I. INSTRUMENTAL ANALYSIS
SEMESTER: FALL 2003
PREREQUISITE: CH 03224 or CH 03226
LECTURE/LAB HOURS: M 1-4 PM
OPEN LAB HOURS: TBA
II. INSTRUCTOR: Dr. Salim M. Diab
OFFICE: Room 215, St. Albert
PHONE: 740-3855 (Ext. 855)
OFFICE HOURS: MWF 11:00 - noon
HOME PHONE: 730-8302
email: sdiab@stfrancis.edu
Homepage: http://www.stfrancis.edu/ns/diab/etherman.htm
III. COURSE DESCRIPTION: This course is designed to give the students a broad experience in the theory of instrumentations. The labs will be investigative in nature where students are required to use the Internet and the Chemical literature to explore practical ways of using instruments for solving chemical problems qualitatively and quantitively. The students will survey the theory and application of instruments such as: visible, ultra violet, Infra red, Fluorescence, Nuclear Magnetic Resonance, Atomic absorption, Chromatography, and Mass Spectrometry.
COURSE OBJECTIVES: Upon successful completion of this course, the student should be able to:
1. understand and appreciate the role of instruments in solving problems
in the physical, chemical and biological sources.
2. understand the theoretical concepts behind each instrument.
3. operate, manipulate, and generate data for each instrument.
4. appreciate the connectivity between math, physics, chemistry, and
biology in this course.
5. solve chemical problems quantitatively and qualitatively by making
appropriate choices among the various instruments.
6. appreciate the complexity of each instrument, its strength, and
its limitation.
7. explore the use of Internet (Netscape) as an educational source
in instrumentation
IV. REQUIRED TEXTS/ MATERIALS:
1. Principles of Instrumental Analysis, 5th edition, Skoog, Holler,
and Nieman, saunders, 1998.
2. Lecture notes packet to accompany above text, S. Diab, editor.
3. A 3 1/2" computer disk to be used for lab portfolio.
4. Course Supplement: http://www.stfrancis.edu/ns/diab/Insanalysis.htm
ADDITIONAL REFERENCES:
1. Instrumental Methods of Analysis, 5th edition, Willard, Merritt,
and Dean.
2. Introduction to Chromatography, Bobbitt, Schwarting, and Gritter.
3. Absorption of Light and Ultraviolet Radiation: Fluorescence and
Phosphorescence Emission, Shenk.
4. Spectroscopic Methods in Organic Chemistry, 3rd edition, Williams
and Fleming.
5. High Resolution NMR, Becker.
6. Spectroscopic Techniques for Organic Chemistry, Cooper.
7. NMR of Chemically Exchanging Systems, Kaplan and Fraenkel.
8. Applied Headspace Gas Chromatography, Kolb.
9. Analytical Atomic Absorption Spectroscopy, Van Loom.
10. High Performance Mass Spectroscopy, Gross.
11. Applications of Absorption Spectroscopy of Organic ompounds, yer.
12. Infrared Spectroscopy, 2nd edition, Conley.
13. Introductory Mass Spectrometry, Shrader.
14. Nuclear Magnetic Resonance, Paudler.
15. Spectrometric Identification of Organic Compounds, 4th edition,
Silverstein, Bassler and Morrill.
16. More Spectroscopic Problems in Organic Chemistry, 2nd edition,
Baker, Cairns, Eglinton and Preston.
17. Organic Spectral Problems, Dyer.
18. Analytical Chemistry, 3rd edition, Christian.
19. Fundamentals of Analytical Chemistry, 2nd edition, Skoog and West.
20. Analytical Chemistry - 2nd edition, Pietrzky and Frank.
21. Internet Web Sites (see attachment).
LECTURE TOPICS TO BE COVERED:
Ch. 5:Introduction/Signal
and Noise
Solve problems: 5-2, 5-8, 5-12
Ch. 6,7,13:Electromagnetic
Radiation/Instruments for Optical Spectroscopy/Absorption Spectra
Solve problems: 6-1, 6-3, 6-4, 6-6, 6-7,
6-11/ 7-1, 7-8, 7-10, 7-11, 7-13, 7-15, 7-19
13-1(d-f), 13-2(d-f), 13-4, 13-6, 13-8,
13-13(e-h), 13-19
Ch. 14,15,16:UV-VIS
Spectroscopy/Molecular Fluorescence/IR Spectroscopy
Solve problems: 14-6 (b), 15-1, 15-5, 15-6
(a & d), 16- 2, 16-8, 16-11,
IR supplementary assignment.
Ch.19: NMR Spectroscopy
Solve
problem: 19-1, 19-10, 19-24, 19-28, 19-30
Ch. 26,27:Chromatography/Mass
Spectrometry
Solve
problems: 26-1, 27-25, 27-26, MS supplementary assignment
Ch.9: Atomic Absorption and Fluorescence Spectrometry (if time permits)
LABORATORY EXERCISES:
Overall Strategy:
The strategy for these lab exercises is collaborative, investigative,
and integrative in nature and fall into three levels:
A.
elementary exercises to become familiar with the operation of the various
intruments and interpretaion of data;
B. identification of two unknown samples vis instrumental methods;
C. designing and performing an investigative research project that requires
the use of one or more instrument.
The following instruments are available to you:
1. Spec. 20 Visible
2. Spec. 21 UV-VIS
3. Buck Scientific, UV-VIS Spectrophotometer
4. Chemanal VIS/fluorescence/Naphelometry
5. Varian Cary 219 UV-VIS
6. GBC UV-VIS 911
7. HP UV-VIS spectrophotometer
8. Beckman Acculab 1 IR and a Nicolet
410 FTIR
9. Bruker FT-NMR 300 MHz, remote operation.
10. Gowmac GC
11. HP GC/MS
12. Perkin-Elmer - 107 AA Spectrophotometer
Experiments:
I. Absorption Spectra
1. Visible Spectroscopy
a. Familiarize yourself with the operation of the UV-VIS instrument.
b. Generate a visible spectrum for a known solution and establish
its maximum wavelength.
c. Generate a calibration curve (Beer's Law) for above known solution then
estimate the
concentration on an unknown sample from the curve.
d. Generate a set of UV spectra for a series of common solvents
(water, methanol, hexane, etc)
e. Run UV spectra of pure acetone then show the solvent effect by running
a solution of acetone in both
polar and non-polar solvent.
f. Generate a set of UV spectra for a number of known chromophores
(Acetone, Toluene, etc).
g. Generate UV spectra for your unknowns.
2. Infrared (IR) Spectroscopy
a. Familiarize yourself with the operation of the FT-IR instrument.
b. Determine the path length of a given IR cell.
c. Generate IR spectra for a set of known solid, liquid, and gas sample.
d. Generate IR spectra for your unknowns.
3. Atomic Absorption (AA) Spectroscopy (Do last if time permits).
Calibrate instrument and bring a water sample from your home and analyze
it for water hardness.
II. Nuclear Magnetic Resonance(NMR) Spectroscopy
Use the MockNMR computer program to familiarize yourself with the operation
of the NMR instrument.
(A qualitative study), then generate spectra for your unknowns using the
FT-NMR.
III. GC/MS Spectrometry
Generate MS spectra for your unknowns
VI. Investigative Research Project/Presentations
Set up a conference meeting with
me ASAP.
V. EXPECTATIONS OF STUDENTS:
1. Attendance is required. A good attendance including the transcription
of a good set of notes will greatly improve the student's chances for achieving
a satisfactory grade in this course.
2. Homework problems will be assigned and graded. Compile homework
in the portfolio.
3. A complete portfolio of all experiments, lab exercises, data, and
lab reports.
4. Investigative research project/oresentation.
5. A comprehensive final examination (ACS standardized exam).
6. Academic integrity must be always preserved. Any violation will
be handled according to the guidelines of the College Catalog.
7. Breakdown for grading :
Homework/Quizzes
30%
Experiments
30%
Investigative Research Project 20%
Final Exam 20%
Total
100%
Scale:
91- 100% = A
81- 90% = B
71-80% = C
61-70% = D
LAB REPORT: You may design your portfolio in any way you wish, as long as it contains the following information:
a) your name, title of each exercise, date, and a statement of objective;
b) all generated data, spectra, and graphs;
c) a discussion of the data generated from lab exercises;
d) a discussion of and conclusion to your unknowns' identity in a neat
and orderly fashion; and
e) a brief discussion and conclusion of the Investigative research project.
IMPORTANT NOTE:
Students with disabilities who require reasonable accommodations to
fully participate in course activities or meet course requirements are
encouraged to register with the Office of Disability Services to discuss
access issues. Please contact Dr. MeShelda A. Jackson by email mjackson@stfrancis.edu
or phone 815-740-3461.