Instructor: Dr. Gregory L. Milligan
Lecture days: M, W, F 10:00-10:50
Lab days: Open
Classroom: Room 100
Office: Room 103
Office hours: M, U, W, F 11:00-11:50 U, H 12:00 – 12:50
Textbook: F. Rouessac and A Rouessac, Chemical
Analysis, Modern Instrumentation Methods and Techniques, John Wiley and
Sons,
Midterm Exams: Friday, March 2; Friday, April 20
Final exam date: TBA
Grading: 10 Experiments @ 15 points each = 150 points
2 Midterm Exams @ 50 points each = 100 points
1 Final exam @ 100 points = 100 points
Total = 350 points
The purpose of this course is to introduce the student to modern methods of molecular structure analysis. As an upper-division course, the concepts will be a bit more challenging, the techniques more demanding, and the equipment more sophisticated than lower division. Furthermore, the student will need to call upon his or her judgment and ingenuity to solve problems that inevitably will be encountered.
Experiments are worth 15 points each. One midterm and a final exam will be given. The midterm will last about 1/2 hour and will be worth 50 points. The final will last about 1 hour, and will be worth 100 points. Final grades will be assigned the “old-fashioned” way: 90-100% = “A”, 80-89% = “B”, 70-79% = “C”, 60-69% = “D”, and below 60 = “F”.
Safety is of the utmost importance. No experiment is worth an injury. The most important piece of safety equipment
is the brain of the student. Think about
what you are doing all the time. Ask yourself
if you are doing things in the safest way possible. Plan for the worst. No work may be done
outside of scheduled lab times unless approved by the instructor!
Safety glasses MUST be worn AT ALL TIMES in the lab. The glasses must be in place before the student enters the lab, or first thing upon arrival. I strongly suggest that the student wear a lab coat or apron. This need not be elaborate; an old shirt or apron worn over street clothes offers a measure of protection. Aprons are available in the lab for students' use. Under no circumstances may the student wear shorts, short skirts, or open-toed shoes. Latex and vinyl gloves are provided for students' use in the lab but be aware that the gloves, vinyl especially, are attacked by organic solvents and offer only limited, temporary protection.
The textbook will be followed loosely; sometimes a handout will provide details of the day's work. All relevant sections of the text should be read before the experiment is begun. In most cases, any handouts will be available for download from the instructor's web site.
Each student will keep a proper notebook. Notebooks may be purchased at the Bookstore. You may use a notebook from General or Organic Chem. Lab as long as it has duplicate, numbered pages. All notations and calculations must be written in the notebook; not on any other piece of paper. The student will write down everything that can be written down in advance of the actual experiment. When the experiment is performed, any changes from the original plan are noted, as are any observations made. When an item needs to be changed, it is crossed out with a single line and the new item is added. After the experiment is done, the student completes all calculations and data analysis in the notebook. The report that is turned in is a carbonless copy of the notebook pages for that experiment; as such, it is not expected to be a “cleaned-up” version of events. It will have crossed-out mistakes and changes, spills, burn marks, etc. This will not affect the grade for the lab; what counts is that the required items are present. The student is expected to learn to use ChemSketch to generate structures for inclusion in lab reports.
Finally, the student is reminded that labs are fun! If you work safely and efficiently, I am confident you will find this lab enjoyable and rewarding.
If you need course adaptations or accommodations because of a disability, if you have medical and/or safety concerns to share with me, or if you need special arrangements in case the building must be evacuated, please make an appointment with me as-soon-as possible.
Schedule
Week of 1/15 Intro to instruments: colorimetry
Week of 1/22 Infrared Spectroscopy
Week of 1/29 Ultraviolet Spectroscopy
Week of 2/5 Intro to 1H NMR spectroscopy
Week of 2/12 1H NMR cont
Week of 2/19 Heteronuclear NMR
Week of 2/26 Two-dimensional
NMR; COSY, HETCOR, APT, DEPT spectra
Week of 3/5 NMR continued
Week of 3/19 Mass
Spectrometry
Week of 3/26 Gas chromatography
Week of 4/2 High
Performance Liquid Chromatography
Week of 4/9 HPLC, GC continued
Week of 4/16 Atomic absorption/emission/ICP
spectroscopy
Week of 4/23 Electroanalytical Chemistry
Week of 4/30 Voltammetry/potentiometry
Week of 4/25 Wrap-up
Experiments
Colorimetric determination of iron in water
IR analysis of known and unknown compounds
UV-Vis spectra of known and unknown compounds
1H NMR of known compounds
1H NMR of unknown compounds
13C NMR of known and unknown compounds
31P and 19F spectra of known and unknown compounds
2-D NMR spectra of known and unknown compounds
GC analysis of an unknown mixture
HPLC analysis of an unknown mixture