Evaluation of Speciation Technology - OECD Nuclear Energy Agency

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[37] W. Runde, M.P. Neu, S.D. Conradson, D.L. Clark, P.D. Palmer, S.D. Reilly, B.L. Scott, C.D. Tait, Sci. Basis Nucl. Waste Man. XX. W.J. Gray, I.R. Triay, eds., MRS, 693 (1997). References for nuclear magnetic resonance spectroscopy [38] R.D. Fischer, in NMR of Paramagnetic Molecules: Principles and Applications, G.D. La Mar, W.D. Horrocks Jr., R.H. Holm, eds., Academic, New York, pp. 521-553 (1973). References for electrochemical methods [39] S. Kihara, Z. Yoshida, H. Aoyagi, K. Maeda, O. Shirai, Y. Kitatsuji, Y. Yoshida, Pure Appl. Chem., in press (2000). [40] H. Aoyagi, Z. Yoshida, S. Kihara, Anal. Chem., 59, 400-405 (1987). [41] S. Kihara, Z. Yoshida, H. Muto, H. Aoyagi, Y. Baba, H. Hashitani, Anal. Chem., 52, 1601-1606 (1980). [42] I. Goldberg, D. Meyerstein, Anal. Chem., 52, 2105 (1980). 397
Reagent TTA PMBP DBM HDEHP Table 1. Chemical separation methods for redox speciation Table 1a. Solvent extraction Conditions, Actinides Advantages/disadvantages/ key anal. parameters (III) (IV) (V) (VI) limitations, other comments pH-dependent D Rapid, quantitative separation pH 0-1 X O X X TTA is photosensitive pH 4.5 O O X O pH-dependent D pH 0-1 pH 4.5 pH-dependent D pH 8 pH 5.0-5.5 pH-dependent D pH 0 pH 1 Hexone 4.0 M Ca(NO3)2 1 M HNO3 , D ≤ 30 Diethylether 10 M NH4NO3 1 M HNO3 O: extracted, X: not extracted Reagent LnF3 0.8 M HNO3 , 0.25 M H2SO4, 0.5mM K2Cr2O7 BiPO4 X O O X O O X O X X X X X O O O Used to replace TTA Stable reagent Very small pKa (4.11) Stable reagent pKa = 9.2 Slow extn. kinetics Liq. cation exchanger 7 X O O O X X O O Low selectivity for redox state X O X O High salt concn. required 4 X X X O High salt concn. required Selective for An(VI), but not quantitative Difficult manipulation of the solvent Table 1b. Precipitation Conditions, key Actinides anal. parameters (III) (IV) (V) (VI) 0.25 M HNO3 Bi 3+ 25 mg/L H3PO4 ≤ 0.1 M Advantages/disadvantages/ limitations, other comments O O X X Drastic treatment is required to redissolve. Incapable of distinguishing V and VI O O X X Dence, crystalline ppt. Readily separable. Soluble in concn. HNO3 Incapable of distinguishing V and VI Zr(IO3)4 2 M HNO3 – O X X Probable involvement of IO3 - 4 in redox reaction (III ↔ IV) NaUO2(AcO)3 1 M HNO3 5 M NaNO3 3 M CH3COONa X X X O Specific for AnO2 2+ 4 O: precipitated, X: not precipitated Introduce α-activity to the sample. Time consuming Ref. 3, 4, 5, 7, 9 8, 9 6 4 Ref. 3, 4, 7, 9, 10, 11 12, 13, 14 398
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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
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Introduction Thermodynamic data pro
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secondary mineral formation in immo
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Additionally, if a phase is impure,
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REFERENCES [1] T. Murakami, T. Ohnu
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Figure 1. (a) Backscattered electro
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CHEMICAL ANALOGY IN THE CASE OF HYD
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4f-electrons of the lanthanides, an
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Since water molecules are substitut
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REFERENCES [1] D. Rai, J.L. Swanson
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Table 3. Effective charges of actin
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Figure 3. Atomic number dependence
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POSTER SESSION Part A: Methods for
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Introduction Several complementary
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migration. Consequently, only one p
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Some solutions are under test, such
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DEVELOPMENT PROGRAMME OF ANALYTICAL
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Evaluation of the footprints in the
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REFERENCES [1] B. Pellaud, “IAEA
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MATRIX-ASSISTED LASER DESORPTION/IO
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Preparation of the samples There ar
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Acknowledgement SHIMADZU Handelsges
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Figure 3. Clusters of uranium(VI) o
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ASSOCIATION OF ACTINIDES WITH DISSO
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carried out by the ultra-filters wi
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REFERENCES [1] N.A. Marley, J.S. Ga
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Figure 3. Molecular size distributi
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SPECIATION OF “HOT PARTICLE” BY
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The clear results were obtained reg
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in some tens volt per centimetre an
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APPLICATION OF X-RAY AND LOW ENERGY
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of 12.5 keV to 23.0 keV. The coeffi
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[7] R.C. Gatti, H. Nitsche, et al.,
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Figure 1. Calibration results for 2
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Introduction HQ was used as the ext
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Iron(III) speciation can be achieve
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Figure 1. Solubility of HMOnQ in 4
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SPECIATION OF ENVIRONMENTAL RADIONU
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precipitate (humic acid fraction) w
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Acknowledgements This research has
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Figure 1. Speciation procedure A: e
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POSTER SESSION Part B: Methods for
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Introduction The possibility of dis
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fluorescence decay rate of the diff
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Table 1. Spectroscopic characterist
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Figure 3. Peak deconvolution of a m
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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
Page 347 and 348: Table 2. Spreadsheet arrangement of
Page 349 and 350: Introduction Scientific studies aim
Page 351 and 352: Figure 2. Comparison of non-linear
Page 353 and 354: The analysis shows a probability of
Page 355 and 356: Internationally accepted QA/QC stan
Page 358: SUBGROUP REPORTS 357
Page 361 and 362: Advantages On-line CE-MALDI/TOF MS
Page 363 and 364: • Colloidal state: - Membrane fil
Page 365 and 366: [10] P.A. Bertrand, G.R. Choppin,
Page 368 and 369: METHODS FOR MACRO CONCENTRATION SPE
Page 370 and 371: Advantages are a complete structure
Page 372 and 373: X-ray photoelectron spectroscopy: X
Page 374 and 375: The advantages are: • A multi-ele
Page 376 and 377: [12] S. Tsutsui, M. Nakada, M. Saek
Page 378: [44] H. Capdevila, P. Vitorge, E. G
Page 381 and 382: Molecular structure Molecular struc
Page 383 and 384: The detection limit of these method
Page 385 and 386: By analysing the chemical shifts an
Page 387 and 388: Current Chemistry. No. 157, K. Yosh
Page 390 and 391: AN OVERVIEW OF ACTINIDE REDOX SPECI
Page 392 and 393: Related to this technique is comple
Page 394 and 395: Main advantages of the electrochemi
Page 396 and 397: Extraction method with use of PMBP,
Page 400 and 401: Reagent BaSO4 Silica gel CaCO3 Tabl
Page 402: Figure 1. X-ray absorption edge ene
Page 405 and 406: The following sections address the
Page 407 and 408: priority and are supplemented by do
Page 409 and 410: has been addressed, albeit somewhat
Page 411 and 412: Table 1: Comparison of •G° f for
Page 413 and 414: The full range of environmental par
Page 415 and 416: [21] P.L. Brown, R.N. Sylva, “Uni
Page 418 and 419: RECOMMENDATION It was recommended t
Page 420: There should be allowance for datab
Page 424 and 425: Annex 1 LIST OF PARTICIPANTS BELGIU
Page 426 and 427: ARISAKA, Makoto Tel: +81 29 282 549
Page 428 and 429: NAGAISHI, Ryuji Tel: +81 29 282 549
Page 430 and 431: YASUOKA, Hiroshi Tel: +81 29 282 50
Page 432: RAI, Dhanpat Tel: +1 509 373 5988 P
Page 435 and 436: Participants of the Workshop on Eva
Page 437 and 438: ORDER FORM OECD Nuclear Energy Agen
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