Text Box:

Patrick J. Desrochers

(501) 450-5936

Manion Hall, Rm 205

patrickd@uca.edu

Office hours (drop in times):

Text Box: Course Links

Chem 3150, Advanced Inorganic Laboratory

Spring 2016

Laney 302
Tu 10:50 am - 1:30 pm

 

Other times available by appointment.

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 HxWO3 and WO3

Observe time and air effects on HxWO3

Determine W redox states involved

Characterize the W…...H interaction in HxWO3

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 AlF6and 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)6and Fe(CN)64-

Chemically oxidize Fe(CN)6 to Fe(CN)63-

Determine the meff 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 Mo2Cl84-

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 FeIII(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 Cu
2+(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