This project is designed to develop the research skills that are required to tackle projects that are larger and more complex than those encountered in first and second year chemistry courses. The lab is an integrated project-oriented laboratory including synthesis and the use of instrumental techniques such as UV-Visible and infrared, 1H-NMR and 13C-NMR spectrometry, chromatography (HPLC, TLC) and cyclic voltammetry. Attention also will be paid to developing general laboratory skills such as lab safety, literature searching, experiment design, working with laboratory instruments, keeping a laboratory notebook and oral presentation
Usually students will work together in groups. Each student (or group) will undertake three or four projects, of 3-4 weeks duration, chosen in consultation with the laboratory instructors. At the beginning of each project students will meet together with the laboratory instructors to generate a detailed plan for laboratory work. This phase includes literature searching, study and presentation of the framework of the project, experiment design and optimization (if appropriate), familiarization with instruments, and detailed planning of the experimental procedures. In addition, students will answer all questions in the procedures when appropriate. Students are required to write appropriate pre-lab in their laboratory notebooks for each day's activities.
This is one of five projects that students in Advanced Laboratory perform in the spring semester. Students work in groups of two or three. The project is usually three weeks long involving two three hour periods in a week.
Students will be able to carry out more extended synthetic procedures.
Students will learn to use various analytical instrumentation to characterize the complexes.
Students will write at least a six page lab report.
Students will incoporate the experimental data into the report and interpret the data in relation to the structural changes observed in the complexes.
Students will learn to communicate their report in an oral presentation.
- IR spectrophotometer
- All reagents are provided.
Students are required to consult the given references for the necessary procedures.
Day 1: Cracking of dicyclopentadiene and the synthesis of ferrocene (Reference: Woollins, J. D., editor; Inorganic Experiments; VCH publisher, Inc., New York, NY. 1994;)
Day 2: Determine the melting pt. of ferrocene. Record the IR and the UV-vis (in ethanol) spectra of ferrocene, 1H NMR (in CDCl3) spectra of ferrocene. Record the cyclic voltammogram of ferrocene (in CH2Cl2 with tetrabutylammoniun hexaflorophosphate as supporting electrolyte).
Day 3: Synthesis of acetylferrocene from ferrocene (Reference: Woollins, J. D., editor; Inorganic Experiments; VCH publisher, Inc., New York, NY. 1994; p60)
Day 4: Determine the melting pt. of acetylferrocene. Record the IR and the UV-vis (in ethanol), 1H NMR (in CDCl3) spectra of acetylferrocene. Record the cyclic voltammogram of acetylferrocene (in CH2Cl2 with tetrabutylammoniun hexaflorophosphate as supporting electrolyte).).
Day 5: Reduction of acetylferrocene with LiAlH4 (Reference: Hamilton, D. E.; J. Chem. Educ. 1991, 68, A143)
Day 6: Record the melting point, IR and the UV-vis (in ethanol), 1Hnmr (in CDCl3) spectra of ferrocenylethanol. Record the cyclic voltammogram of ferrocenylethanol (in CH2Cl2 / tetrabutylammoniun hexaflorophosphate as supporting electrolyte).). Resolution of enantiomers by HPLC (Reference: Armstrong, D. W.; DeMond, W.; Czech, B. P.; Anal. Chem. 1985, 57, 481-484.)