INSTRUMENTAL ANALYSIS
Lecture: 03-325-1 - 3 credit
hours
Lab: 03-326-1 - 2 credit hours
I. INSTRUMENTAL ANALYSIS
SPRING: 2005
PREREQUISITE:
LECTURE HOURS: M 6:30-9:00 PM
LAB HOURS: F 1:00-5:00 PM
II.
INSTRUCTOR: Dr. Salim M.
Diab
OFFICE: Room 215,
PHONE: 740-3855 (Ext. 855)
OFFICE HOURS: MWF 9:00 - 10:00 AM
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 Chemical literature (library journals, internet, etc) to explore practical ways of using instruments to solve chemical problems qualitatively and quantitatively. The students will survey the theory and application of a number of instruments such as: Visible, Ultra Violet, Infrared, 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
world.
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 the Internet 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 and lab manual to accompany above text,
3. 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,
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. Contemporary Instrumental Analysis, Robinson and Robinson.
22. Spectroscopy Source Book, Science Reference Series, Sybil Parker, editor.
23. Organic Spectroscopy, William Kemp
24. Organic Spectroscopy, Jag Mohan.
25. Handbook of Analytical Techniques, Vol. I and II, helmut Gunzler and Alex Williams, eitors.
26. Internet Web Sites (see attachment).
Web Sources:
Tutorials and Exercises
General:
1. http://www.spectroscopynow.com/Spy/basehtml/SpyH
2. http://www.uvm.edu/~jgoldber/courses/chem221/links.html
3. http://www.chemguide.co.uk/analysismenu.html
UV-VIS:
1. http://www.chemistry.ccsu.edu/glagovich/teaching/472/uvvis/uvvis.html
IR and NMR:
1. http://www.cem.msu.edu/~parrill/AIRS/
2. http://wwwchem.csustan.edu/Tutorials/INFRARED.HTM
3. http://orgchem.colorado.edu/hndbksupport/spect.html
4. http://chipo.chem.uic.edu/web1/ocol/spec/IR.htm
NMR:
1. http://www.wfu.edu/~ylwong/chem/nmr/h1/(H-NMR)
2.
http://www.wfu.edu/%7Eylwong/nmr/c13/
(carbon NMR)
3. http://www.ch.ic.ac.uk/local/nmr/ (H-NMR, IR, MS Tutor)
4. http://www.cis.rit.edu/htbooks/nmr/nmr-main.htm (FT-NMR)
5. http://science.widener.edu/svb/nmr/nmr.html
(NMR General)
6. FT-NMR.html.ppt
7. http://chipo.chem.uic.edu/web1/ocol/spec/NMR.htm
MS:
1. http://staging.mc.vanderbilt.edu/msrc/tutorials/ms/ms.htm
2. http://chipo.chem.uic.edu/web1/ocol/spec/MS.htm
2. http://ull.chemistry.uakron.edu/gcms/
Chromatography:
1. http://ull.chemistry.uakron.edu/chemsep/index.html
(Great Tutorial on Separation techniques)
2.
High-performance liquid hromatography(HPLC)
3.
http://kerouac.pharm.uky.edu/ASRG/HPLC/hplcmytry.html(HPLC)
Exercises:
http://www.chem.wisc.edu/~concept/spectro.html(quiz in NMR)
http://www.chem.vt.edu/chem-ed
http://www.chem.uic.edu/web1/OCOL-II/WIN/SPEC.HTM(organic
IR,NMR,MS)
http://www.chem.ucla.edu/~webspectra/(NMR)
http://www.nd.edu/~smithgrp/structure/workbook.html(organic
Structure Elucidation)
http://webbook.nist.gov/chemistry/name-ser.htm(NIST
database search)
http://www.shu.ac.uk/schools/sci/chem/tutorials/(Spectroscopy
tutorial/exercises)
http://www.chem.uni-potsdam.de/tools/index.html
(Spectral Tools)
http://rainier.chem.plu.edu/fid_archive.html
(FT-NMR Free Induction Decay Archive)
http://www.aist.go.jp/RIODB/SDBS/menu-e.html
(Integrated Spectral Data - Excellent Search site)
LECTURE TOPICS TO BE COVERED:
Introduction to
Spectroscopy and Instrumental Analysis
Supplementary Lecture and
Ch1.
Solve problems: 5-2, 5-8, 5-12
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
Solve problems: 13-1(d-f), 13-2(d-f), 13-4, 13-6, 13-8, 13-13(e-h), 13-19
14-6
(b)
Ch. 15,16,17: Molecular
Fluorescence/IR Spectroscopy
Solve problems: 15-1, 15-5, 15-6 (a & d),
16- 2, 16-8, 16-11, and solve IR supplementary problems
Ch.19:
NMR Spectroscopy
Solve
problem: 19-1, 19-10, 19-24, 19-28, 19-30
Ch.20: MS Spectrometry
Solve supplementary problems
Ch. 26,27,28: Chromatography
Solve problems: 26-1, 27-25,
27-26,
LABORATORY EXERCISES,EXPERIMENTS,
AND RESEARCH
PART
I
Absorption Spectra
Exercises
UV-Visible
Spectroscopy
a. Familiarize yourself with the operation of the UV-VIS
instrument.
b. Establishing maximum wavelength:
Generate a visible spectrum for a known solution and establish its
maximum wavelength.
c. Solvent Effect: Generate a set of
UV spectra for a series of common solvents (water, methanol, hexane, etc)
e. Hypsochromic and bathochromic
Shifts: Generate a UV spectra of pure acetone then show the solvent effect
by running a solution of acetone in both polar (water) and non-polar (Toluene)
solvents.
f. Chromophores: Generate a set of UV spectra for a
number of known chromophores that contain aromatics
and carbonyls (Acetone, Toluene, etc).
g. Conjugation and UV spectra: Generate
a set of UV spectra for a series of
conjugated and isolated pi bonded organic compounds (cyclohexene, toluene, naphthalene, anthracene, etc).
h. Do Exp. 358: A Beer's law Study.
i. Unknowns: Generate UV spectra for your
unknowns for Part II.
Infrared Spectroscopy
a. Familiarize yourself with the operation of the
FT-IR instrument.
b. Path
Length: Determine the path length of a given IR cell using interference
lines method.
c. Sampling:
Generate IR spectra for a set of knowns: solid,
liquid, and gas samples.
d. Do Exp.26: Quantitative IR Analysis of Isopropyl alcohol in Toluene.
e. Generate IR spectra for your unknowns for Part III.
PART
II
IDENTIFICATION
OF
UNKNOWNS
Part II of this lab is an investigative one in which you generate spectral data for two unknowns using the following instruments: UV-VIS, FT-IR, NMR. And GC-MS. Make sure that you analyze characteristic peaks and assign chemical property to each one. Finally, a brief narrative of how you arrived to the identity of your unknowns is required, giving a final conclusion of the identity of your unknowns, using supporting evidence from your spectral data – see lab manual for more details.
PART
III
Research Projects
Applications and
Investigations
Stage I: Select a project and do the literature study on it.
Stage II: A project outline detailing the experiment including the theory, and all necessary materials (both equipment and chemicals).
Stage III: Involves the bench work and
data collection for the project.
The final stage is the completion of a written report.
Introduction: Here you must accomplish two things. You must explain the specific goal of your experiment, and what principles of quantitative analysis will allow you to accomplish this goal. It should read like one of the introductions to the experiments we did in this course. The introduction should include any pertinent chemical reactions (remember to reference any sources used including lab manual and your text).
Apparatus: You need to list any equipment that you will need beyond that in your locker. This must be done in order to prepare lab services.
Chemicals: You must list not only the chemicals necessary, but the quantities as well. This is particularly important; otherwise you may run out before the completion of your experiment.
Safety: If any equipment/chemicals/ procedure requires any special safety considerations, you need to describe them here. Also, state how you will dispose of your chemicals when you are finished - I suggest that you keep at hand all MSDS information for every chemical that you need.
Procedure: The procedure should be explained, either in paragraph or list format, in enough detail so that you may complete the experiment without any additional information.
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
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 (GSU)
10. Gowmac
GC
11. HP GC/MS
12. Perkin-Elmer - 107 AA Spectrophotometer
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. Frequent quizzes will be also given and graded.
3. A
complete lab report of all experiments: lab exercises, unknowns analysis,
identification and report, and investigative research project/presentation.
5. A comprehensive final examination (A takehome
exam and 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 of Lecture Grades
:
Homework
30%
Quizzes
20%
Mid-Term Exam
20%
Final Exam 30%
Total 100%
8. Breakdown of lab Grades: Criteria used to
arrive at the final grade will depend on the following:
a. completion of
Part 1 - lab exercises/report;
b. organization, calculations, and quality of
writing;
c. documentation of all relevant data, spectra, graphs, etc;
d.
completion of part II - correct identification of unknowns/report;
e.
completion of Part III - investigative project/report and presentation.