisation)UHIIMC, Projet of marocain academie (oïl shales valorisation)
    • 2. plan Interfaces solid/ water anlysis - Context: - Main objectives - Description - Present work: Study of Solid compartment- Area, samples and anlysis- Results- Conclusion
    • 3. Global Context- Migration of stable and radioactive metals at the interface between Solid/ solution.- Behavior of heavy and radioactive metals in the environment.- Process which control the behavior of metals in natural environments (clay, phosphates, Black shale,…) 3
    • 4. Aims•Process influencing the distribution and transfer ofmetals.•Natural and anthropic Materials for the sorption andtrapping these elements!: waste mangement applications•Methods and proceedures of separation: application tothe separation of minor actinides and the recovery of U(case of phosphates, oil shales and other matrix). 4
    • 5. Description•Scientific context:- Processes of retention: exchange of ions on clays, the substitution of ions in phosphates, formation of complexes/precipitates of surface on oxides, clays and phosphates and formation of Coprecipitates.- studies of the questions which remain posed as for thespecies formed on the mineral surface in the naturalenvironments i.e. in the presence of many inorganic(phosphate, carbonate) and organics (humâtes) ligands.-Second step: applications: séparation, material élaboration and metal recovery-First step: compartment solid study, surronding water alaysis and interfacesolid/water analysis. 5
    • 6. Present work: Study of Solid compartment Optimization of the isotopes analysis methods: U, Th and of Ra and their descendants: Gamma and alpha spectrometry and ICP-MS. Characterization of the phases which concentrate the isotopes of U, Th and Ra… Applications of the methods for study of Sedimentary deposits (Layers) Separation of the particle size of sediment rocks as a solid horizon study of distribution of the natural radionucléides in the different phases and grains which constitute solid phase (case of phosphates sediments). Processes of extraction of U and other heavy metals starting from phosphates , fossil, Black oil shales, clays, and calcerous … 6
    • 7. Area, samples and anlysisI. Phosphates from Oulad Abdoun Basin :1. Samples : from different layers and interlayer drilling of different areas:2. Principal aims:- - geochemistry and distribution of natural radionuclides depending on the depth and the drilling facies.- - sequential extraction: contribution of the different phases in the trapping radionuclides: (intrinsic distribution in appatite, limestone, and fossils,- - contribution of 3 main particle size of phosphate ores in total radioactivity.II. The Mesozoic basins essaouira-Abda and Doukkala : Moroccan Atlantic marginclay, bsaltes, limestone and carbonate, evaporite of 4 drills are analysed( geochemirstry of radionucléides, oil and gaz research)III. Black Oil Shale samples from M layer of Timahdit : sorption and sequential extraction of natural radionuclides mainly U . 7
    • 8. Geographical and geological framework of the Study Areas 1. Oulad Abdoun Basin: Phosphate ores 8
    • 9. Disturbances 1. Oulad Abdoun Basin : DisturbanceThe normal configuration of the phosphatic series is from time totime disturbed by structures which modified the usual succession ofthe levels phosphatic. What are the levels of radionuclides (U) in this matrix? 9
    • 10. II. BlackOil Shale of M.L. Timahdit III. Mesozoic basins essaouira-Abda- DoukkalaMap of oil Shale of Timahdit Geological Map of Mesozoic deposits  10
    • 11. The Timahdit blackoil shale- 42 billion tons of oil shale / 15 billion barrels ofoil in place.- four lithological layers (T, Y, X and M),correlated throughout the deposit. Total area 350km ² 11
    • 12. - Fakhi and al, géochimie des forages OYB-1 et NDK-2Lithostratigraphic columns and sample location of boreholesOYB-1 and NDK-2 (Mesozoic deposits) 12
    • 13. Radiochemical procedures- gamma and alpha spectrometry, ICP-MS- The thin alpha sources were prepared by chemicalelectrodeposition of U and Th and by sorption of Ra on MnO2coated polyamide discs.- U and Th were separated by using the ion-exchangeschromatography before their deposition.- An other method was carried out by using alkaline fusion byLiB4O7 and LiBO2, of U and Th determination in sedimentsamples.<<The proposed methods have been applied for U, Th and Raisotopes determination in the sedimentary rock: phosphate andblack shale and coastal of Paleozoic and Mesozoicsedimentary rocks, and Leach solutions >> 13
    • 14. I. Phosphates from Oulad Abdoun Basin : Morphological characterization by SEM  The majority of the par ticles (seed phosphated, coprolithe and of the osseous remains), present angular forms with sizes estimated between 3 and 700µ m.  The semi-quantitative composition of the phosphate par ticles was determined by SEM-EDXS, shows contents of Ca, O, Si and P and Fe, Al, Mg, Na, F and S. Morphology of the grains of the phosphatic series 14
    • 15. X-rays diffraction analysis  . - phosphate sample mainly contains fluoroapatite carbonated of general Ca 5(PO 4)3F formula: 40 Ca10− z ( PO4 ) 6− x CO3− x F2+ x − 2 z 35 .- - The matrix contains, moreover other Ca Mg(CO 3)2 Ca Mg(CO 3)2 30 forms such: Ca10 ( PO4 ) 6 F2 Ca10 ( PO4 ) 6 OH 2 25Intensité Ca 5(PO 4)3F Ca 5(PO 4)3F 20 Ca 5(PO 4)3F Ca 5(PO 4)3F Ca 5(PO 4)3F Ca 5(PO 4)3F Ca Mg(CO 3)2 Ca 5(PO 4)3F SiO2 ( Ca, Mg )( CO3 ) 2 Ca 5(PO 4)3F CaCO 3 Q Q 15 CaCO 3 Ca ( Mg 0,5 Fe0,5 ) ( CO3 ) 2 Q Q 10 CaCO 3 Q CaCO 3 5 Q Q Q Q 0 10 15 20 25 30 35 40 45 50 55 60 65 70 2theta - mudstone, organic matter and the trace éléments 15
    • 16. Sample facies %C % O.M. GT12 Phosphate 0,73 1.25 GT 8 Limestone 0,97 1,67 Fossil Myliobatis 1,33 2,30 dixoni 16
    • 17. Concentration : U and Th (alpha spectrometry), the stable by ICP-MS 17
    • 18. 238 U, 235U , 234U in Bq/Kg as a function of depth -The figure shows that very observable change between the concentration of 234 U in phosphates and mainly limestones facies. 18
    • 19. Activity Ratio 234U / 238U and desequilibrium 2 234 U/ 238 U 230 Th/ 238 U 1 8 9 10 11 12 13 14 15 16 17 18 19 20 21 PROFONDEUR (m) U/238U> 1: Interactions of mineral phases with fluids containing 234U234234 U/238U< 1 : the main process is the alteration of rock, damage essentially par alpharecoil.230 Th/238U: most important in determining the direction and magnitude of mobilization 230 Th/238U> 1 mobilization of U than for altered sample: 230 Th>238U>234U 19230 Th/238U< 1 accumulation of U
    • 20. DisturbancesBq/Kg 20
    • 21. contribution of 3 main particle size of phosphate ores in total radioactivity 1. size separation by appropriate sieving (3 fractions):- fine fraction(0.05 to 0.1mm): mainly clay and quartz- medium fraction (0.1 and 0.5 mm): grains of phosphate- coarse fraction (0.5 mm and 2.25 mm). fragments of shells ofinvertebrates, vertebrate bone debris, coprolites, and aggregates of grains weakly cemented phosphate (Sand fraction). 2. purpose of the analysis: in industrial phosphate, before traitement, an initial Size séparation is effected: 1.A clay fraction 2.A sand fraction 3.Phosphate fraction Contribution of each fraction in the total radioactivity??? 21
    • 22. Contribution of each fraction in the total radioactivity Sample GT20 as example : sillon B, Ypresian age. % /act 234 U/238U 230 Th/238U 238 U 230 Th 234 U CrudeSamples 1279±146 1194±115 1229±141 0,96 0,93 coarse 201±21 121±13 180,96±19,1 15,71 0,90 0,60fractionMedium 79,67 0,94 0,78 1019±183 799±95 956,68±172,8fraction Fine 4,3 0,90 0,93 55±7 51±7 49,32±6,35fraction 22
    • 23. GT 12 and GT 20 (phosphate layers bound by marl) samples from Gahar tajerphosphate ores : it correspond to detrital rock, porous, often layered,consisting of grains bound by a cement GT1- Wet phosphatic marl facies,. Depht: 20,6m Concentration of 238 U = 1456±7 Bq/Kg) or 117,98 ppm GT12- Phosphate at the base yellowish coarse coprolite very thin and marly roof, with reddish oxidation and discrete laminations. Depht: 13,5m Concentration of 238 U = 1807±51 Bq/Kg)or 146,4ppm 23
    • 24. II. The Mesozoic basins essaouira-Abda and Doukkala : MoroccanAtlantic marginLithology of Depht (m) Age samples U Bq/Kg 238 Dolomite 1170 25 (2.0 ppm) limestone portlandian Clay- 1893,8 Dogger 30 (2.4 ppm)sandstone Basalts 812 15 (1.2ppm) upper Triassic gray clay 350 Berrisian 7 (0.51 ppm) 24
    • 25. Activities RatioVariation in the ratios 226Ra / 238U and 214Pb / 238U 25
    • 26. 1. (Black oil shale of timahdite)Element 238 U 235 U 234 U 232 Th 230 Th 228 Th 234 U/238U 230 Th/238UFraction 21.9 ± 19.5 ±Bulk sample 522 ± 41 26 ± 2 521 ± 41 519 ± 48 1.0 ± 0.1 0. ± 0.1 2.1 2.0F1 Soluble in 4.0 ± 0.4 < LD 7.4 ± 0.6 < DL 26 ± 2 < DL 1.8 ± 0.2 6.5 ± 0.8water. 0.17±F2 exchangeable 17 ± 1 1.1 ± 0.2 32 ± 2 < DL 2.9 ± 0.9 < DL 1.9 ± 0.2 0.05 0.07 ±F3: carbonates. 53 ± 3 2.9 ± 0.5 100 ± 5 < DL 3.9 ± 0.9 < DL 1.9 ± 0.1 0.02F4 apatite phase, Manganese / 0.09 ± 44 ± 3 2.1 ± 0.4 60 ± 3 < DL 4±2 < DL 1.4 ± 0.1iron oxides and 0.05hydroxidesF5 Organic matter 11.9 ± 10.6 ± 0.78 ± 0.94 ± 394 ± 22 23 ± 2 308 ± 18 371 ± 66and pyrite 1.3 1.9 0.06 0.05 11.4 ± 10.0 ± 1.01 ±F6 Residual. 19 ± 1 0.8 ± 0.2 19 ± 1 92 ± 9 5.4 ± 0.7 1.3 1.8 0.09HCl + HF leaching 16 ± 1 0.8 ± 0.1 23 ± 2 13 ± 1.4 118 ± 10 9.5 ± 1.1 1.5 ± 0.2 7.4 ± 0.8 26
    • 27. 2. limestone Bulksample 238 U (Bq/Kg) 235 U (Bq/Kg) 234 U (Bq/Kg) 230 Th (Bq/Kg) 232 Th (Bq/Kg) (GT8) M 1494±120 71±15 1303±110 1363±100 12±4 F1 7,47±0,5 <LD 16,94±2 54±4 <LD F2 32±3 2±0,2 48±3 27±2 <LD F3 64±5 3±0,7 80±7 12±1,6 <LD F4 813±61 35±3,6 703±62 580±30 5±0,6 F5 567±48 28±2,1 484± 44 504±29,8 4,±1 F6 44±5 3±0,8 52±4 68± 10 1,5±0,1 F7 59,79±5,67 2,04±0,2 39,12± 5,84 142,50± 10 1,29± 0,5 27
    • 28. 4. Phosphate faciesGT6 phosphate 238 U (Bq/Kg) 235 U 234 U (Bq/Kg) 230 Th (Bq/Kg) 232 Th (Bq/Kg)Bulk sample (Bq/Kg) M 2220±137 98±24 2119±131 1821±128 53±10 F1 13 ±1,2 <LD 25±2 98±9,6 <LD F2 25±3,02 1,6±0,2 15±0,62 40±3 <LD F3 69±6,43 3±0,6 100±5 41±3 <LD F4 1332±42 62±3 1296±43 961±23 28±0,2 F5 643±20 30±2,3 593±22 510±18 14±2 F6 161±13,01 9±1,2 105,±9 77±09 5±1,05 F7 111±10 7±2 127±10 91±8 5±1 28
    • 29. Conclusion :The research on compartment solid phase:I.PHOSPHATES SAMPLES Radiochemical analysis by alpha spectrometry shows that:•The specific activities of the identified radionuclides areindependent depth of drilling.•They seem to depend on the nature of the deposits and on theprocesses of assimilation of appropriate radionuclides•Radionuclides seem rather concentrated in the sediment ofphosphates. 29
    • 30. Conclusion :-The deposits are mainly of marine origin, and most of the calcareoussediments are more or less altered.- In this work, we have shown, moreover, through the use of isotopic ratios, thatthe porous interface (limestone) is generally places of preferential alteration.This phenomenon is elucidated by the fractionation of U from these sites andtheir mobility to the lower layers.- For the phosphate facies, the U content varies from 76 ppm to 181 ppm(GT6).- For the intercalated layers of limestone, the U content varies from 28 ppm to122 ppm (GT8).- The higher uranium concentration in GT6 and GT8 formations relative tostrata above and below results from the accumulation of phosphorites in thisarea due to its leaching from above and redeposited below.-The process is not uniform, various sections and various horizons haveaccumulated more U than others.- Marly sediments have U concentration equal to 72 ppm, whereas in themarly argillite, it is 43 ppm.- Analysis of these results shows that in despite of their degree of weathering, 30limestones have an economic interest in the recovery process of U.
    • 31. - The main mineral phases, implied in the retention of trace elements, arequartz, clays, calcite and dolomite. Accessory minerals consist of pyrite,hydroxyl-apatite, anhydrite, feldspars.- uranium is highly enriched in the shale (55ppm). The actinide isassociated predominantly with humic acids in the +4 oxidation state , theprecursor of kerogen. - It has been deposited under anoxic reducing environment. - Carbonates and apatite contribute also to the retention of uranium. - The same phenomena is obseeved for phosphate sediments 31
    • 32. Conclusion :-In rocks called << Disturbances >> which constitute a permanent obstacle tothe exploitation of phosphate ores contains 113 ppm of U.- The study performed on the sample size of phosphate GT20, ageYpresian (- 53 46 AM), shows that:- The fine fraction(0.05 to 0.1mm): mainly clay and quartz contributes with4.3% in the total uranium of sedimentary rock.,- The medium fraction (0.1 and 0.5 mm): grains of phosphate has animportant contribution estimated at 79.67%,- The coarse fraction (0.5 mm and 2.25 mm). fragments of shells ofinvertebrates, vertebrate bone debris, coprolites, and aggregates of grains weakly cemented phosphate (Sand fraction), participates with15.71% to the total content of uranium. 32
    • 33. - The low activity ratios of 232Th/238U confers to the sediment a marinecharacter for all analysed sediments (phsphate, oil schales, andcenezoic one) other - the retention capacities of the black shale can be highlighted. Relevant metals are actually retained most probably via some active interfaces, resulting from an intimate association between organic matter and the inorganic matrix, especially silicates - The use of such black shale as a potential precursor of storage material for future possible high level waste repositories is under investigation: The adsorbents showed good properties; a specific area equals 270 m 2g- 1 and 600 m2g-1 (Patent) 33
    • 34. ​U, Th and Ra sorption kinetic by supports made from oil shale U Th Ra 34
    • 35. •Collaborators:- Mixed Unit of Research between CNESTEN and UHIIMC- Hubert Curien Multidisciplinary Institute t Strasbourg, France- Applied Nuclear Physics University of Seville.-Spagne•National Office Hydrocarbon Research.• Creation of the International Network of Research on InterfacesSolid / water.- The international patent Contract with NANOTECH•- -INVESTMENTS society on TSN process (Mai 2007). for your attention : for all information on the card carried out by Morocco: mining, seismic exploration for petroleum, consult Activity report of the National Office of Hydrocarbons and Mining (ONHYM-Morocco) 35
    • 36. THANK YOU FOR YOUR ATTENTION 36
    • 37.  the sequential extraction protocol 1g of sample rock + 30 ml of dionized water -Agitation during 24h -Centrifugation + washing two time by 2ml of water dionized 1st filtrate -Cetrifugation Residue of the 1st extraction +30 ml de MgCl2(1mol/l) Each filtrate -Agitation during 24hacidified at pH -Centrifugation + washing two time by 2ml of water dionized < 1 with 2sd filtrate concentrated hydrochloric -Cetrifugation Residue of the 2sd extraction + 30ml of acid and (CH3 COONa 1M, CH3COOH 1M)stored at 4°C -Agitation during 24h for analysis -Centrifugation + washing two time by 2ml of water dionized 3rd filtrate -Cetrifugation Residue of the 3rd extraction + 35ml of (NH2OH 0.04M, C2H3OOH 25%) -Agitation during 24h -Centrifugation + washing two time by 2ml of water dionized 4td filtrate -Cetrifugation
    • 38. Residue of the 4th extraction is calcined at 450°C during 2 h The calcined Residue of the 4th extraction 25 mL 30% H2O2 –15 mL 0.02M HNO3 (pH=2) 15 mL 30% H2O2 – 9 mL 0.02M HNO3 (pH=2) +(CH3COONa 3.2M, HNO3 20%) -Agitation during 24h the sequential extraction protocolth filtrate -Centrifugation + washing two time by 2ml of water dion -Cetrifugation Residue of the 5th extraction is Calcinated and attacked by HCl and HF 

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