Advanced Laboratory, Chemistry 471 Syllabus, Winter Semester 2007 Instructor: Office: Phone: Office Hours: Lab. Hours: Email: Dr. Les Manner 223 Romney 496-1923 MWF 10:00-11:00 am MF 2:00-4:45 pm mannerl@byui.edu COURSE DESCRIPTION: Chemistry 471 is an advanced laboratory with an emphasis on synthetic technique applicable to modern inorganic chemistry. Where applicable, the concepts and principles covered in chemistry 470 will be reinforced in this laboratory. Techniques for the synthesis, purification, and characterization of coordination complexes, organometallic compounds, and solid-state materials will be introduced. Laboratory exercises will expose students to a wide range of techniques common to inorganic synthetic chemistry including vacuum lines, Schlenk manipulations (air-sensitive compounds), and tube furnace reactions. Characterization of synthesized products will be performed by modern spectroscopic techniques such as nuclear magnetic resonance, UV-vis, infrared, and magnetic susceptibility. Molecular mechanics and quantum mechanical calculations will be performed on selected products using computational software (e.g. Spartan). Properties derived from these calculations will be compared to experimental results. RESOURCES: Textbook (required): G.S. Girolami, T.B. Rauchfuss, and R.J. Angelici, Synthesis and Technique in Inorganic Chemistry: A Laboratory Manual; University Science, 3rd Ed., 1999 Supplemental textbooks (on reserve in the library): F.A. Cotton, G. Wilkinson, Advanced Inorganic Chemistry; Wiley, 6th Ed., 1999 N.N. Greenwood and A. Earnshaw, Chemistry of the Elements; Pergamon, 2nd Ed., 1997 Ch. Elschenbroich and A. Salzer, Organometallic Chemistry; Weinheim, 2nd Ed., 1992 D.F. Shriver and M.A. Drezdzon, The Manipulation of Air-Sensitive Compounds, Wiley, 2nd Ed., 1986 Easy reading textbooks (on reserve in the library): M.J. Winter, d-Block Chemistry, Chemical Bonding, and Foundations of Inorganic Chemistry; Oxford, 1994 Reading assignments and lecture materials: For each assigned synthetic procedure you are required to read the entire applicable chapter. If you have any questions regarding the procedure, please speak with the instructor. The reading assignments are specified below. GENERAL INFORMATION AND POLICIES: Course Work The course will consist of five experiments. As noted on the schedule, these may take anywhere from one to three weeks to complete. Within two days after completion of the experiment, you will be expected to hand in your completed laboratory notebook. The score for a given experiment will be based on the completeness and quality of the work reported in your laboratory notebook. The expected format for writing your laboratory notebook will be covered during the first day of the laboratory. The final score/grade for the semester will be determined by averaging the five scores received on your experiments. There is no curve and no experiment will be dropped to calculate your final grade. A grade will be assigned as shown below: A 85 B 70 C 55 D 40 F 40 Lab Safety Safety is the single most important consideration in the design and execution of any experiment in this laboratory. You need to be aware of the potential hazards that are associated with the experiment to which you are assigned. Reading through the experimental procedure before coming to lab is one of the best ways to ensure that you are familiar with the potential hazards and precautions that must be taken. Some important safety precautions are: 1. Eye protection and close-toe shoes will be worn at all times while in the lab. Gloves should be worn when handling caustic or poisonous materials. You need to refer to the MSDS for more information on chemical hazards. 2. You should consider the potential hazards of your experiment to your labmates as well as to yourself. All laboratory equipment should be suitably secured before starting a procedure. This is particularly important in the case of reactions to be heated, and anything that is hot should be clearly indicated. Make sure tubing or wiring is routed so that no one can get caught in it. Clean up spills and broken glassware immediately. Gas cylinders must always be secured when in use. 3. Any reaction that is to be left overnight must be cleared myself prior to leaving lab. 4. Volatile materials should be handled in the fume hood. 5. Know the location of safety equipment, which includes eyewash fountains, safety showers, fire extinguishers, and safety blankets. 6. Hazardous waste must be disposed of in the proper container, and must never be poured down the drain. 7. All materials, compounds, solutions, etc. that you prepare should be properly labeled, particularly those that are stored in the refrigerator, glovebox, or oven. A label such as "Compound 1" is not acceptable. Use the correct IUPAC or other generally accepted name for a chemical compound. All such samples should also have your name or initials on it. You should refer to the Introduction of your text for more information about safe lab practices. Good laboratory etiquette is also expected. 1. For the lab to run efficiently, it must be kept the lab neat and clean. Do not leave materials or equipment lying about. Put everything away immediately when you are finished with it. 2. You are responsible for cleaning and drying your own glassware before returning it to the shelf or drawer. Remember, someone else will need the same equipment next week. Experiments: Experiment # Procedure Check-in, safety, and lab practices Experiment 12 Experiment 1 Experiment 11 Experiment 14 Experiment 23 The Paramagnetic Complex, Mn(acac)3 The 1-2-3 Superconductor YBa2Cu3O7 Metal-Metal Quadrupole Bonds Optical Resolution of [Co(en)3]3+ Copper(II) Tetraphenylporphyrinate Required time Week 1 Week 2 One week Two weeks Three weeks Three weeks Honor Code: All aspects of the BYU-I Honor Code will be observed during lecture and labs. Please dress appropriately. After taking a test, do not discuss the test with other students who have not yet taken the test. Preventing Sexual Harassment: Title IX of the Education Amendments of 1972 prohibits sex discrimination against any participant in an educational program or activity that receives federal funds, including Federal loans or grants. Title IX also covers student-to-student sexual harassment. If you encounter unlawful sexual harassment or gender-based discrimination, please contact the Personnel Office at 496-1130. Students with Disabilities: Brigham Young University-Idaho is committed to providing a working and learning atmosphere, which reasonable accommodates qualified persons with disabilities. If you have any disability which may impair your ability to complete this course successfully, please contact the (Services for Students with Disabilities Office, 496-1158). Reasonable academic accommodations are reviewed for all students who have qualified documented disabilities. Services are coordinated with the student and instructor by this office. If you need assistance or if you feel you have been unlawfully discriminated against on the basis of disability, you may seek resolution through established grievance policy and procedures. You should contact the Personnel Office at 496-1130.