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CHEM 429 CHEMICAL SEPARATION TECHNIQUES

SYLLABUS ~ Spring 2015 MWF 1:30 - 2:20 PM Bagley Hall 261

INSTRUCTOR: Professor Robert E. Synovec Chemistry Library Bldg. 149


685-2328, synovec@chem.washington.edu

OFFICE HOURS: Monday, Friday, 2:30 3:30 PM, or by appointment

TEXTBOOKS: (1) "Unified Separation Science" by J.C. Giddings


(2) "Principles and Practice of Modern Chromatographic Methods
by K. Robards, P.R. Haddad and P. E. Jackson.
Limited quantities are available in the University Book Store.
If current stock is empty, they can order one for you.

LECTURE NOTES: Lecture note supplemental information will be available on the class
WEB site at http://synoveclab.chem.washington.edu. Print out prior
to the lectures for convenience.

PROBLEM SETS: Problem sets are on the class web site. They are not graded but
students are urged to master these problem sets. Problem sets,
keys and previous exams are all posted on the class WEB site.

COURSE READING: Text Chapters:


Giddings Robards, Haddad,Jackson
-----------------------------------------------------------------------------
Role of Separation Techniques in Chemical Analysis 1 1
General Chromatography Theory and Background 11, 12 (3-5, 9.13, 10 optional) 2
High Performance Liquid Chromatography (HPLC) 5, 6
Gas Chromatography (GC) 3
Two-Dimensional and Hyphenated Separations 6 (esp.6.4)
Supercritical Fluid Chromatography (SFC) 7
Size-Exclusion Chromatography (SEC) 6.2
Ion Chromatography 6.3
Electrophoresis 8

COURSE SCHEDULE: See pages 2 and 3

COURSE GRADING: Grades are calculated based on your final percentage (100% possible).
There will be two mid-term quizzes (25% each), and a final exam (50%). Quizzes and/or the final
exam can not be dropped. With an excused absence, students will have the opportunity to make
up a missed quiz and/or the final exam. All excused absence requests will be evaluated for
approval by Paul Miller in Undergraduate Services in Bagley 303D. The average grade for the
past five years has been 3.1. An overall percentage of 90% will earn a 4.0 grade.
COURSE SCHEDULE
Chemistry 429: concepts and topics (Spring 2015) page 2

Lectures Topic(s)

Mar 30 Introduction to course and separation science issues.

Apr 1 Chromatography illustration of separation mechanism,


instrumentation, data and band broadening (BB), with thermodynamics
and mass transfer kinetics.

Apr 3, 6 Motivations to study band broadening (BB): C(t), S(t), LOD, Rs and N.
Column and stationary phase materials.

Apr 8 BB Theory molecular basis: define H, and contributions to H,


stationary phase materials, fluid dynamics: convection and diffusion.

Apr 10, 13, 15 Comprehensive BB equation (Giddings) - separation performance:


Gas vs. Liquid mobile phase behavior. Separation trade-offs and
optimization chemical selectivity (w.r.t. resolution), instrumental
performance and analysis time.

Apr 17 Liquid Chromatography: Normal Phase (NP-LC) and Reversed


Phase (RP-LC) Modes; Bonded Phase HPLC; RP-LC mechanism.

Apr 20 Peak width dependence on the retention factor, k, packed column


(Modified Giddings equation); General elution problem, RP-LC
separation optimization through gradient elution; NP-LC case study.

April 22 Review

Friday, April 24 Quiz 1 Lectures Mar 30 Apr 20 (50 pts, 25%)

Apr 27 Detection methods for LC, GC and CE; univariate and multichannel
detection approaches

Apr 29 Gas Chromatography: instrumentation, separation theory for capillary


(Golay equation), GC-MS (mass spectrometry detection)

May 1 Resistively heated GC-on-a-chip, high-speed GC

May 4 2D Separations, GC x GC, etc (separate lecture notes)


COURSE SCHEDULE
Chemistry 429: concepts and topics (Spring 2015) page 3

Lecture Topic(s)

May 6 Supercritical Fluid Chromatography: SF behavior as mobile phase,


instrumentation, LC with water: theory and examples

May 8 Size Exclusion Chromatography: stationary phase design, separation


mechanism, theory, data analysis for molecular weight determination.

May 11 Monolithic stationary phases; Chiral stationary phases & separations

May 13 Review

May 15 Guest Lecture: Special Topics in Separation Science

Monday, May 18 Quiz 2 Lectures Apr 27 May 11 (50 pts, 25%)

May 20 Ion Chromatography: stationary phase design, ion-exchange


theory, selectivity and separation of anions

May 22 Ion Chromatography: Detection and Instrument Development:


conductivity detection, micromembrane suppression

May 27 Mixed Mode RP-LC: cation separations, mobile phase chemistry, post
column reagent chemistry to enhance sensitivity, mixed mode chemistry
ion exchange and hydrophobic interactions, micelles and surfactants

May 29 Electrophoresis: electrophoretic migration, capillary electrophoresis,


electro-osmotic flow, BB behavior and separation optimization

Jun 1 Capillary electrophoresis state-of-the-art: Theory vs. Experiment,


CE-on-a-chip

Jun 3 Guest Lecture: Topic TBA

Jun 5 Review

FINAL EXAM: Monday, June 8, 2:30 4:20 (100 pts, 50%)


Comprised of Lectures May 20 May 29 (30 pts), and Comprehensive Review
(70 pts)