Experiments

Objectives

Tools

First Day Practice

Manipulation of an airfree sample.

UV-vis, ATR IR, and EPR spectrometers

Electronic presentation of spectral data

UVvis, IR, EPR

Inert atmosphere cannula transfer

WO₃/H₂ intercalation

Compare conductivities of H_xWO₃ and WO₃

Observe time and air effects on H_xWO₃

Determine W redox states involved

Characterize the W^…...H interaction in H_xWO₃

IR, Mag. Suscept.

conductivity

Ammine-borane hydrolysis

Investigate the M²⁺ hydrolysis of NH₃BH₃

Monitor hydrolysis by H₂ evolution & ¹¹B NMR

IR, NMR (¹¹B and ¹H)

Al³⁺ solution chemistry

Characterize Al³⁺ species at high and low pH.

Contrast the ¹⁹F NMR of AlF₆^3– and PF6‾

Monitor Al³⁺ binding to natural dye and MPD

²⁷Al, ¹⁹F NMR

Co-NO₂ linkage isomers

Prepare [Co(ONO)(NH₃)₅]Cl₂

Investigate linkage using ATR IR spectroscopy

Investigate base-catalyzed isomerization in

   using UV-vis spectroscopy

UVvis, IR (variable T), NMR (⁵⁹Co?)

Iodine-PPh₃

Monitor the reaction of PPh₃ with I₂ by NMR and

   electronic spectroscopy

UV-vis, ³¹P NMR

Metal Complex UVvis/magnetism

Contrast transition metal complexes

   1. d-to-d transitions

   2. ligand spectrochemical series

   3. magnetism vs dⁿ electron count

   4. complex ion symmetry

   5. Mⁿ⁺ charge effects on ligand field

Interpret electronic spectra using
  Tanabe-Sugano diagrams

UVvis, NMR (⁵⁹Co?)

Scorpionate synthesis

Prepare KTp* using MW heating

Prepare Tp*-complexes of Ni(II), Zn(II), Fe(III)

Characterize by IR, NMR, UVvis

MW assisted synthesis

IR, UV-vis, NMR (¹H, ¹³C, ¹¹B)

Redox behavior of iron complexes

Record CV’s for Fe(CN)₆^3– and Fe(CN)₆^4-

Chemically oxidize Fe(CN)₆^4– to Fe(CN)₆^3-

Determine the m_eff of K₃Fe(CN)₆

Contrast IR of Fe(II)-CN vs Fe(III)-CN

IR, E-chem

RuCl₂(dppb)(phen) isomerism

Prepare RuCl₂(phen)(dppb)

Document cis/trans isomerization by ³¹P NMR Contrast cis/trans forms by cyclic voltammetry

Inert atmosphere, NMR (³¹P), E-chem

(bipy)PtCl₂

Prepare (bipy)PtCl₂ using MW heating

Characterize by ¹⁹⁵Pt and ¹H NMR

Monitor additional ligand-substitution reactions

NMR (¹⁹⁵Pt)

Mo-Mo quadruple bonded complex

Prepare a sample of Mo₂(O₂CCH₃)₄

Characterize by ATR IR, diffuse refl. UV-vis

Prepare sample of Mo₂Cl₈^4-

Inert atmosphere, MW assisted synthesis

IR, diffuse reflectance UV-vis

Other Experiments
(not available this year)

Objectives

Tools

Synthesis of ND₃ and HD gases

Prepare ND₃ from Mg₃N₂ and D₂O

²H and ¹H NMR

Tube furnace

Metal-porphyrins

Investigate spin of Fe^III(TPP)⁺ as a function of

   axial ligation

Investigate the spectra of Ni(TPP) in the
   presence of coordinating ligands

NMR, Mag. Suscept.

Doped ZnS phosphors

Prepare Mn-doped ZnS phosphors

Confirm luminescence of phosphors

Study variable Cu or Mn doping on luminescence

UV exposure, fluorescence?,
Tube furnace

Cu(Gly-Gly) hydroxyl radicals

Compare hydroxyl radical formation by
             Cu(Gly-Gly) vs Cu²⁺(aq)

Cu(en)_x²⁺, Ni(en)_y²⁺ Job plots

Determine x for Cu(II) and y for Ni(II) using the
   Job plot method

Contrast these two different metal ions.

Spec 20