I. Identification

A. School - Arts and Sciences

B.  Department - Chemistry

C. Course Number - CHE 540

D. Course Title - ADVANCED ANALYTICAL CHEMISTRY

E. Catalog Description - An advanced course in the use of modern instrumentation, both spectroscopic and chromatographic techniques, for the solution of chemical problems.
    The emphasis will be on the applications of each instrumental method. 3 credits.

F. Prerequisites - CHE 371 and CHE 440 or Departmental Permission

G. Special Conditions - none

H. Plan of Rotation - Offered every even-numbered Fall semester

I. Text ó F. A. Settle, Handbook of Instrumental Techniques for Analytical Chemistry, Prentice-Hall, New Jersey, 1997

J. Instructor ó Dr Robert J Snyder

The discipline of Chemistry is typically sub-divided into Analytical, Organic, Inorganic and Physical Chemistry. Offering a required course in Advanced Analytical Chemistry will ensure that our students are receiving the latest information in all of the four basic areas of chemistry. Basically you canít do modern Chemistry without a knowledge of Analytical chemistry. Recent faculty acquisitions in the Chemistry Department have provided a faculty base for offering this course.

A.    Course Objectives - Analytical Chemistry is the science of chemical measurements. Most modern chemical measurements are performed with the use of instrumentation. After a brief review of the theoretical background of each instrumental method discussed, as well as a discussion of the general principles of that techniqueís instrument design, the students will be shown the utility and actual application of each analytical technique. In addition, this advanced course will address instrumental techniques not ordinarily covered in a typical undergraduate course in instrumental analysis.

B.    Course Outcomes The students should emerge from this course with an idea of what the various instrumental methods are capable of doing in order to solve a problem or make a measurement. On written examinations the student will be able to answer two kinds of questions: 1) given the output from an instrument, e.g. a spectrum, the student will be able to perform post-data-acquisition calculations including statistical methods for evaluating and interpreting data; and 2) the student will be asked to explain the theoretical basis for the data acquired by the various instrumental techniques. Thus the student will be able to explain the distinction between qualitative and quantitative goals of determination. Also, in written form on examinations or verbally in class discussions, the student will be asked to suggest the correct sampling method for the various states that a typical sample could exist as, i.e. solid, liquid, gas, solution,etc. The student will also be asked to identify sources of error and learn to identify interferences in instrumental analysis. Since most modern analytical instruments are interfaced with computers, the student will be exposed to computer-based acquisition systems for analytical instruments. The course will provide an overview of the true modern analytical chemist - selecting the right tool for the job at hand.

C.    Course Outline:

    I. Introduction to the use of Instrumentation for Chemical Analysis ( 10% )

    II. Spectroscopic Techniques ( 30% )

        1. Ultraviolet/Visible Absorption Spectroscopy

        2. Fluorescence, Phosphorescence and Chemiluminescence

        3. Atomic Absorption Spectroscopy using Flame and Electrothermal Atomization

        4. Infrared and Raman Spectroscopy

        5. Nuclear Magnetic Resonance Spectroscopy

        6. Mass Spectrometry

    III. Chromatographic Techniques ( 20% )

        1. Gas Chromatography

        2. High-Performance Liquid Chromatography

    IV. Thermal and Calorimetric Methods of Analysis ( 20% )

        1. Thermogravimetry

        2. Differential Thermal Analysis

        3. Differential Scanning Calorimetry

    V. Combined Analytical Techniques ( 20% )

        1. GC-MS

        2. GC-IR

        3. TG-IR

D. Modes of Instruction - Since the Chemistry Department has many of the modern analytical instruments that we will be discussing, there will be a liberal sampling of actual hands-on experience as well as classroom instruction. Also, because the class will consist of graduate students in Chemistry who actually work full-time in chemical industry and use many of the instruments that we will be studying, there will be ample opportunity for classroom discussion.

E. Evaluation - The final course evaluation will be determined by three methods: a mid-term examination worth 30%, a final examination worth 30% and a course project worth 40%. The mid-term and final examinations will each be two hours long and will contain questions taken directly from the material covered in class, including material from class discussions and questions concerning the hands-on training. The course project will be a ten (10) page written review of an original research article from the past yearís literature of a new technique, improvements in instrumentation or methods, or an application of a technique to a specific analysis. The article should be from a refereed journal such as Analytical Chemistry, Applied Spectroscopy, Journal of the American Chemical Society, etc. This review will include, in addition to a synopsis of the paper, a review of the current status of the area of research, the studentís critical evaluation of the paper, and an evaluation of the significance of the research.

F.Selected Bibliography:

Personal Library ( A )    ( these books may be borrowed at anytime by the students for one week )

1.    J. A. Dean, Analytical Chemistry Handbook, McGraw-Hill, New York,1995
2.    D. A. Skoog, D. M. West, F. J. Holler, Fundamentals of Analytical Chemistry, 7^th Edition, Saunders College Publishing, Philadelphia, 1996
3.    F. W. Fifield, D. Kealey, Principles and Practices of Analytical Chemistry, Fourth Edition, Blackie Academic and Professional, London, 1995
4.    D. A. Skoog, E. J. Holler, T. A. Nieman, Principles of Instrumental Analysis, Fifth Edition, Saunders College Publishing, Philadelphia, 1998
5.    H. H. Willard, L. L. Merritt, J. A. Dean, F. A. Settle, Instrumental Methods of Analysis, Seventh Edition, Wadsworth Publishing Company, California,1988
6.    G. D. Christian, J. E. OíReilly, Instrumental Analysis, Second Edition, Allyn & Bacon, Massachusetts, 1986
7.    J. D. Ingle, S. R. Crouch, Spectrochemical Analysis, Prentice-Hall, New Jersey, 1988
8.    R. M. Silverstein, G. C. Bassler, T. C. Morrill, Spectrometric Identification of Organic Compounds, Fifth Edition, J. Wiley & Sons, New York, 1991
 

Buley Library ( B )

1.    L. Voress, Instrumentation in Analytical Chemistry, 1988-1991, American Chemical Society, Washington, D. C. , 1992
2.    P. Delahay, New Instrumental methods in Electrochemistry; Theory,Instrumentation, and applications to Analytical and Physical Chemistry, Interscience Publishers, New York, 1954
3.    J. Kenkel, Analytical Chemistry for Technicians, Lewis Publishers, Florida, 1994
4.    P. Meier, Statistical Methods in Analytical Chemistry, J. Wiley & Sons, New York, 1993
 

CSU System ( C )

1.    G. W. Ewing, Analytical Instrumentation Handbook, M. Decker, New York, 1990
2.    F. Settle, Handbook of Instrumental Techniques for Analytical Chemistry, Prentice-Hall, New Jersey, 1997
3.    S. A. Borman, Instrumentation in Analytical Chemistry, 1982-1986, American Chemical Society, Washington, D. C., 1986
4.    A. J. Senzel, Instrumentation in Analytical Chemistry, 1973-1982, American Chemical Society, Washington, D. C., 1982
5.    G. D. Christian, Analytical Chemistry, 5^th Edition, J. Wiley & Sons, 1994
6.    J. A. Dean, Analytical Chemistry Handbook, McGraw-Hill, New York, 1995
7.    J. Kenkel, Analytical Chemistry: Refresher Manual, Lewis Publishers, Florida, 1992
8.    H. L. C. Meuzelaar, T. L. Isenhour, Computer-Enhanced AnalyticalSpectroscopy, Plenum Press, New York, 1992
9.    G. Schwedt, The Essential Guide to Analytical Chemistry, J. Wiley & Sons, New York, 1997
10.    D. A. Skoog, D. M. West, F. J. Holler, Fundamentals of AnalyticalChemistry, 6^th Edition, Saunders College Publishing, Texas, 1992
11.    F. Settle, Handbook of Instrumental Techniques for Analytical Chemistry, Prentice-Hall, New Jersey, 1997
12.    J. Zyka, Instrumentation in Analytical Chemistry, Horwood, New York, 1991
13.    Milestones in Analytical Chemistry, edited by the Washington Staff of Analytical Chemistry, American Chemical Society, Washington, D. C., 1994
 

Samples of recent articles
NOTE: The American Chemical Society (ACS ) has a web page at http://pubs.acs.org where all of the journals of the ACS can be found on-line.
 

1.    K. Ohta, Y. Naitoh, K. Tominaga, N. Hirota, K. Yoshihara, Femtosecond Transient Absorption Studies of Trans- and Cis- 1,3,5,- Hexatriene in Solution, Journal of Physical Chemistry, A, 102,35 (1998)

2.    R. Schweitzer-Stenner, G. Sieler, N. G. Mirkin, S. Krimm, Intermolecular Coupling in Liquid and Crystalline States of trans-N-Methylacetamide Investigated by Polarized Raman and FT-IR Spectroscopies,
       Journal of Physical Chemistry, A, 102, 118 (1998)

3.    T. J. Wenzel, R. Eversten, B. E. Perrins,T. B. Light, A. C. Bean, Solid-Phase Lanthanide Luminescence Detection in Liquid Chromatography, Analytical Chemistry, 70, 2085 (1998)

4.    A. J. Hillis, D. H. Lenschow, J. W. Birks, Dimethyl Sulfide Measurement by Fluorine-Induced Chemiluminescence, Analytical Chemistry, 70, 1735 ( 1998 )

5.    K. Heinig, C. Vogt, G. Werner, Separation of Nonionic Surfactants by Capillary Electrophoresis and High-Performance Liquid Chromatography, Analytical Chemistry, 70, 1885 (1998)

6.    Y. V. Gankin, A. Gorshteyn, S. Smarason, A. Robbat, Time-Condensed Analysis by Mass Spectrometry, Analytical Chemistry, 70, 1655 (1998)

7.    S. J. Oh, J. Koenig, Phase and Curing Behavior of Polybutadiene/Dially Phthalate Blends Monitored by FT-IR Imaging using Focal-Plane Array Detection, Analytical Chemistry, 70, 1768 (1998)