SPRING 2014: 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 |
TBA |
10:50 AM - 12:05 PM |
Chem 475
Task |
Possible Grades |
Connexions account and signed up to working group |
10 |
Topic on time |
10 |
Topic goals |
20 |
Topic outline |
30 |
Topic Figures |
20 |
Topic draft |
20 |
Copyright |
10 |
Topic word |
50 |
Topic upload |
10 |
Final corrections due |
15 |
Homework #1 |
25 |
Homework #2 |
25 |
Homework #3 |
25 |
Class presentation |
30 |
Total grade |
300 |
Elemental composition
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.
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.
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.
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
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
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.
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.
Homework
Projects
Possible ModuleTopics |
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Total Carbon, TOC, TIC |
SIMS |
UV visible ? |
Multidemensional NMR |
Fast Atom Bombardment |
Liquid chromatography |
Gas chromatography |
Supercritical fluid chromatography |
Ion chromatography |
Neutron activation analysis |
EXAFS |
Thermal conductivity |
Dielectric thermal analysis |
Band gap measurements of QDs |
Viscosity |
Dynamic light scattering |
Strength and deformation testing |
Gas and liquid permeability |
Microwave structure determination |
Multidimensional NMR |
Determination of energetics of fluxional species by NMR |
CONNEXIONS SITE
In order to upload your project content to the Connexions Site,
please follow the instructions for creating a module - http://cnx.org/
NAME |
PROJECT TOPIC |
PROJECT GOALS |
Date of
Presentation |
REFERENCES |
PROJECT
(PDF)
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EXAFS |
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TOC, TIC, Total Carbon |
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Thursday,
April 17 |
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Garcia Piantanida, Alejandra L. |
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Gas chromatography |
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Tuesday
April 15 |
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Neutron Activation Analysis (NAA) |
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Tuesday
April 15 |
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General principles of 2D NMR |
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Tuesday
April 15 |
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Liquid chromatography |
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Tuesday,
April 22 |
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Dynamic light scattering |
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Thursday,
April 17 |
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Supercritical fluid chromatography |
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Thursday,
April 17 |
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Determination of energetics of fluxional compounds by NMR |
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Thursday,
April 17 |
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Attenuated Total Reflection-FTIR |
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Tuesday,
April 22 |
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Fast Atom Bombardment MS |
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Tuesday,
April 22 |
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Viscosity |
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Tuesday,
April 22 |
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Ion Chromatography |
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Tuesday
April 15 |
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Band gap measurements of quantum dots |
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Tuesday,
April 22 |
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SIMS |
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Thursday,
April 17 |
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Multidimensional NMR |
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Thursday,
April 17 |
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Tuesday,
April 22 |
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