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Text: Rubinson, K.A., Rubinson, J.F. Contemporary Instrumental Analysis. Prentice Hall: Upper Saddle River, NJ, 2000.

Outcomes:

This course will introduce the student to the theories and principles of instrumental methods of chemical analysis. Upon successful completion of this course, a student should be able to:

• distinguish between analog and digital signals.
• understand and apply the concepts of signal, noise, sensitivity, detection limit, resolution, dynamic range, and selectivity to an instrumental analysis.
• calibrate an instrumental method.
• be knowledgeable about electromagnetic sources and detection systems used in instrumental methods of chemical analysis.
• choose a suitable instrumental method of analysis for a given analyte and matrix.
• understand the underlying principles of basic instrumental methods such as atomic absorbance and emission; IR, UV, visible, and fluorescence spectroscopy; mass spectrometry; nuclear magnetic resonance; gas and liquid chromatography.

Attendance:

Attendance is mandatory. Excessive absences can be cause for loss of a grade or failure. Three consecutive unexplained absences must be reported to the registrar.

Assignments:

There will be weekly homework assignments which will be graded for a large portion of your final grade. These assignments should be completed as carefully as possible, since this material will be on the cumulative final exam. Weekly homework assignments will be collected on Mondays. Late assignments will not be accepted, and will result in a grade of zero. The homework is a large part of the grade, so special attention should be paid to them. There will be no tests, except for the cumulative final at the end of the semester. The final will focus heavily on the homework assignments.

Laboratory:

Each student is responsible for reading the sections of the text pertaining to the laboratory experiments. This is imperative before a laboratory is run, because the instructor will need to check you out on the equipment before you are allowed to proceed with your experiment.

The majority of class time will be spent in the laboratory. There are seven categories of lab experiments for which your team will be responsible. Your team may complete them in any order, with some variation within each category. You may work at your own pace, spending as much time as is necessary to complete experiments in all categories.

A summary report from your group is due on Wednesday of each week, outlining the laboratory progress made and plans for the next week. This report should include the roles of each team member, a summary of the week's activities, a summary of results, a plan for the lab work to be performed during the next week, and a list of chemicals or equipment needed for the next week's experiments.

Laboratory reports are due one week after the completion of the experiment. Five (5) points will be deducted for each day past the deadline, up to five days. Any lab report more than 5 days late will not be accepted and a grade of zero will be assigned.

Laboratory Experiments:

The following are possible labs you could perform in each of the seven categories. You are free to develop your own experiment for any of the categories with consultation and approval of the instructor.

UV/Visible Spectroscopy

• The spectrophotometric Determination of the pKa of Bromothymol Blue
• The simultaneous Determination of Caffeine and Acetylsalicylic Acid in an Analgesic by Ultraviolet Spectroscopy

IR Spectroscopy

• Analysis of Lead by Complexation with EDTA and Quantitation using IR Spectroscopy
• Analysis of Trans-Fatty Acid Content of Margarines
• Infrared Analysis of Keto-Enol Tautomerism
• A study of Hydrogen Bonding using Infrared Spectroscopy Measurements
• Determination of Octane Number in Gasoline by Near IR Spectroscopy

Fluorescence Spectroscopy

• Fluorometric Determination of Acetylsalicylic Acid in an Aspirin Tablet
• Fluorometric Determination of Quinine in Urine
• Determination of Nitrate in Natural Water and Soil by Fluorescent Quenching of dichlorofluorescein
• Flourometric Determination of Histamine in Tuna
• Fluorometric Determination of Aluminum in Water
• The Determination of Riboflavin in Urine

Atomic Absorption

• Determination of Iron in Dog Food by AA Spectrophotometry
• Determination of Lead in Water, Soil, Paint Chips, or Earthenware
• Determination of Iron in Wine

Gas Chromatography

• The Relationship Between the Flow Rate and Column Efficiency/ Determination of Detection Limits
• GC Determination of Low-Molecular-Weight Alcohols
• GC Analysis of Alcohol in Wine

HPLC

• Determination of Anthracene, Benzene, and Naphthalene in a Mixture
• Determination of Caffeine and Acetylsalicylic Acid in an Analgesic
• Is Decaf really Decaf?
• Quantitation of Indole in Seafood using HPLC/ Fluorescence
• Determination of Polyaromatic Hydrocarbons in Whiskey
• Determination of Polyaromatic Hydrocarbons in Cigarette Smoke
• Determination of Vitamin A in Infant Formula
• Chlorophyl a, Chlorophyl b and -Carotene in Collard Greens
• Coumarin in Vanilla Extracts
• Riboflavin in Milk and Cheese
• UV absorbers in sunscreens
• Pungency Quantitation of Hot Pepper Sauces

NMR

• Determination of an Unknown Organic by NMR analysis
• NMR analysis of Tetraphenylporphyrins
• Employing NMR Spectroscopy to Evaluate the Transmission of Electronic Effects in 4-Substituted Chalcones

Electrochemistry

• Electropolymerized Conducting Polymers as Glucose Sensors

Grading:

• Homework 35%
• Final Exam 15%
• Lab reports 35%
• Weekly summaries 5%
• Preparation/Participation/ Performance 10%

A 90-100%                 C+ 75-77%

A- 88-89%                  C 70-74%

B+ 85-87%                 C- 68-69%

B 80-84%                   D+ 65-67%

B- 78-79%                  D 60-64%

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