Chemistry of the Heaviest Elements
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1 6th Asian-Pacific Symposium on Radiochemistry September 17-22, 2017, Jeju Island, Korea Chemistry of the Heaviest Elements Yuichiro Nagame 1,2 1 Advanced Science Research Center, JAEA 2 Graduate School of Science & Engineering, Ibaraki Univ. JAEA Tokai
2 Transuranium elements : Z 93 Transactinide elements: Z 104 The heaviest elements The heaviest elements: The elements with Z 101 that are produced only in heavy-ion-induced nuclear reactions. one atom-at-a-time H Li Na Rb Be B C N O F Ne Mg K Ca Sc Ti Sr Y Cs Ba La Zr Hf Fr Ra Ac Rf V Nb Ta Cr Mo W Re Db Sg Bh Mn Fe Co Ni Cu Zn Ga Ge Tc Ru Hs Rh Mt Pd Os Ir Pt Au Ds Ag Rg Cd Hg Tl Pb Bi Po At Cn Al In Nh Si Sn Fl P As Sb Mc S Se Te Lv Cl Br I Ts He Ar Kr Xe Rn Og Lanthanides Actinides La Ce Pr Nd Pm Sm Eu Gd Tb Dy Ho Er Tm Yb Lu Ac Th Pa U Np Pu Am Cm Bk Cf Es Fm Md No Lr 2
3 Naming four new elements nihonium and symbol Nh, for the element 113 moscovium and symbol Mc, for the element 115 tennessine and symbol Ts, for the element 117 oganesson and symbol Og, for the element 118 Talk by S. Dmitriev (IA-508) 3
4 Impact on science Searching for and producing new elements and their chemical / physical (nuclear) characterization are very challenging subjects in recent advanced nuclear & radiochemistry. How many chemical elements may be synthesized on earth? How can they be produced? How long can they survive? Which properties do determine their stability? What are their chemical and physical properties? How are the orbital electron configurations affected in the strong electric field of heavy atoms? These are the most fundamental questions in science. Yu. Ts. Oganessian & K. P. Rykaczewski, Phys. Today, August 2015, p. 32 4
5 Contents 1. Introduction: Chemical studies of the heaviest elements Atom-at-a-time chemistry Relativistic effects on electronic structure 2. Recent highlighted studies of liquid-phase chemistry 2-1. Complex formation of 104 Rf 2-2. Electrochemistry of 101 Md & 102 No 3. Atomic properties of the heaviest actinides 3-1. Ionization energy of 103 Lr 4. Summary & perspectives JAEA Tandem Accelerator 5
6 Objectives: 1. Introduction Chemical studies of the heaviest elements provide crucial & challenging opportunities to advance our understanding of properties of matter at the limits of existence to elucidate the influence of relativistic effects on atomic electrons to architect the Periodic Table at the farthest reach The heaviest elements (Z > 100): available in quantities of only a few atoms or often one atom-at-a-time Chemical characterization with an atom-at-a-time scale: Extreme Chemistry 6
7 Chemical properties: complex formation abilities 1. Introduction oxidation states & redox potentials valence electronic states, etc. role of relativistic effects on valence electronic structure of heavy atoms 1. Relativistic effects 2. Atom-at-a-time chemistry 7
8 Relativistic effects (1) General: relativity - increase of the mass with increasing velocity At heavy elements: Increasing nuclear charge plays as the accelerator of the velocity of electrons. Electrons near the nucleus are attracted closer to the nucleus and move there with high velocity. mass increase of the inner electrons and the contraction of the inner electron orbitals (Bohr radius) 1. Direct relativistic effects 8
9 Relativistic effects (2) Electrons further away from the nucleus are better screened from the nuclear charge by the inner electrons, and consequently the orbitals of the outer electrons expand. 2. Indirect relativistic effects 3. Spin-orbit (SO) splitting of levels with l > 0 into two levels with j = l ± 1/2 It is expected that the heaviest elements would show a drastic rearrangement of electrons in their atomic ground states, and as the electron configuration is responsible for the chemical behavior of elements, such relativistic effects can lead to surprising chemical properties. Increasing deviations from the periodicity of chemical properties based on extrapolation from lighter homologues in the Periodic Table are predicted. 9
10 Cracks in the Periodic Table E. Scerri, Scientific American, June 2013, p. 68..table may be losing its power due to relativistic effects. 10
11 Typical production rates of the heaviest nuclides used for chemical studies Z Nuclide T 1/2 Reaction σ / nb Production rate* Md 27 min 248 Cm( 11 B, 4n) min No 3.5 min 248 Cm( 12 C, 5n) min Lr 27 s 249 Cf( 11 B, 4n) min Rf 68 s 248 Cm( 18 O, 5n) 13 4 min Db 35 s 249 Bk( 18 O, 5n) 6 2 min Sg 14 s/9 s 248 Cm( 22 Ne, 5n) h Bh 17 s 249 Bk( 22 Ne, 4n) h Hs 10 s 248 Cm( 26 Mg, 5n) d Cn 4 s 242 Pu( 48 Ca, 3n) 287 Fl 283 Cn d -1 * Assuming typical values of 0.8 mg/cm 2 for the target thickness and beam intensities of 3 x particles per second. 11
12 Atom-at-a-time chemistry Because of the short half-lives and the low production rates of the heaviest nuclides, each atom produced decays before a new atom is synthesized. Any chemistry to be performed must be done on an "atom-ata-time" basis. This imposes stringent limits on experimental procedures. Rapid and very efficient radiochemical procedures must be devised. 12
13 Atom-at-a-time experiments 1. Gas-phase chemistry: Thermochromatography Isothermal chromatography Talk by A. Türler (IA-518) 2. Liquid-phase chemistry: Liquid-liquid extraction Ion-exchange chromatography Reversed-phase extraction chromatography Redox chromatography 13
14 Highlighted chemical studies Chemical properties of element 106 (seaborgium) M. Schädel et al, Nature 388, 55 (1997). Chemical characterization of bohrium (element 107) R. Eichler et al., Nature 407, 63 (2000). Chemical investigation of hassium (element 108) Ch. E. Düllmann et al., Nature 418, 859 (2002). Chemical characterization of element 112 R. Eichler et al., Nature 447, 72 (2007). Synthesis and detection of a seaborgium carbonyl complex J. Even et al., Science 345, 1492 (2014). Measurement of the first ionization potential of lawrencium, element 103 T. K. Sato et al., Nature 520, 209 (2015). Atom-at-a-time laser resonance ionization spectroscopy of nobelium M. Laatiaoui et al., Nature 538, 495 (2016). 14
15 Recent review articles M. Schädel and D. Shaughnessy. Eds (2014) Chem. Rev. 113, (2013) Nucl. Phys. A 944, (2015) Special Issue on Superheavy Elements Edited by Christoph E. Düllmann, Rolf-Dietmar Herzberg, Witold Nazarewicz and Yuri Oganessian 15
16 Presentation in APSORC2017 Overview A. Türler (IA-518): A postcard from the island of stability: what s new in superheavy element chemistry Production & Nuclear reaction mechanism J. V. Kratz (A-036): Radiochemical investigation of the kinematics of multi-nucleon transfer reactions in 48 Ca Cm collisions 10% above the Coulomb barrier H. Haba (A-079): Production and decay studies of 261 Rf, 262 Db, 265 Sg, and 266 Bh for superheavy element chemistry at RIKEN GARIS 16
17 Presentation in APSORC2017 Liquid-phase chemistry Y. Komori (A-078): Development of a rapid solvent extraction apparatus coupled to the GARIS gas-jet transport system to aqueous chemistry of the heaviest elements Gas-phase chemistry & atomic properties T. Tomitsuka (A-209): Adsorption of lawrencium (Z = 103) on a Ta surface N. M. Chiera (A-160): Unexpected transport to the cryo-on-line-detector COLD) setup of a volatile At species K. Shirai (A-035): Influence of surface condition of quartz column for gas chromatographic behavior of ZrCl 4 and HfCl 4 Y. Nagame (A-259): First ionization energies of heavy actinides Development of new innovative apparatuses! 17
18 Atom-at-a-time chemistry: 2. Recent liquid-phase chemistry To get statistically significant results with single atoms, it is indispensable to repeat the same experimental procedure several hundred or even several thousand times with cycle times of about the lifetime of the nuclide under investigation. The behavior of the heaviest elements is compared with that of its lighter homologs under identical conditions. Extensive series of detailed investigations have been made possible by the development of computer-controlled automated systems that have greatly improved the ability to perform rapidly and reproducibly large numbers of chemical (chromatographic) separations on miniaturized columns and to systematically vary ligand concentrations, thus allowing determining the stoichiometry of the eluted species: K d vs. [ligand]. The experiments with automated devices have produced detailed and sometimes surprising results that called for a detailed theoretical modeling of the chemical properties with improved quantum-chemical calculations. 18
19 Recent highlighted liquid-phase chemistry 2-1. Complex formation of 104 Rf - Fluoride complex formation of Rf complex formation abilities 2-2. Electrochemistry of 101 Md & 102 No - Redox reactions of Md & No oxidation states & redox potentials 19
20 Experiments with Rf in the liquid-phase 1. Production of a specific heaviest nuclide 2. Rapid transport of this nuclide to chemical separation devices 3. Fast chemical characterization that includes dissolution in an aqueous solution containing inorganic/organic ligands for complex formation 4. Preparation of a sample suitable for α-spectroscopy 5. Detection of nuclides through their characteristic nuclear decay properties for unambiguous identification The automated rapid chemistry apparatuses ARCA II and AIDA enable cyclic column chromatographic separation. Automated rapid chemistry apparatuses ARCA II and AIDA 20
21 AIDA: Automated Ion-exchange separation apparatus coupled with the Detection system for Alpha-spectroscopy 8 vacuum chambers Signal out He/KCl gas-jet Pulse motors 600 mm 2 PIPS detectors Preamp. Air cylinder ARCA II Eluent bottles Micro-columns Halogen lamp He gas heater Ta disk reservoir Sampling table Cyclic discontinuous column chromatographic separation of short-lived nuclides & automated detection of α-particles within a typical cycle time of 60 s 21
22 Photo of AIDA 22
23 2-1. Fluoride complex formation of Rf 248 Cm( 18 O, 5n) 261 Rf (T 1/2 = 68 s) : σ = 13 nb Experimental approach should involve detailed comparison of the chemical properties of the heaviest elements with those of their lighter homologues under identical conditions H Li Na Rb Be B C N O F Ne Mg K Ca Sc Ti Sr Y Cs Ba La Zr Hf Fr Ra Ac Rf V Nb Ta Cr Mo W Re Db Sg Bh Mn Fe Co Ni Cu Zn Ga Ge Tc Ru Hs Rh Mt Pd Os Ir Pt Au Ds Ag Rg Cd Hg Tl Pb Bi Po At Cn Al In Nh Si Sn Fl P As Sb Mc S Se Te Lv Cl Br I Ts He Ar Kr Xe Rn Og Lanthanides Actinides La Ce Pr Nd Pm Sm Eu Gd Tb Dy Ho Er Tm Yb Lu Ac Th Pa U Np Pu Am Cm Bk Cf Es Fm Md No Lr 23
24 Fluoride complex formation of Rf H. Haba et al., J. Am. Chem. Soc. 126, 5219 (2004). John Emsley, in NATURE S BUILDING BLOCKS, Oxford 2011 Rutherfordium: Element of surprise Rutherfordium is not like the higher member of group 4 in its behavior with fluoride ions. Like hafnium and zirconium, it forms a complex ion with six fluorides: RfF 6 2- but it does not form RfF 7 3- whereas the other two metals do. The reason appears to be that relativistic effects are coming into play and these affect the behavior of its bonding electrons. 24
25 2-2. Electrochemistry of Md & No Redox studies of the heaviest elements are expected to give valuable information on valence electronic states influenced by strong relativistic effects, such as oxidation states & redox potentials. Reduction of 101Md : Md 3+ Md 2+ Oxidation of 102No : No 2+ No Cm( 11 B, 4n) 255 Md (T 1/2 = 27 min) 248 Cm( 12 C, 5n) 255 No (T 1/2 = 3.1 min) Development of a rapid electrochemical apparatus Redox reactions with an atom-at-a-time technique Solution 25
26 Flow electrolytic column chromatography Rapid & effective redox reactions A. Toyoshima et al., Radiochim. Acta 96, (2008). Reference electrode (Ag/AgCl) Md 3+ Inlet Working electrode (Glassy carbon fibers) Counter electrode (Pt) Flow Md 3+ Md 2+ e - e - Carbon fiber Outlet Md 2+ Cation-exchanger (Nafion) Carbon rod Electrolyte solution: 0.1 M HCl Both electrochemical and cation-exchange reactions in the column Different cation-exchange behavior between the different oxidation states 26
27 Redox reactions of Md & No 120 A. Toyoshima et al., Inorg. Chem. 52, (2013). 120 A. Toyoshima et al., J. Am. Chem. Soc. 131, (2009). Reduction probability / % Eu 3+ +e - Eu 2+ Md 3+ + e - Md 2+ Oxidation probability / % No 2+ No 3+ + e Applied potential / V Applied potential / V Redox reactions based on an atom-at-a-time scale were successfully conducted with the newly developed flow electrochemical apparatus. This new technical approach will open up new frontiers of the chemistry of the transactinide elements. 27
28 3. Atomic properties of the heaviest actinides Study of atomic properties of the heaviest elements is indispensable to understand electronic ground state configurations. The first ionization potential/energy (IP 1 ) is an atomic property which most sensitively reflects the outermost electronic configuration. Precise and accurate determination of IP 1 provides significant information on the binding energy of the valence electrons and, thus, on increasingly strong relativistic effects. Electron Nucleus Inner electron orbital Outer electron orbital Contraction Expansion 28
29 3-1. First ionization energy (IP 1 ) of Lr Cover of Nature: 9 April 2015 EXTREME CHEMISTRY Experiments on rare lawrencium atoms illuminate a relativistic region of the periodic table 29
30 Valence electronic structure of Lr The ground-state electronic configuration of Lr is predicted to be [Rn]5f 14 7s 2 7p 1/2, in contrast to that of its lanthanide homolog Lu, [Xe]4f 14 6s 2 5d, as the7p 1/2 orbital is expected to be stabilized below the 6d orbital in Lr by strong relativistic effects. The determination of IP 1 sheds light on the important role of relativistic effects on the electronic structure of heavy elements. Lr: [Rn]5f 14 7s 2 7p1/2 Lu: [Xe]4f 14 6s 2 5d No IP 1 data beyond Es (Z = 99) New atom-at-a-time technique H Li Be B C N O F Ne Na Mg K Ca Sc Ti Cr Mn Fe Co Ni Cu Zn Ga Ge Rb Sr Y V Cs Ba La Zr Tc Ru Fr Ra Ac Rf Nb Mo Ag Hf Ta W Re Os Ir Pt Au Hg Tl Pb Bi Po At Rn Db Sg Bh Hs Rh Mt Pd Ds Rg Cd Cn Al In Nh Si Sn Fl P As Sb Mc S Se Te Lv Cl Br I Ts He Ar Kr Xe Og the heaviest element ion beams Lanthanides Actinides La Ce Pr Nd Pm Sm Eu Gd Tb Dy Ho Er Ac Th Tm Pa U Np Pu Am Cm Bk Cf Es Fm Md Yb No Lu Lr 30
31 Valence electronic structure of Lr The ground-state electronic configuration of Lr is predicted to be [Rn]5f 14 7s 2 7p 1/2, in contrast to that of its lanthanide homolog Lu, [Xe]4f 14 6s 2 5d, as the7p 1/2 orbital is expected to be stabilized below the 6d orbital in Lr by strong relativistic effects. The determination of IP 1 sheds light on the important role of relativistic effects on the electronic structure of heavy elements. Lr: [Rn]5f 14 7s 2 7p1/2 Lu: [Xe]4f 14 6s 2 5d No IP 1 data beyond Es (Z = 99) New atom-at-a-time technique Y. Nagame, Nature Chem. 8, 282 (2016) H Li Be B C N O F Ne Na Mg K Ca Sc Ti Cr Mn Fe Co Ni Cu Zn Ga Ge Rb Sr Y V Cs Ba La Zr Tc Ru Fr Ra Ac Rf Nb Mo Ag Hf Ta W Re Os Ir Pt Au Hg Tl Pb Bi Po At Rn Db Sg Bh Hs Rh Mt Pd Ds Rg Cd Cn Al In Nh Si Sn Fl P As Sb Mc S Se Te Lv Cl Br I Ts He Ar Kr Xe Og the heaviest element beams Lanthanides Actinides La Ce Pr Nd Pm Sm Eu Gd Tb Dy Ho Er Ac Th Tm Pa U Np Pu Am Cm Bk Cf Es Fm Md Yb No Lu Lr 31
32 Experimental set-up Complex system: surface ionization, mass separation and detection of Lr ions 249 Cf( 11 B, 4n) 256 Lr 249 Cf target T. K. Sato et al. Nature 520, 209 (2015) Skimmer Mass separation 11 B beam Gas-jet transport Ionization cavity Extraction electrode α-particle detector Ion source Lr atoms are ionized to the +1 charge state via the interaction with a solid metal surface at high temperature and is selectively mass-separated from nuclear reaction by-products. 32
33 First ionization energy (IP 1 ) of Lr IP / ev Exp ± 0.08 Cal * The good agreement with theoretical prediction obtained using relativistic calculations, which favor a 7s 2 7p 1/2 configuration in the Lr atom, supports this ground state configuration. Actinides Lanthanides This quantitatively reflects and confirms the theoretically predicted situation of closed 5f 14 and 7s 2 shells with an additional weakly-bound electron in the valence orbital. Lr: last actinide actinide series in the Periodic Table 33
34 Liquid-phase chemistry 5. Summary & Perspectives Surprising chemical properties of Rf (and 105 Db) Heavier elements: New technical development: Continuously working system consisting of a rapid chemical separation device and a flow-through α-particle detection apparatus, coupled to a recoil pre-separator Talk by Y. Komori (A-078) New approach with the heaviest element (ion) beams IP 1 Talk by Y. Nagame (A-259) Adsorption behavior of Lr Talk by T. Tomitsuka (A-209) Ion beams, Atomic & Molecular beams New frontier chemistry 34
35 ChemHaiku Oganesson (Og) The end of the line, your millisecond half-life brings down the curtain 35
36 Suggested Periodic Table up to Z 172 P. Pyykkö, PCCP 13, 161 (2011) 33
37 Thank you for your attention 37
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