CHEMISTRY 231,
SPRING, 2013
CHEMICAL
SEPARATIONS LABORATORY
Syllabus
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
Instructor:
Roy Dixon (office – Sequoia 446C, phone 8-6893, email:
rdixon@saclink.csus.edu)
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
Course
Emphasis:
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
Tentative
Schedule
Discussion
Topic Week
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
Laboratory
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
Grading:
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.