CHEMISTRY 445
INORGANIC PREPARATIONS AND TECHNIQUES
SPRING 2010
Instructor: Dr. Keith M. Davies
Office Hours:
Tu 10:30-12:00 (331 ST1)
MWF (410 Occoquan, PW) by appointment
703-993-1075
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CHEM 445 is a six hour/week laboratory course involving the synthesis, purification, and spectroscopic characterization of inorganic compounds. A variety of inorganic and organometallic coordination compounds will be prepared. Techniques involving inert-atmosphere manipulations, microscale and template synthesis and magnetic susceptibility measurements (Evans Balance) will be employed. Products will be purified by thin layer and column chromatography and characterized by I.R. (KBr disk), UV-visible and NMR spectrophotometry.
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Experiments |
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1. |
Preparation of [Co(NH3)5Cl]Cl2 and [Co(NH3)5 NO2]Cl2 |
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Preparation and [Co(NH3)5DMF](NO3)3. Spectroscopic Identification of the Donor Atom by UV, IR, and NMR Spectra |
| 3. | Preparation of [Co(NH3)5ONO]Cl2. Kinetics of Solid State Isomerization to [Co(NH3)5NO2 ]Cl2 by IR spectroscopy |
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4. |
Mn(acac)3.
Preparation
and magnetic susceptibility measurement. UV-visible spectra |
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5. |
Chromatography of Ferrocene Derivatives. Separation of Ferrocene and
Acetyl-Ferrocene using Thin Layer and Column Chromatography. I.R., NMR,
Spectra |
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6. |
Organometallic Synthesis and IR Spectra of Molybdenum Carbonyl Compounds. Mo(CO)4(piperidine)2 and cis- and trans-Mo(CO)4(PPh3)2. |
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7. |
Microscale Synthesis: Vaska's Complex, IrCl(CO)[P(C6H5)3]2 and its O2 adduct. Wilkinson's Catalyst, RhCl(PPh3)3. IR Spectra. |
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8. |
Preparation of
Molybdenum(II) Dimers.
Tetra(acetato)dimolybdenum(II), Mo2(O2CCH3)4 and Potassium
Octachlorodimolybdate(II), K4Mo2Cl8.2H2O.
UV-visible and IR Spectra.
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9. |
Preparation of Schiff Base Ligand,
N,N'-Bis(salicylaldehyde)ethylenediamine, salenH2, and Co(II)salen |
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Text: Synthesis and Techniques in Inorganic Chemistry,
3rd Edition, by G. Girolami, T. B. Rauchfuss and R. J. Angelici.
University Science Books, 1999.
Inorganic Preparations and Techniques Laboratory Course Supplement. Copy Shop.
Supplementary Reading:
Microscale Inorganic Chemistry by Z. Szafran, R. M. Pike and M. M. Singh. J. Wiley, 1991.
Infrared and Raman Spectra of Inorganic and Coordination Compounds by K. Nakamoto. 4th edition,1986.
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Chemistry 445 Course Requirements/Procedures.
Experiments should normally be done individually. If experiments have to be done in pairs, it is expected that both students involved will be present during the experiment. Credit for experiments done in pairs will not be given to a student who is absent and not involved in the whole experiment. Lab reports should be written up individually. It is an honor code violation to hand in data that you have not collected, to claim credit for an experiment that you have not carried out or to copy the experimental write up of any other student.
Students should keep a lab notebook into which they should record, during the lab period itself, details of experimental procedures carried out and all weighings and experimental results obtained.
Completed experiments should be written up as typed reports.
Reports, accompanied by products and spectra, should be submitted for grading by the due dates indicated in the lab report schedule below.
Safety glasses must be worn in the laboratory at all times. Any work carried in the laboratory outside of the scheduled class period, must first be authorized by the instructor.
Laboratory Reports
Completed experiments should be written up as typed reports, which should include:
(1) Introduction This should be fairly brief (<one page) with some background (and minimal theory).
(2) Experimental Procedure A concise description of what you did in the lab, preferably written in the past tense (i.e. describe what was done (past tense/passive voice) rather than a set of instructions).The style should resemble the Experimental Section of a research paper in the literature. It should be short and concise. It should include all relevant chemical equations.
(3) Data/Results This should include all measurements you have made in the laboratory. If not numerical data, it should describe things observed or found (i.e. a description or sketch of the separations observed on the TLC plates). The Results section is a very important part of the report as it shows the results of your efforts in the course. This section should also contain a calculation of the theoretical and % yield in a synthesis, which may be neatly hand-written. It should contain a summary of kinetic data (Abs/Time/log Abs) or spectral data (λmax values) etc. Data should be organized in tabular form where possible.
(4) Calculations (of magnetic moments or kinetic rate constants etc) should follow, but should be separate from the results. All original spectra (or copies of them) should be attached. Spectra should identify what compound it describes, the date it was taken and should identify the relevant bands in an IR, UV or NMR spectrum.
(5) A conclusion summarizing the findings of the experiment.
The lab report:
i) should enable someone, other than the instructor, with no prior knowledge of the experiment, to read and understand what you have done and found.
ii) does not need a list of chemicals or equipment used.
iii) does not need a long theoretical section copied from the book.
iv) should be written is a short and concise style resembling the experimental section of a research paper in the literature.
v) should include all relevant chemical equations.
Lab