Chemistry 502 - Instrumental Methods of Analysis – Spring 2003

Qualitative and quantitative methods of chemical analysis for organic, biochemical, and inorganic compounds fall into two categories, classical (or wet) methods and instrumental methods. Chemistry 313 surveyed many classical methods and some instrumental methods of analysis. Although there is not always a clear barrier between the two, the primary difference arises from the type of physical property used to provide information. Classical methods often rely on reactivity or physical properties such as solubility, melting and boiling points, odors, or refractive indices for qualitative information, while gravimetric, volumetric, and titrimetric measurements provide quantitative information. Classical methods for the separation of mixtures are mainly solvent extractions or distillations. Instrumental methods typically utilize other physical properties such as absorption or emission of light, mass-to-charge ratio, or electrode potential. Separations are carried out by more efficient chromatographic methods.

Instrumental methods certainly extend well beyond the chemistry lab. These instruments are found in biotechnology, environmental, geological, materials, forensic, medical, nutritional, and industrial labs. Unfortunately, some scientists view and utilize these instruments as "black boxes". This term implies a device in which the scientist places a sample and somehow a number is generated that influences the scientist’s decision-making process. It should be apparent that this approach could be dangerous, as the old saying "Garbage In/Garbage Out" is often true. As such any scientist using such sophisticated equipment needs at least a basic understanding of how these instruments work.

Instrumental Methods of Analysis is a broad subject, but the methods are generally categorized as either spectroscopic, electrochemical, or chromatographic. We will essentially take the cover off the "black box" and see how these instruments are constructed and measurements made from the underlying chemical and physical properties of the substance. Quantitative problem solving will be utilized as a means to demonstrate physical principles applied in the design and performance of instruments.

The goal of this course is not to make you an "expert" on each type of instrumentation encountered, but rather to introduce and educate you to the many types of instruments available for chemical analysis and the type(s) of information these instruments provide. It is my hope that you will then expand your knowledge of the instruments you come into contact with during your scientific career, thereby avoiding the "black box" problem.

Specific Course Objectives:

By the end of this course, you should:

Have an understanding of how chemical and physical properties of substances are used in the design and construction of sophisticated instrumentation used in chemical analysis
Have a broad knowledge of the types of instrumentation generally available and the information provided by each
Understand the advantages, disadvantages, and limitations of different instruments used for similar types of analyses
Use rigorous mathematical methods for evaluating instrument performance

Time/Location: 11:00 - 12:15 TR / Sims 301-B

Professor: Dr. C. Calloway callowayc@winthrop.edu

Office: 312-B Sims Hall; 323-4945

Office Hours: TRF 8:00 - 10:00 a.m. {and other times by appointment.}

Textbook: Principles of Instrumental Analysis, 5^thedition,Skoog, D.A., Holler, F.J., Nieman, T.A.

You may find the website, "Chemistry Hypermedia Project" (Analytical Chemistry Tutorial), a useful tool.

Grading/Evaluation:

Note: Since all graded work (including homework to be collected, quizzes, papers, mid-term examinations, final examination, research proposals, laboratory results and reports, etc.) may be used in the determination of academic progress, no collaboration on this work is permitted in this course unless the instructor explicitly indicates that some specific degree of collaboration is allowed. This statement is not intended to discourage students from studying together, seeking help from the instructor, or working together on assignments that are not to be collected.

Grades in this course will be determined from three sources, as follows:

Homework (20%): Periodically, homework problems will be assigned, from the textbook or as handouts, and collected. Of those assigned, a random number, or all, will be graded and returned. Due dates given for each assignment are the final date each assignment will be accepted.
Mid-term Exams (60%): There will be 4 exams given during the term covering the topics listed below. Make sure to bring a pencil and calculator to the exam. No make-up exams will be given. If an exam is missed with a valid excuse, as determined by the instructor, the final exam will count as the missed exam grade. The exams are scheduled as follows:

Exam 1: February 4
Exam 2: March 4
Exam 3: April 8
Exam 4: April 24

Final Examination: 20% {Thursday, May 1/11:30 a.m.} There will be a cumulative final examination given during exam week. If you score higher on the final exam than your lowest mid-term exam, the final exam grade will replace the lowest exam grade, before averaging.

Letter grades will be assigned as follows:

90 - 100%: A

80-89%: B

70-79%: C

60-69%: D

Menu of Topics:

Analytical Figures of Merit, Basic Electronics, Signal-to-Noise Theory (Ch. 1,2,and 5)

Exam 1

Spectroscopic Instrument Design & Atomic Spectroscopy - (Ch. 6 – 10)

Exam 2

Molecular Electronic and Vibrational Spectroscopy (Ch. 13-18)
Nuclear Magnetic Resonance Spectroscopy- (Ch. 13-19)

Exam 3

Atomic and Molecular Mass Spectrometry (Ch. 11,20)
Surface Analysis (Ch. 21)
Electro-analytical Chemistry (Ch. 22-25)

Exam 4

Students with Disabilities: If you have a disability and need classroom accommodations, please contact Services for Students with Disabilities, at 323-2233, as soon as possible. Once you have your “professor notification letter”, please notify me so that I am aware of your accommodations well before the first test.

My advice, to help you succeed in this endeavor:

Read your textbook.
Be sure you know how to do mean, standard deviation, and linear regression on your calculator.
Stay ahead of the lectures in your reading.
Work the homework problems by yourself, without any aid.
Don’t fall behind.
Wear sunscreen.
Read your textbook.
Floss at least once a day.
Talk to your professor, especially if you are confused.
Get a good night’s rest.
Read your textbook.
Sing occasionally.
Above all, read your textbook.

We, the members of the Winthrop University Community, pledge to hold ourselves and peers to the highest standards of honesty and integrity