CHEM 435
INSTRUMENTAL ANALYSIS
LABORATORY
Spring 2004
SYLLABUS
Dr. M. Shabangi Dr. K. Johnson
Office: SL 2341 Office: SL 3116
E-mail: mshaban@siue.edu E-mail: kevjohn@siue.edu
Phone: 650-2420 Phone: 650.5934
Office Hours: Open or by appointment.
Textbook: Handouts
LABORATORY NOTEBOOKS:
Each student is required to keep and maintain a well-organized lab notebook. The lab notebook is to be the record of all experimental data and observations. This should include a record of the pre-experimental calculations, solution preparations, instrumental parameters, measurements performed, experimental observations, summary of the data calculations, and conclusion. The lab notebook should be maintain in such a manner that anyone familiar with scientific methodology can read and understand (i) how the experiment was performed, (ii) what equipment and materials were used, (iii) what results were obtained, and (iv) what was learned from the experiment. Completeness is more important than neatness, however, everything should be legible. The first page should be a running Table of Contents for the entire notebook. Each page should be numbered. With this in mind, each student is required to buy a CHEMCLUB notebook (only 10 $), no loose-leaf notebooks will be permitted. All notebook work must be written in ink.
PRIOR TO THE ASSIGNED EXPERIMENT:
Each student should perform the following pre-experimental preparation prior to the first laboratory meeting for an experiment. The TA will review laboratory notebooks, early in lab session. The experiment may not be started until the notebook work is completed.
1. Read the assigned laboratory experiment and background material in the texts.
2. Record in your notebook the experiment title and primary references for the experiment.
3. State in your own words (one or two sentences) the purpose of the experiment.
4. List the important reagents and chemicals to be used.
5. Record all calculations for the preparation of solutions, reagents or standards.
6. Record an outline of the experimental procedure to be performed. This will serve as a summary of what has to be done during the laboratory class. A checklist style is recommended.
LABORATORY REPORTS:
Laboratory reports must be TYPED and neatly organized. There is no page number requirement for the reports, however, all essential elements of the report must be present. In general, these elements should include the following items (unless otherwise noted):
The cover page should include the title of the experiment, your name, the date the experiment was performed, the date the experiment is due, the name of your lab partners, and your abstract.
This should be a paragraph, which summarizes the purpose of the experiment, the specifics of the system you studied, and the final result(s) including comparison to the literature (if applicable) and statistics.
This section will describe the purpose of the experiment (a WELL DEFINED PROBLEM), and HOW THE INSTRUMENT WORKS (in your own words, don’t copy from books).
The following should be included:
1. Any procedural changes that have been made or any important information given during the laboratory that was not included in the original handout.
2. Important experimental parameters, equipment and reagent used.
3. Information about the instrument make and model, and instrumental parameters.
4. Any necessary safety precautions and chemical disposal procedures.
The following should be included (in a logical order):
1. The actual weights or volumes used.
2. The actual concentrations for any solution.
3. Tabulation of all measurements, including raw data and calculated values. Careful thought and planning will help make this information accessible to the reader.
4. Statement of any important observations.
5. A complete sample calculation for each type of calculation, including uncertainty analysis when required.
6. Preparation of graphs.
7. Presentation of correlations, concentration determinations, or unknown identification.
8. Figures (actual data) should be organized, labeled and pasted in a report.
This section should discuss the results obtained, the conclusion drawn from the data, and any errors that may have affected your results. You must decide whether the intended correlations are correct, whether your spectra make sense, and what the results tell you. When possible you should compare your data with the literature or available data. Any relevant statistical analysis should be included in your discussion. This is an important section because it is your analysis of the data and your effort to make sense out of your results. The reader must be able to judge whether you have accomplished what was intended and also the quality of your results.
Any literature references used to write up the report must be given and cited in text. Use the ACS standard reference format.
Experiments will be conducted in groups. Each student in a group will have the same results. Therefore, it is reasonable for students to work on the calculations together. However, all pre-experimental preparation and post-calculation work (discussion and conclusion) should be completed independently and represent the work of your laboratory experience. Failure to comply with these guidelines is considered academic dishonesty and will be subjected to a grade of F in the course. If you are not sure about something, please ask.
(Any late report will be reduced by 5 points per day)
Pre-laboratory preparation (in notebook) 5 pts
Cover Page & Abstract 5 pts
Introduction 10 pts
Experimental 5 pts
Results/Discussion/Conclusions 10 pts
References (should have at least 3) 5 pts
Overall presentation (spelling, grammar, non sense…) 10 pts
_________________________________________________________
Total 50 pts
90 – 100 % A
80 – 89 % B
70 – 79 % C
60 – 69 % D
less than 60 % F
1.
UV: Optimization of
Experimental Condition by a Simplex procedure
2.
IR: Quantitative Analysis of a xylene Mixture using an Internal Standard
3.
AA (flame): Determination of Na+/K+ Levels in Urine. Johnson
4.
AA (graphite): Determination of Trace
Metals in Urine. Johnson
5.
HPLC: Optimization of Experimental Conditions: Separation & quantification
of components in diet soda. Johnson
6.
GC: Optimization of Experimental Conditions: Determination of Impurities in
Whiskey Using GC. Johnson
7.
GC-MS: Detection and Determination
of Fuel Components by GC and GC-MS. Johnson
8.
ISE: Determination of Fluoride
in drinking water.
9.
CV: Cyclic Voltammetry.
SPECIAL TOPICS
NMR:
Demonstration
CE: Capillary Electrophoresis
DTA:
Thermal Analysis
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Group 1A and 1B |
Group 2A and 2B |
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Week 1 (Jan 13) |
No lab |
No lab |
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Week 2 (Jan 20) |
Check in |
Check in |
|
Week 3 (Jan 27) |
UV |
IR |
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Week 4 (Feb 3) |
IR |
UV |
|
Week 5 (Feb 10) |
AA (flame/graphite) |
No lab |
|
Week 6 (Feb 17) |
Special topic |
No lab |
|
Week 7 (Feb 24) |
No lab |
AA (flame/graphite) |
|
Week 8 (Mar 2) |
No lab |
Special topic |
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Week 9 (Mar 9) |
Spring Break |
Spring Break |
|
Week 10 (Mar16) |
NMR demo |
NMR demo |
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Week 11 (Mar 23) |
GC |
HPLC |
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Week 12 (Mar 30) |
GC-MS |
GC-MS |
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Week 13 (Apr 6) |
HPLC |
GC |
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Week 14 (Apr 13) |
CV |
ISE |
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Week 15 (Apr 20) |
ISE |
CV |
|
Week 16 (Apr 27) |
GC-MS |
GC-MS |