Actinides (f-block) 1-1

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1 Actinides (f-block) Actinide Chemistry Speciation Role of Oxidation State Complexation Specific Actinides U, Pu, Am Example: Am and Cm transport at Oak Ridge Use of laboratory data to determine chemical species Conclusions 1-1

2 Actinide Chemistry Actinides Th, Pa, U, Np, Pu, Am, Cm, Bk, Cf, Es, Fm, Md, No, Lr Most are synthetic elements Chemistry is dictated by oxidation state Various oxidation states Th: 4+ U: 3+, 4+, 6+ Np: 4+, 5+, 6+ Pu: 3+, 4+, 5+, 6+ Am, Cm:

3 Actinides Actinides begin to fill 5f orbital Electronic configurations Th [Rn]6d 2 7s 2 Pa [Rn]5f 2 6d 1 7s 2 U [Rn]5f 3 6d 1 7s 2 Np [Rn]5f 4 6d 1 7s 2 Pu [Rn]5f 6 7s 2 Am [Rn]5f 7 6d 1 7s 2 Isoelectronic with the lanthanides Differences between 5f and 4f account for 1-3 greater oxidation state variability of actinides

4 1-4

5 1-5

6 1-6

7 Actinide Chemistry Electronic configuration yield different properties Solubility Complexation Spectroscopy Differences utilized in separations Pu from U Pu at 4+, 3+, while U at 6+ Oxidation state has profound effect on environmental behavior 1-7

8 Complexation Chemistry Wide variety with a number of complexes Different oxidation states Variation in behavior with ph complexation with inorganic and organic ligands * properties of compounds redox optical, volatility * solution * salts 1-8

9 Trivalent Actinides Am, Cm Am does have oxidation states 3-6 most prevalent state is 3+ Similar chemical behavior Trivalent lanthanides can be used as homologs Thermodynamic data can be interchanged Alpha emitters Produced through neutron capture 1-9

10 1-10

11 A=241 Isotopes 1-11

12 237 Np Levels 1-12

13 244 Cm Levels 1-13

14 1-14

15 Industrial Uses Smoke detectors 241 Am Starting material for production of transcurium isotopes Heavy actinides Transactinides SNAP batteries 242 Cm Production of 238 Pu 1-15

16 Metallic Am, Cm MP = 1176 C Formed from reduction of fluoride or oxide compounds D= g/cm 3 Dissolves in mineral acids Formed in subgram quantities 1-16

17 Compounds Oxides AmO, Am 2 O 3, AmO 2 AmO 2 is stable and can be reduced with hydrogen CmO 2 is unstable Cm 2 O 3 is stable (MP =2020 C) Halides Formed with HF at elevated temperature AmF 3, AmF 4 can be formed CmF 4 can be formed, but not as stable of AmF

18 Solution chemistry Oxidation states Am (3-6) Am 3+, AmO 2+, AmO 2 2+ can be made Am 4+ rapidly disproportionates in solution except concentrated fluoride or phosphate Cm (3 and 4) Cm 4+ is a strong oxidizing agent Cm 4+ can be stabilized in high fluoride concentrations forming CmF 5- or CmF

19 Trivalent State In solution forms Carbonates Hydroxides Organic complexes Easily separated from other actinides by redox properties Behaves similar to trivalent lanthanides 1-19

20 Absorption and fluorescence process of Cm 3+ Wavenumber (10 3 cm -1 ) Optical Spectra H G F A 7/2 Excitation Fluorescence Process Emissionless Relaxation Fluorescence Emission 0 Z 7/2 1-20

21 1-21

22 Hexavalent Actinides U, Np, Pu, and Am can form MO 2 2+ ions in solution Stability U > Pu > Np > Am AmO 2 2+ is a strong oxidizing agent Environmentally Relevant: UO 2+ 2 NpO 2+ 2 and in some case PuO 2 2+ and Uranium prominent in natural decay series Uranium has fissile isotopes 233 U, 235 U 1-22

23 Uranium Isotopes Isotope Half-life Decay Mode Source min α (80%), EC (20%) min α (20%), EC (80%) d α d EC a α E5 a α 233 Pa E5 a α Natural E8 a α Natural E7 a α min β E9 a α Natural min β h β min β 1-23

24 235 U Decay Chain 1-24

25 1-25

26 238 U Decay Chain 1-26

27 1-27

28 233 U Decay Chain 1-28

29 Natural Abundances of the Uranium Isotopes Mass Number % Abundance ± ± ± U is of importance due to fission from slow neutrons 235 U + n fission products + energy n Energy about 200 MeV 1 MWd 1 g 235 U Neutron capture of 238 U produces plutonium and higher actinides 1-29

30 Uranium Occurrence in Nature Occurrence Concentration (mass U/g) Igneous Rocks 4 µg Basalt 0.2 µg Granites 25 µg Sedimentary Rocks 2 µg Phosphate Rocks 100 µg Bituminous shale 65 µg Lignite 50 µg Ocean Water 1 ng 1-30

31 U in nature tons of U in the crust of the earth tons of U in the oceans Minerals are generally U(IV) Upon weathering uranyl(vi) forms High amount of uranium in high silica rock as granite Frequent association with carbon compounds Increased solubility of uranyl(vi) Uranyl(VI) carbonate minerals Mining by a variety of methods Drift mining Solvent 1-31

32 Uranium treatment Uranium separation from ore Solvent extraction Ion exchange Based on oxidation states Separation of uranium isotopes Gas centrifuge Formation of volatile UF 6 Laser Ionization of isotopes 1-32

33 Plutonium Chemistry dictated by oxidation state oxidation states of 3, 4, 5, and 6 Electronic configuration yield different properties Solubility Complexation Spectroscopy Differences utilized in separations Most abundant synthetic actinide element Used in Reactors Weapons Batteries 1-33

34 1-34

35 Pu Isotopes 238 Alpha, short lived 239 Fissile 240 Neutron capture of Fissile, neutron capture of Longest lived isotope Small amount in spent fuel 1-35

36 Pu Separations Number of different separations examined Solvent extraction Precipitation Ion exchange Most separations for the purification of Pu Separation from U and fission products Large scale processes developed 1-36

37 Solvent Extraction and Precipitation 1-37

38 1-38

39 Complexation Chemistry Wide variety with a number of complexes Different oxidation states Variation in behavior with ph complexation with inorganic and organic ligands * properties of compounds redox optical, volatility * solution * salts 1-39

40 1-40

41 1-41

42 1-42

43 1-43

44 Eh-pH diagram for Pu 1-44

45 Formation of tetravalent colloids 1-45

46 Speciation of Pu in the Solid Phase Introduction Pu solid phase Recent Publication Experiment Procedures Results Discussion of Results Implications for waste management Further studies 1-46

47 Pu Solids Solids can be made with different oxidation states Carbonates, hydroxides, fluorides 3+, 5+ and 6+ oxidation states need special conditions to be stabilized 4+ states tend to be most stable Pu binary oxides is expected to be most stable state (PuO 2 ) Thermodynamic considerations Inability to prepare other oxide oxidation states 1-47

48 Pu Solids Pu 2 O 3, Pu 2 O 5, and PuO 3 tend to be unstable Can make the equivalent U species For PuO 2 formation, excessive mass gains during metal oxidation by H 2 O observed Pu (s) + O 2 PuO 2(s) H 2 O sorption to high surface area of oxide 1-48

49 Recent Study Examined Pu oxides by two methods X-ray diffraction (XRD) Gives information about structure * Lattice parameters X-ray photoelectron spectroscopy (XPS) Used to evaluate binding of oxygen Examined reaction of PuO 2 with H 2 O from 25 C to 350 C 1-49

50 Results Mass spectrometric analysis shows production of H 2(g) PuO 2(s) +xh 2 O (abs) <--> PuO 2+x(s) + xh 2(g) 350 C H 2 pressure formation 300 C 250 C 200 C Time (hr) 1-50

51 Results Lattice parameter change Attributed to increase in Pu:O ratio Cubic lattice parameter variation a o = (O:Pu) Relative insensitivity attributed to formation of Pu(VI) Extra O forms plutonyl O/Pu ratio 1-51

52 Results X-ray photoelectric spectroscopy data High binding energies for the oxide 442 ev, 429 ev * 4f 5/2, 4f 7/2 Pu(VI) or Pu(VII) No Pu(V) O 1s spectrum consistent with oxide Absence of OH - attributed to continued reaction of water 1-52

53 Results PuO 2+x formed via catalytic cycle Driven by H 2 O sorbed to surface If O 2 present, H reforms water Formation of water drives catalytic cycle 1-53

54 Implications for Waste Management PuO 2(s) has an extremely low solubility PuO 2(s) + 2H 2 O <--> Pu OH - K sp = [Pu 4+ ][OH - ] Pu oxidation state log K sp Changing oxidation state from 4+ increases solubility Actual Pu concentration in environment should be higher than estimated 1-54

55 Solubility studies Further studies See if Pu(VI) is in solution Increase in Pu solution concentration should occur Pu(VI) known to occur from Pu(IV) solids Spectroscopic determination of Pu(VI) UV-Visible (absorbance) EXAFS (plutonyl oxo groups) Both can differential Pu(VI) from Pu(IV) 1-55

56 Pu:O ratio Further Studies Formation of CO 2 from oxide starting material Based on thermodynamic data Methods of oxidation Water greater oxidizer than O 2 Degree of Oxidation Around 25% of Pu in hexavalent state 1-56

57 XRD studies Comments on Results Only indicates changes in lattice Role of radiolysis Discounted in experiments due to activation energy measurement for reaction Needs to be closely examined Catalytic cycle Pu known to have catalytic properties Cycle not thermodynamically favored Formation kinetics Cycles is slow even the the presence of oxidants 1-57

58 Cm and Am Containing Drums Disposed at Waste Area Group 5 (WAG-5) at Oak Ridge National Laboratory Am and Cm found 50 m from burial site 1-58

59 Conditions at WAG-5 at ORNL Cm and Am migrated from disposal site ph near 7 Carbonate system High concentration of natural organic matter (fulvic acid) Use modified data from literature and verify [Fulvic acid (III)] =2 µmol/l [An 3+ ] t = [Cm 3+ ] + [Am 3+ ] = 20 pmol/l aqueous carbonate concentration evaluated from the measured alkalinity ionic strength at 0.02 M 1-59

60 Hydrolysis Hydrolysis is critical environmental reaction Limits solubility Colloid formation Varies with metal ion Dissolved material in groundwater moves Dissolved ions move ligands can complex metal ions Pu 4+ + H 2 O PuOH 3+ + H + Pu 4+ + OH PuOH 3+ K hydx,y = [M x (OH) xz y y ][H + ] y 1-60 [M z+ ] x [OH ] y [M z+ ] x ß xy = [M x (OH) y xz y ]

61 Carbonate Complexes Carbonate is another important environmental ligand Comes from CO 2 (g) equilibrium with atmosphere Atmospheric partial pressure is CO 2 (g) + H 2 O <--> H 2 CO 3 (aq) carbonate can be found by ph and partial pressure of CO 2 log [CO 3 2- ] = ± log P CO2 + 2pH Pu 4+ + CO 3 2 PuCO

62 Colloids in Transport IV VI V solid phase colloid radionuclide II III I Particles suspended in solution Radionuclide behavior can be dictated by colloidal behavior 1-62

63 Formation of Pu colloids 1-63

64 Solubility [Actinide] tot =fn(k sp ) K sp is the solubility constant For the reaction: M x L y (s) <--> xm + yl K sp = [M] x [L] y Solubility reactions are expected to limit migration of radionuclides Solubility varies with oxidation state Solubility for Pu Pu 4+ < PuO 2 2+ Pu 3+ < PuO 2 + Pu(OH) 4 Pu OH 1-64

65 -2 Plutonyl Carbonate Solubility 1% CO 2 tot (mol/l) % CO 2 Ref log[co 3 2 ] (mol / L ) 1-65

66 Estimated Stability Constants for Am, Complex Cm with Organics at ORNL logß (L/mol) AnFA(III) 6.09±0.12 An(OH)FA(II) 13.04±0.20 An(OH) 2 FA(I) 17.24±0.30 An(CO 3 )FA(I) 12.74±0.30 Also carbonate and hydrolysis data Estimated Constants Based on Identified Trends Between Fulvic and Humic Acid Agrees with experimental data 1-66

67 TRLFS of Cm Fulvic Acid 1.0 Relative Intensity [FA(III)] total O M 5e-7 M 7.5E-7 M 1e-6 M 2.5e-6 FA M 5e-6 FA M Free Cm 3+ peak (594 nm) CmFA(III) peak (599 nm) nm 1-67

68 Cm Experimental Results Increase in CmFA(III) concentration seen by TRLFS Deconstruct spectra to determine [Cm 3+ ] free and [CmFA(III)] Anion Exchange Studies CmFA(III) complex retained by column Free Cm 3+ eluted Count eluant to determine [Cm 3+ ] free Stability Constant Results TRLFS experiment: log ß (L/M) = 6.08 ± 0.14 Anion exchange experiment: log ß (L/M) = 6.12 ±

69 1.0 ORNL WAG-5 Estimated Speciation Relative Species Concentration An 3+ AnFA(III) Total An bound water range AnCO 3 FA(I) AnCO 3 AnOHFA(II) ph Calculation based on thermodynamic data 1-69

70 ORNL Conclusions Purified ORNL Fulvic Acid Similar to Other Fulvic Acids Proton Exchange Capacity and ß value Complexation Behavior In Good Agreement With Values Estimated from Experimental Observations Consistent Complexation Model Can Use Literature Results from Other Humics 1-70

71 Actinide Environmental Chemistry Conclusions behavior depends upon oxidation state Different oxidation states for same element possible Change due to redox conditions Host phase Stability Mobility Near field Eh, ph Sorption 1-71

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