Evaluation of Speciation Technology - OECD Nuclear Energy Agency

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carried out by the ultra-filters with 100 k, 30 k, 10 k and 5 k Daltons. The radioactive concentrations of 238 Pu and 241 Am in each size fraction were determined by liquid scintillation counting in a Packard Tri-Carb 2550 liquid scintillation counter. The percentage of these nuclides in each size range was estimated from the radioactivity concentration in each molecular size. Blank experiments for Pu and Am in NaClO4 solution and artificial sea water were carried out with the same procedure. The association experiments were performed in duplicate or triple except for Pu and Am in the Imaichi and Pu in the Mobara. Results and discussion Characteristics of groundwater organics The Imaichi groundwater shows yellowish colour, and the Tokachigawa and Mobara exhibit brownish colour. UV-VIS spectra of the groundwaters are shown in Figure 1. The absorption spectrum of the Mobara has two broad absorption peaks at 241 nm and 280 nm. The Tokachigawa sample exhibits featureless curve. The Imaichi groundwater has three broad peaks at 265 nm, 379 nm and 417 nm. The absorbance at three peaks consist mainly of organics (89-94%) with molecular size less than 5 k Daltons The EEM contour plots for the groundwater samples are shown in Figure 2. The Imaichi groundwater has two distinct peaks at Ex. 220 nm/Em. 320 nm and Ex. 275 nm/Em. 320 nm, and a broad peak at Ex. 330 nm/Em. 415 nm. The Tokachigawa and Mobara samples have two broad peaks. These broad peaks are detected at similar wavelengths among these groundwaters, and are consistent with the HA and FA isolated from the groundwater samples [6, Nagao unpublished data]. The excitation and emission spectra of HS show broad peaks typically occurring around 260, 310-350 nm and 380-460 nm, respectively [7-9]. The protein-like fluorescence arises from the fluorescence of aromatic amino acids, either free or as protein constituents, and is observed at an emission of 300-305 nm (tyrosine-like) and 340-350 nm (tryptophan-like) from excitation at 220 and 275 nm [10]. Therefore, the fluorescent organics of Tokachigawa and Mobara groundwaters consist mainly of HS. The RFI is increased in the order of the Imaichi< the Tokachigawa< the Mobara. The Imaichi groundwater contains protein-like materials because the fluorescence peak disappears after the ultra filtration with ultrafilters having 100 k Daltons. The RFI is 7-30 times higher than that of humus-like materials. Figure 3 shows molecular size distribution of UV-absorbing organics, humic acid (HA) and fulvic acid (FA) isolated from the groundwater by the XAD extraction procedure. These size patterns of organics are almost similar with the humic substances (HA and FA). Therefore, the groundwater UV-absorbing organics are mainly occupied by HS. These results indicate that the groundwater samples can be classified into three groups: • The Imaichi sample, humus-poor groundwater containing protein-like materials. • The Tokachigawa sample, humus-rich groundwater. • The Mobara sample, humus-rich saline groundwater. 183
Molecular size distribution of Pu and Am in groundwaters Figure 4 shows size distribution of Pu and Am in the absence of organics. Pu and Am added to NaClO4 solutions and artificial sea water are mostly retained by the 0.45 µm filters, although about 20% of Pu is found in molecular size less than 5 k Daltons. There is no difference in the size distribution of Pu and Am in NaClO4 solutions and artificial sea water. The both nuclides may undergo hydrolysis and form particles. Figure 5 shows the size distribution of Pu and Am in organic-rich groundwaters together with that of dissolved organics. The 73% of the humus-poor groundwater from Imaichi is found in molecular size from 0.45 µm-100 k Daltons. On the other hand, the dominant fraction of Pu in the humus-rich groundwaters is 30k-10k Daltons for the Tokachigawa and
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Nuclear Science Evaluation of Speci
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ORGANISATION FOR ECONOMIC CO-OPERAT
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OPENING ADDRESS - Satoshi Sakurai,
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SESSION D Methods for Redox Speciat
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Part D: Methods for Redox Speciatio
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EXECUTIVE SUMMARY The Workshop on E
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Speciation methods evaluated in the
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SPECIATION IMPERATIVES FOR WASTE MA
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matrices poses difficult challenges
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Table 1 lists some of the more comm
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In the complex biosphere there are
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SESSION A Methods for Trace Concent
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Introduction Experimental tests of
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complexes. As a result, fulvic acid
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possibility of selective extraction
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Table 1. Data on radiochemical anal
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Figure 1. Flowsheet of isolation of
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NANOSCOPIC SPECIATION OF AQUATIC AC
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A number of spectroscopic methods h
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Figure 4. LPAS and UV-Vis spectra o
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composite and hence it is called br
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[11] J.V. Beitz,, J.P. Hessler, “
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SPECIATION FROM PHOTON TO ION DETEC
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technique for speciation (i.e. the
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Figure 2. TRLIF spectra and lifetim
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Figure 5. ES-MS of uranium hydroxo
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[11] “Dual use of Micellar Enhanc
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Introduction The solution chemistry
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of the metal sorbed was less than 9
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For the hydrated ions without any c
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those of sorbed Cm(III) and Eu(III)
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Conclusion The luminescence propert
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[34] Graffeo, A.J., Bear, J.L., J.
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Figure 1. Luminescence decay consta
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Figure 3. Plot of the inner-sphere
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Figure 5. Distribution coefficients
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Figure 7. Dissolved fraction of Eu(
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SESSION C Methods for Empirical For
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Introduction The application of X-r
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The mica was left in the solution f
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That the GIXAS spectra of the Hf(IV
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[7] Frauenfelder, H., Steffen, R.M.
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Figure 3. Grazing incidence XAFS be
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Figure 7. Hf L3 edge GIXAFS spectra
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Introduction Nuclear magnetic reson
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ecause there is no longer an anisot
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20-30 MHz is observed for slowly tu
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[12] P. Caravan, J.J. Ellison, T.J.
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Figure 4. NMRD curves of free Gd 3+
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SESSION D Methods for Redox Speciat
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What is meant by speciation In the
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• It is non-invasive and non-pert
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Table 1. Selected absorption bands
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Figure 3. Shift in absorption edge
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Introduction Energy production reli
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then Pu in higher oxidation states
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• Reliability and reproducibility
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Conclusion Currently existing techn
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Table 1. Systems studies; the metho
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SESSION E Predictive Approach to Sp
Page 135 and 136: Introduction Thermodynamic data pro
Page 137 and 138: secondary mineral formation in immo
Page 139 and 140: Additionally, if a phase is impure,
Page 141 and 142: REFERENCES [1] T. Murakami, T. Ohnu
Page 143 and 144: Figure 1. (a) Backscattered electro
Page 146 and 147: CHEMICAL ANALOGY IN THE CASE OF HYD
Page 148 and 149: 4f-electrons of the lanthanides, an
Page 150 and 151: Since water molecules are substitut
Page 152 and 153: REFERENCES [1] D. Rai, J.L. Swanson
Page 154 and 155: Table 3. Effective charges of actin
Page 156 and 157: Figure 3. Atomic number dependence
Page 158: POSTER SESSION Part A: Methods for
Page 161 and 162: Introduction Several complementary
Page 163 and 164: migration. Consequently, only one p
Page 165 and 166: Some solutions are under test, such
Page 168 and 169: DEVELOPMENT PROGRAMME OF ANALYTICAL
Page 170 and 171: Evaluation of the footprints in the
Page 172 and 173: REFERENCES [1] B. Pellaud, “IAEA
Page 174 and 175: MATRIX-ASSISTED LASER DESORPTION/IO
Page 176 and 177: Preparation of the samples There ar
Page 178 and 179: Acknowledgement SHIMADZU Handelsges
Page 180 and 181: Figure 3. Clusters of uranium(VI) o
Page 182 and 183: ASSOCIATION OF ACTINIDES WITH DISSO
Page 186 and 187: REFERENCES [1] N.A. Marley, J.S. Ga
Page 188 and 189: Figure 3. Molecular size distributi
Page 190 and 191: SPECIATION OF “HOT PARTICLE” BY
Page 192 and 193: The clear results were obtained reg
Page 194 and 195: in some tens volt per centimetre an
Page 196 and 197: APPLICATION OF X-RAY AND LOW ENERGY
Page 198 and 199: of 12.5 keV to 23.0 keV. The coeffi
Page 200 and 201: [7] R.C. Gatti, H. Nitsche, et al.,
Page 202: Figure 1. Calibration results for 2
Page 205 and 206: Introduction HQ was used as the ext
Page 207 and 208: Iron(III) speciation can be achieve
Page 209 and 210: Figure 1. Solubility of HMOnQ in 4
Page 212 and 213: SPECIATION OF ENVIRONMENTAL RADIONU
Page 214 and 215: precipitate (humic acid fraction) w
Page 216 and 217: Acknowledgements This research has
Page 218 and 219: Figure 1. Speciation procedure A: e
Page 220: POSTER SESSION Part B: Methods for
Page 223 and 224: Introduction The possibility of dis
Page 225 and 226: fluorescence decay rate of the diff
Page 227 and 228: Table 1. Spectroscopic characterist
Page 229 and 230: Figure 3. Peak deconvolution of a m
Page 232 and 233: SPECIATION ANALYSIS ON EU(III) IN A
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ACTINYL(VI) SPECIATION IN CONCENTRA
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Preparation and characterisation of
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Characterisation of solid AnO2CO3 T
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Solubility data of uranyl in carbon
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CHARACTERISATION OF OXIDE FILMS FOR
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Figure 1. Relative concentration of
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Figure 4. Schematic structure of ox
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Introduction The actinide elements
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5LI-(Me-3,2-HOPO (X=CH2 5LIO-(Me-3,
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Uranium sequestering agents Uranium
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REFERENCES [1] (a) K.N. Raymond, in
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SPECIATION OF PU(IV) COMPLEXES WITH
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will have an absorption spectrum th
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As shown in our earlier work, Eq (1
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Figure 1. Plots of log Ka-2 D(I) vs
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As demonstrated above, laser induce
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DIRECT SPECTROSCOPIC SPECIATION OF
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4 Energy relative to Pu(IV) 3 2 1 0
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Introduction In R&D on the “back
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distribution ratios of Am are not s
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Figure 1. The crystal structure of
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Table 1. Selected geometrical param
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Introduction The two important oxid
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to these two minerals. Ferrihydrite
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REFERENCES [1] J.K. Osmond and M. I
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ELECTROANALYTICAL DATA ON URANIUM,
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- system of Eq. (2), which is measu
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The following consideration indicat
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Figure 1. Coulopotentiograms for U,
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SEPARATION AND DETERMINATION OF URA
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HPEC procedure An aqueous solution
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REFERENCES [1] T. Braun, G. Ghersin
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Figure 3. Effect of pH on the reten
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Introduction Voltammetry or polarog
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voltammograms in Figures 2(a)-2(c)
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Figure 2. Voltammograms for U(VI) s
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Introduction One of the most unique
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The ∆V1/2 of anodic and cathodic
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Table 1. Half wave potential for ac
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REDOX SPECIATION OF NP IN TBP EXTRA
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Analyser). Nitric acid concentratio
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papers dealing with Np oxidation in
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Figure 2. Np distribution coefficie
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Figure 6. Np distribution coefficie
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POSTER SESSION Part E: Predictive A
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Introduction In the back-end of the
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CO2 in the solution and were calcul
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Table 1. Thermochemical cycles for
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Introduction The essence of data pr
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(sensitivity analysis). In order to
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[G15] = LOG(SUM(D15:F15)) (25) Here
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Table 2. Spreadsheet arrangement of
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Introduction Scientific studies aim
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Figure 2. Comparison of non-linear
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The analysis shows a probability of
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Internationally accepted QA/QC stan
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SUBGROUP REPORTS 357
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Advantages On-line CE-MALDI/TOF MS
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• Colloidal state: - Membrane fil
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[10] P.A. Bertrand, G.R. Choppin,
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METHODS FOR MACRO CONCENTRATION SPE
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Advantages are a complete structure
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X-ray photoelectron spectroscopy: X
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The advantages are: • A multi-ele
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[12] S. Tsutsui, M. Nakada, M. Saek
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[44] H. Capdevila, P. Vitorge, E. G
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Molecular structure Molecular struc
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The detection limit of these method
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By analysing the chemical shifts an
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Current Chemistry. No. 157, K. Yosh
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AN OVERVIEW OF ACTINIDE REDOX SPECI
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Related to this technique is comple
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Main advantages of the electrochemi
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Extraction method with use of PMBP,
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[37] W. Runde, M.P. Neu, S.D. Conra
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Reagent BaSO4 Silica gel CaCO3 Tabl
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Figure 1. X-ray absorption edge ene
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The following sections address the
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priority and are supplemented by do
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has been addressed, albeit somewhat
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Table 1: Comparison of •G° f for
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The full range of environmental par
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[21] P.L. Brown, R.N. Sylva, “Uni
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RECOMMENDATION It was recommended t
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There should be allowance for datab
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Annex 1 LIST OF PARTICIPANTS BELGIU
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ARISAKA, Makoto Tel: +81 29 282 549
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NAGAISHI, Ryuji Tel: +81 29 282 549
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YASUOKA, Hiroshi Tel: +81 29 282 50
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RAI, Dhanpat Tel: +1 509 373 5988 P
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Participants of the Workshop on Eva
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ORDER FORM OECD Nuclear Energy Agen
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