CHEMISTRY 231, SPRING, 2013
CHEMICAL SEPARATIONS LABORATORY
Meeting time, place:
Discussion – 5:00 – 5:50 pm, Monday, Sequoia 450
Laboratory – 6:00 – 8:30 pm, Monday and Wednesday, 5:00 - 7:30 pm, Sequoia 540
Roy Dixon (office – Sequoia 446C, phone 8-6893, email: email@example.com)
Tentative office hours: Monday 1:00 to 2:00, Thursday 11:00 to 12:00 and Friday 3:00 to 4:00.
Course Website: http://www.csus.edu/indiv/d/dixonr/C231/C231.htm
The main point to this laboratory is to provide students with “hands-on” and realistic experience in chemical separations. Since there is a “discussion” component to this class, we will also cover more practical aspects of separations and chromatography than topics covered in Chem. 230. Initial class work, demonstrations, and experiments will be aimed at providing experience on various instruments or methods, while later experiments are expected to be conducted by students fairly independently (e.g. I will provide advice but not detailed instructions). The separations to be covered will include "simple" separations (e.g. solid phase extractions) and chromatography. I expect this class will involve more analysis type applications and less reaction chemistry than expected from reading the catalog description.
Prerequisite: Chem 230
Introduction, Data Handling and Simple Extractions Jan. 28
Simple Extraction - Calculations, Feb. 4
Equipment and Methods
Extractions + low performance Chromatography Feb. 11
Quantitative Chromatography Feb. 18
Practical Aspects of GC Feb. 25
Practical Aspects of HPLC March 4
Remaining topics March 11
Student Derivatization Presentations Around April 29
Final Exam To be determined
Locker Check In Jan. 28
Instrumentation Demonstration Feb. 4
Set 1 Labs Started Feb. 6
Set 2 Labs Started March 4
Spring Break March 25
Set 3 Labs Started April 1
Term Project Started April 22
Homework and Quizzes (10%)
Final exam (15%)
Lab reports - written (65%) and oral (10%)
Homework and quizzes will be given more heavily at the beginning of the semester. You will be expected to learn how to do calculations related to standard and sample preparation and quantification of unknowns, including determination of uncertainties. Other calculations will be aimed at predicting the separations using simple methods and in calculating chromatography performance parameters. Other homework assignments will involve your use of scientific literature to find information of importance if you were developing a new method.
There will be a written final exam given following the completion of the lecture portion of the class (but no later than the week of May 13).
Lab reports generally will be due two weeks after the lab work is scheduled to be completed. Additional details on the lab reports will be given in a more detailed handout covering writing of reports and in the instructions for the individual laboratory experiments. You will give an oral report on the results of the set 3 laboratory experiment that will be oriented toward your selected sample. This will be graded on the preparation of the materials and on the delivery of the report.
Set 1 Labs will involve using HPLC and GC to a) learn how to use the instruments and b) develop methods for separating a set of compounds. Students will select one experiment (HPLC or GC) while the other experiment will be completed for training purposes with no report required. Once students have completed the Set 1 labs, you will be allowed to work with less supervision.
Set 2 Labs will involve using simple separation methods (solid phase extraction and solid phase microextraction) along with HPLC and GC.
Set 3 Labs will involve analysis of unknowns and samples of your choice using a chromatographic method that requires derivatization. Derivatization reactions will include derivatize fatty acids or carbonyl compounds (and perhaps the derivatization of sugars). In addition to the written report, you will give a brief (10 min.) oral presentation of your results, focusing on the samples of your choice.
There will be two term project options. One option will be to isolate an active ingredient in drugs or a natural product in foods or spices. Ideally, the isolated compound will then serve as a quantitative standard for analyzing the product. The other option is to utilize other chromatographic equipment (different than used for labs 1-3) for an analysis of a compound or compounds in a specific sample matrix. The other chromatographic equipment would be HPLC with an aerosol charge detector, HPLC with a fluorescence detector, or GC-MS Either term project is expected to be more independent.
Cheating in class: Student caught cheating during quizzes or exams, falsifying lab data, or plagiarizing reports will be subject to punishment. If you have questions on what constitutes plagiarism, see the instructor. Punishment may range from receiving a zero on the quiz/exam to expulsion from the university.