SPRING 2012: CHEM 475 - PHYSICAL METHODS IN INORGANIC CHEMISTRY

College: School of Natural Sciences
Department: Chemistry

A survey course of research techniques used in modern inorganic chemistry. Topics covered will include X-ray diffraction, matrix isolation, mass spectrometry, magnetism, electrochemistry, and various spectroscopies (IR, Raman, UV-Vis, NMR, EPR, XPS, EXAFS, and Mossbauer). Open to undergraduates by special permission only.  Session: Full Term

Faculty
Email
Telephone
Location
Time
Andrew Barron
arb@rice.edu
713-348-5610
GRB W212
10:50 AM - 12:05 PM

 


Chem 475

Elemental composition

Combustion analysis, ICP AA, EDX , XPS, Auger, RBS, and NMR

i. Reagent control over the size, uniformity, and composition of Co-Fe-O nanoparticles. C. Crouse and A. R. Barron, J. Mater. Chem., 2008, 18, 4146-4153.

ii. Reaction bonded refractory metal carbide/carbon composites. A. N. MacInnes, A. R. Barron, J. J. Li, and T. R. Gilbert, Polyhedron , 1994, 13 , 1315-1327.

iii. The synthesis of chalcopyrite semiconductors and their solid solution by microwave irradiation. C. C. Landry, J. Lockwood, and A. R. Barron, Chem. Mater., 1995, 7, 699.

iv. The interfacial mixing of silicon coatings on niobium metal: a comparative study. P. D. Stupik, M. M. Donovan, A. R. Barron, T. R. Jervis, and M. Nastasi, Thin Solid Films. , 1992, 207 , 138.

v. Epoxidation and deepoxidation of single-walled carbon nanotubes: quantification of epoxide defects. D. Ogrin, J. Chattopadhyay, A. K. Sadana, E. Billups, and A. R. Barron, J. Am. Chem. Soc., 2006, 128 , 11322-11323.

vi. A new method for the determination of trialkylaluminum content in alumoxanes. A. R. Barron, Organometallics, 1995, 14, 3581-3583.

Physical and Thermal

Melting point, DTA , DSC, and TGA

Chemical speciation

MS, IR, XPS, Auger, NMR, EPR, Magnetic suseptability, and UVvis

i. A spectroscopic evaluation of the efficacy of two mass deacidification processes for paper. A. N. MacInnes and A. R. Barron, J. Mater. Chem. , 1992, 2 , 1049.

ii. Reactions of alumino-polyhydride complexes of tungsten. X-ray crystal structures of [Me 3 P) 3 H 3 W( m -H) 2 AlCl( m -N=CHEt)] 2 , {[Me 3 P) 3 WH 5 ]Li} 4 , (Me 3 P) 3 WH 2 I(SiMe 3 ) and (Me 3 P) 3 H 2 W( m -H) 3 AlCl 2 NMe 3 . A. R. Barron, G. Wilkinson, M. Motevalli, and M. B. Hursthouse, J. Chem. Soc. , Dalton Trans. , 1987, 837-846.

iii. Synthesis and characterization of triethylsiloxy-substituted alumoxanes: their structural relationship to the minerals boehmite and diaspore. A. W. Apblett, A. C. Warren, and A. R. Barron, Chem. Mater ., 1992, 4 , 167.

iv. Hydrolysis of tri- tert- butylaluminum: the first structural characterization of alkylalumoxanes, [(R 2 Al) 2 O] n and (RAlO) n . M. R. Mason, J. M. Smith, S. G. Bott, and, A. R. Barron, J. Am. Chem. Soc ., 1993, 115 , 4971.

v. Acylation and esterification of the aryloxide ligand in AlMe(DBMP) 2 . M. B. Power, A. R. Barron, S. G. Bott, E. J. Bishop, K. D. Tierce and J. L. Atwood, J. Chem. Soc., Dalton Trans. , 1991, 241-247.

vi. The interaction of tris- tert -butylgallium with white phosphorus: Isolation of an unusual gallium phosphorous cluster. M. B. Power and A. R. Barron, Angew. Chem., Int. Ed. Engl. , 1991, 30 , 1353-1354.

vii. Tailoring aqueous solubility of functionalized single-wall carbon nanotubes over a wide pH range through substituent chain length. L. Zeng, L. Zhang, and A. R. Barron, Nano Lett . 2005, 5 , 2001.

viii. Solid state 13 C NMR of fluorinated single-wall carbon nanotubes (F-SWNTs): using just MAS to attenuate 13 C- 19 F dipole-dipole interactions, obtain narrow and unusually shielded 13 C signals, and assess extent of fluorination, L. B. Alemany, L. Zeng, L. Zhang, C. L. Edwards, and A. R. Barron, Chem. Mater., 2007, 19, 735

ix. Radical anion complexes of tris-(1,3-diphenyltriazenido) aluminum. J. Braddock-Wilking, J. T. Leman, C. T. Farrar, S. C. Larsen, D. J. Singel, and A. R. Barron, J. Am. Chem. Soc ., 1995, 117 , 1736.

 

Dynamic processes

NMR, TGA, and UV

i. A new mechanism for cement hydration inhibition: solid-state chemistry of calcium nitrilotris(methylene)triphosphonate, M. Bishop, S. G. Bott, and A. R. Barron,Chem. Mater.., 2003, 15 , 3074-3088.

ii. Reactivity of organogallium peroxides: oxidation of phosphine, phosphites and triphenylarsine. X-ray crystal structures of ( t Bu) 2 Ga(O t Bu)(O=AsPh 3 ), ( t Bu) 2 Ga( m - O t Bu)( m -OO t Bu)Ga( t Bu) 2 and ( t Bu) 2 Ga[(O)P(Ph) 2 CH(O)P(Ph) 2 ]. M. B. Power, J. W. Ziller, and A. R. Barron, Organometallics , 1993, 12 , 4908.

iii. Sterically crowded aryloxide compounds of aluminum: reduction of coordinated benzophenone. M. B. Power, J. R. Nash, M. D. Healy, and A. R. Barron, Organometallics , 1992, 11 , 1830.

iv. Steric effects in aluminum compounds containing monoanionic potentially bidentate ligands: towards a quantitative measure of steric bulk. J. A. Francis , C. N. McMahon, S. G. Bott, and A. R. Barron, Organometallics , 1999, 18 , 4399-4416.

v. Substituent effects on the volatility of metal b -diketonates, B. D. Fahlman and A. R. Barron, Adv. Mater. Optics Electron ., 2000, 10 , 223-232.

vi. Increased volatility of barium metal organics by the use of nitrogen Lewis bases. J. M. Buriak, L. K. Cheatham, J. J. Graham, R. Gordon, and A. R. Barron, Mat. Res. Soc. Symp. Proc., 1991, 204 , 545.

vii. 1,4-Dioxobenzene compounds of gallium: reversible binding of pyridines to [{( t Bu) 2 Ga} 2 ( m -OC 6 H 4 O)] n in the solid state. L. H. van Poppel, S. G. Bott, and A. R. Barron, J. Am. Chem. Soc ., 2003, 125 , 11006-11017.

 

Molecular structure

XRD powder, Single crystal XRD, Electron diffraction, and NMR

i. The synthesis of chalcopyrite semiconductors and their solid solution by microwave irradiation. C. C. Landry, J. Lockwood, and A. R. Barron, Chem. Mater., 1995, 7 , 699.

ii. Crystal structure of Al( t Bu) 3 (NH 2 CH 2 CH 2 Ph): a molecular "slinky", C. L. Aitken and A. R. Barron, J. Chem. Cryst. , 1996, 26 , 297

iii. Tert- amyl compounds of aluminum and gallium: halides, hydroxides and chalcogenides. C. J. Harlan, E. G. Gillan, S. G. Bott, and A. R. Barron, Organometallics , 1996, 15 , 5479-5488.

iv. An accuracy assessment of the refinement of partial metal disorder in solid solutions of Al(acac) 3 and Cr(acac) 3 . B. D. Fahlman, S. G. Bott, and A. R. Barron, J. Chem. Soc., Dalton Trans ., 2001, 2148-2147.

v. Chemical vapor deposition of cubic gallium sulfide thin films: a new meta-stable phase. A. N. MacInnes, M. B. Power, and A. R. Barron, Chem. Mater ., 1992, 4 , 11.

vi. Vapor phase laser photochemistry and determination by electron diffraction of the molecular structure of [( t Bu)GaS] 4 : evidence for the retention of the Ga 4 S 4 cubane core during the MOCVD growth of cubic-GaS. W. M. Cleaver, M. Späth, D. Hnyk, G. McMurdo, M. B. Power, M. Stuke, D. W. H. Rankin, and A. R. Barron, Organometallics , 1995, 14 , 690.

vii. Molecular structures of M( t Bu) 3 (M = Al, Ga, In): A study by electron diffraction and ab initio molecular orbital calculations, A. Keys, P. T. Brain, C. A. Morrison, R. L. Callender, B. A. Smart, H. E. Robinson, D. W. H. Rankin and A. R. Barron, Dalton Trans., 2008, 404-410

viii. Adducts of trimethyaluminium with phosphine ligands; electronic and steric effects. A. R. Barron, J. Chem. Soc., Dalton Trans. , 1988, 3047-3050.

Nano to Micro

Particle size, SEM, TEM, AFM, and VLS

i. Phosphonate mediated surface reaction and reorganization: implications for the mechanism controlling cement hydration inhibition. C, Lupu, R. S. Arvidson, A. Lüttge and A. R. Barron, Chem. Commun ., 2005, 2354-2356.


Handouts

PowerPoint #1 - TBA

PowerPoint #2 - TBA

 


Projects

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NAME
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PROJECT
PROJECT
Laurie Cullum Combustion Analysis
Huilong Fei Ion Selective Electrode Analysis
Graham Piburn Energy Dispersive X-ray Analysis
  Hydrogen Analysis by RBS
Shawdon Molavi Melting Point Analysis
Basil Shadfan DSC
Paul Derry IR Sample Preparation: A Practical Guide
  Far IR Spectroscopy: M-L Vibrations
Amanda Jones Auger Spectroscopy
  Quadruple Nuclea NMR
Mayra Hernandez Rivera Lanthanide Shift Reagents
Jarrod Boyd NMR Spin-Spin Coupling
  Analysis of Multi isotope NMR Spectia
Gabriel Oaxaca Solid State NMR
  Stop-flow Reaction Measurements
Chengmin Jiang Chemical Kinetics by NMR
Linyuan Xin Gas Phase Electron Diffraction
Gabriela Escalera Neutron Diffraction
Michelle LaComb Scanning Tunneling Microscopy
Juan Velazquez Thermal Conduction Measurements
Yongji Gong Band Gap Measurements
  Surface Hardness
Sehmus Ozden Molecular Weight of Polymers
Tawana M. Robinson Solution Molecular Weight of Small Molecules

 

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