SPRING 2010: 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
SS 337
Tues/Thurs 10:50 AM - 12:00 PM

PLEASE NOTE: THERE WILL BE NO CLASS ON THURSDAY, FEBRUARY 25

Chem 475

Elemental composition

1. Combustion analysis

2. ICP AA

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.

3. EDX

i. 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.

ii. 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.

1. XPS

2. Auger

i. 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.

1. RBS

 i. 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.

1. NMR

i. 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.

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

Physical and Thermal

1. Melting point

2. DTA

3. DSC

4. TGA

Chemical speciation

1. MS

2. IR

3. XPS

4. Auger

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.

1. NMR

i. 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.

ii. 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.

iii. 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.

iv. 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.

v. 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.

vi. 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.

vii. 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

1. EPR

i. 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.

1. Magnetic suseptability

2. UV

Dynamic processes

1. NMR

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,C., 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.

2. TGA

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

ii. 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.

iii. 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.

3. UV

Molecular structure

1. XRD powder

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.

1. Single crystal XRD

i. 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.

ii. 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.

iii. 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.

1. Electron diffraction

i. 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.

ii. 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.

iii. 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

1. Neutron diffraction

2. NMR

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

Nano to Micro

1. Particle size

2. SEM

3. TEM

4. AFM

5. 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

PowerPoint #2

 

Projects

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Example of paper in final format

NAME
PROJECT TOPIC
PROJECT OUTLINE
Brittany Oliva
UV Detection of Silicon Quantum Dots
Zheng Yan
Characterization of graphene by Raman Spectroscopy
Lauren Harrison

1) Analyzing modified surfaces in XPS

2) Using XPS to analyze metal nanoparticles
Ariana Bratt
XPS of Carbon Nanomaterials
Courtney Payne
Using SERS for surface studies of gold nanoparticles
Meghan Jebb
ICP-MS (comparison with ICP-AES with specific examples)
Yen-Tien Lu
TEM image for multilayers-nanomaterial
Yen-Hao Lin
Size exclusion chromatography and its application on polymer science
Jiebo Li
FTIR of Metal-ligand
Ryan Thaner
Atomic Force Microscopy (AFM) of Carbon Nanomaterials
Sravani Gullapalli
UV-Vis and Photoluminescence spectroscopy of II-VI semiconductor nanoparticles
Varun Shenoy Gangoli
NMR Techniques to Measure Specific Surface Area of Nanoparticle Suspensions
Zhun Zhao
Gas chromatography of the detection of chlorinated compounds PCE, and its reductive products
Charles Conn
Characterizing microparticles via confocal microscopy
Kewei Huang
Fluorescence Charaterization and Its application
Xianyu Li
Current-voltage to measure the electronic property of the solar cell
Xiewen Wen
Pump-probe technology

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