CHEMISTRY 440 INSTRUMENTAL METHODS OF ANALYSIS
Southern Connecticut State University
Dr. Robert J. Snyder Jennings 343 ( 203 ) 392-6263
E-mail: Snyder_r@scsu.ctstateu.edu Spring Semester 1998
Texts: Principles of Instrumental Analysis, Fifth Edition, D.A.Skoog, F.J.Holler, T.A.Nieman, Saunders College Publishing ( 1998 )
Laboratory Manual Chemistry Experiments for Instrumental Methods, D.T.
Sawyer, W.R.Heineman, J.M. Beebe,Wiley ( 1984 )
Introduction: It’s the Instrument, stupid! On December 10, 1996, Robert F. Curl Jr., Sir Harold W. Kroto, and Richard E. Smalley were awarded the 1996 Nobel Prize in Chemistry for their discovery of C60--fancifully named buckminsterfullerene. In his Nobel lecture, Smalley flatly stated: " The INSTRUMENT discovered the fullerenes." He was referring to the laser vaporization, supersonic jet technique that Smalley had invented. Since the time of Galileo and his telescope, new devices, new instrumentation in the hands of the prepared observer, have generated new insights into nature that simply would not have been possible in the absence of the technology.
Course Overview: The course is an introduction to the theoretical background and practical use of modern instruments in the analytical laboratory. After a brief introduction to the use of instrumentation for chemical analysis, the properties of electromagnetic radiation will be discussed. Spectroscopic techniques that will be covered include: Ultraviolet/Visible spectroscopy, Fluorescence and Phosporescence, Atomic Absorption ( Flame and Graphite Furnace ) Spectroscopy, Infrared Spectroscopy and Nuclear Magnetic Resonance Spectroscopy. After an introduction to Chromatographic separations, Gas Chromatography and High-Performance Liquid Chromatography will be discussed. Laboratory experiments will demonstrate the scientific method and illustrate basic concepts presented in the lecture portion of the course.
Final Course Evaluation:
Mid-Term Examination 30 %
Final Examination 30 %
Laboratory Reports 40 % page two
COURSE OUTLINE
I Introduction
Chapter 1: Introduction
Chapter 5: Signals and Noise
II Spectroscopic Techniques
Chapter 6: An Introduction to Spectrometric Methods
Chapter 7: Components of Optical Instruments
Chapter 13: An Introduction to Ultraviolet/Visible Molecular Absorption
Chapter 14: Applications of Ultraviolet/Visible Molecular Absorption
Spectrometry
Chapter 15: Molecular Luminescence Spectrometry
MID-TERM EXAMINATION MARCH 19
Chapter 8: An Introduction to Optical Atomic Spectrometry
Chapter 9: Atomic Absorption and Atomic Fluorescence Spectrometry
Chapter 16: An Introduction to Infrared Spectrometry
Chapter 17: Applications of Infrared Spectrometry
Chapter 19: Nuclear Magnetic Resonance Spectroscopy
III Chromatographic Techniques
Chapter 26: An Introduction to Chromatographic Separations
Chapter 27: Gas Chromatography
Chapter 28: High-Performance Liquid Chromatography
FINAL EXAMINATION MAY 21
The examination questions will be taken directly from the material covered in class. The mid-term examination and the final examination will be two hours long.
page three
LABORATORY EXPERIMENTS
EXPERIMENT 6-1 Spectrophotometry in the Visible Region: Absorption Spectra,
Beer’s Law, and the Simultaneous Analysis of a Two-Component
Mixture page 168
EXPERIMENT 8-2 Infrared Spectra of Aldehydes and Ketones page 236
EXPERIMENT 9-1 Atomic Absorption Determinations page 244
( Graphite Furnace)
EXPERIMENT 9-3 Determination of Calcium, Iron and Copper in Food
by Atomic Absorption ( Flame ) page 258
EXPERIMENT 10-3 Determination of Pharmaceuticals ( Acetylsalicylic and
Salicylic Acids) by Fluorimetry page 279
EXPERIMENT 11-5 Analysis of APC Tablets by Proton NMR page 302
EXPERIMENT 12-3 Resolution and Qualitative Identification of Hydrocarbons
by Gas Chromatography page 336
EXPERIMENT 13-1 Determination of Pharmaceuticals by High Performance Liquid
Chromatography: Determination of Caffeine in Beverages
page 347 page four
The Laboratory Notebook
As observations are made during a chemical process, or as numerical data are recorded and processed, a complete up-to-date record must be made of the observations and data. For these purposes, a laboratory notebook will be kept throughout the semester. The notebook must be permanently bound to prevent the addition or removal of pages. All pages must be numbered consecutively from first page to last page. Your name must be written on the cover of the laboratory notebook. The first few pages of the notebook are to be used as a Table of Contents. As you begin an experiment, make an entry in this table that will permit you to locate information easily e.g. Experiment Title, page number.
Only the right-hand pages of the notebook are to be used for information. Start each experiment on a new, right-hand page. the experiment should include the Title of the experiment, Date, Partner’s Name, all Data and Observations that arise during the experiment ( including proper units and the appropriate number of significant figures) and all calculations that are required.
The left-hand pages of the notebook are used primarily for quick arithmetic calculations and for taking notes during the instructor’s pre-lab instruction, or for recording any special instructions about the experiment.
Mistakes do happen, especially while recording data in a lab notebook. No one expects your experiment to be perfect. If you make a mistake, draw a single line through it and write in the correct value. Never erase data or cover it with correction fluid. Also, never tear pages out of a lab notebook. The lab notebook is a permanent record of what you did in the laboratory, warts and all.
Make sure that the laboratory notebook is kept up-to-date.
The Laboratory Report
The laboratory report is a formal report of what you did in the laboratory. Therefore it should be written in the past tense using the passive voice. It should include only those parts of the experiment actually performed, including any in-lab modifications. The laboratory report should include all of the following parts clearly labeled:
Title of Experiment
Name of Experiment and Laboratory Partner
Date Submitted
The Introduction
Experimental Procedure
The Data and the Results
The Discussion of the results
The Conclusion
References page five
THE INTRODUCTION ( 20 points )
This section should be a description of the purpose of the experiment and the method used. The introduction contains information required for a complete understanding of the experiment, i.e., historical and theoretical material that is relevant to the experiment. The student is expected to consult the course textbooks, use the library and any other sources of information. The use of any basic equations should be justified here. Normal length: 100 to 300 words.
THE EXPERIMENTAL PROCEDURE ( 20 points )
This section should report the main details of the experimental procedure, including the number of runs made and the conditions under which they were carried out (concentration, temperature, etc.) A detailed description of the instrumental method should be given, including a schematic diagram of the instrument used.
THE DATA AND THE RESULTS ( 20 points )
The results should be presented in both tabular and graphic form. Both the basic information ( raw data ) and the calculated results should be included in as concise a form as possible. Include a sample calculation ( where several sets of data have been obtained, only show a sample calculation for one set). All tables should be titled and all graphs plotted on good quality graph paper. The graphs should be titled with both coordinates labeled. The coordinates should be chosen so that the plotted curve uses most of the graph paper. The curve should be smooth and, therefore, will probably not go through all of the points. Curves should be drawn with a ruler or a French curve. Use the method of Least Squares to determine the slope and intercept of all linear plots. Accompanying the tables and graphs should be text that explains their significance and presents any conclusions which can logically be drawn. Any calculation not explained in the introduction should be explained here.
THE DISCUSSION OF THE RESULTS ( 20 points )
This is one of the most important sections of the laboratory report. Here the student provides an interpretation of the information just presented in the Results section. Students should draw from the theoretical material presented in the Introduction and relate this to the results obtained. This section should offer possible explanations for the results obtained. Include a discussion of the possible sources of error and their probable magnitude. The number of significant figures in calculated quantities should be consistent with the estimated error of your measurements. Whenever possible, compare your results with theoretical or experimental values from the literature.
THE CONCLUSION ( 20 points )
The conclusion section should summarize the final results, state the final answer, address the original purpose of the experiment, and briefly indicate whether or not the purpose of the experiment was achieved.
REFERENCES
Any book or article referred to should be indicated at the proper point in the text ( a number in parenthesis ) and included in a bibliography at the end of the report, using proper presentation of literature citations.