CHEM 429 / 529 CHEMICAL SEPARATION TECHNIQUES

SYLLABUS ~ Autumn 2015 MWF 2:30 - 3:20 PM Bagley Hall 261

INSTRUCTOR: Professor Robert E. Synovec

Chemistry Library Bldg. 149
685-2328, synovec@chem.washington.edu

OFFICE HOURS: By appointment only

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, or buy used one.

LECTURE NOTES: Lecture note supplemental information will

be available on the class WEB site at
http://depts.washington.edu/synlab/. 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, et. al.
------------------------------------------
Role of Separation Techniques in Chemical Analysis 1 1
General Chromatography Theory and Background 11, 12 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
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CHEM 429 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 3.0. An overall
percentage of 90% will earn a 4.0 grade.

CHEM 529 COURSE GRADING:

Grades are calculated based on your final percentage (100% possible).

There will be two mid-term quizzes (20% each), and a final exam (40%).
For graduate students, a special topic report (20%) is required. 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 3.5. An overall percentage of 90%
will earn a 4.0 grade.
CHEM 529 Special Topic Report: Technology Development
The special topic report for CHEM 529 is a critical evaluation of an important aspect
of Chemical Separation Techniques and Separation Science. The report can
directly relate to one or more of the concepts/topics covered in the course, however
the scope of possible report topics is not limited to concepts/topics covered in the
course. You can think more broadly. Topics to select from can relate to stationary
phase design, instrumentation such as in detection and microfabrication, novel
sampling and sample prep, data analysis software, and so on. The special topic
report must reflect the integration and/or the building upon the research efforts
from a minimum of two research groups, with at least one publication (since 2000)
from each research group must be critically evaluated. The Report must contain at
least 10 references overall (some references older than 2000 are acceptable in the
total). The report should demonstrate the development of the state-of-the-art in
Chemical Separation Techniques and Separation Science, so the most recently
published references are encouraged. Students enrolled in CHEM 529 must
select their topic and have it approved by the instructor no later than Dec 1,
2015. The due date is Dec 17 at 5:00 PM, submitted electronically as a pdf.

The following rubric must be followed, with all text 1.5-spaced (6 pages text total,
plus figures and tables with captions on 2 pages following the references list), using
bolded words as headings:

Page 1. Report title, author name and affiliation.

Page 1. Abstract: This must be a summary with a 200 to 250 word count. The
abstract must contain quantitative information that relates to your report. For
example, figures of merit and/or performance data that quantitatively (i.e.,
analytically) describes the state-of-the-art for the topic.

Page 2,3. Introduction and Background: Describe the technology topic you have
selected and why you selected it. Basically, include the chemical analysis needs
and challenges that are being addressed by the technology you are reporting.

Pages 4,5. Experimental and Technology: Describe in sufficient detail what the
technology is all about (with references). For example, if it is a new stationary
phase design, go into the dimensional and compositional details and relate as much
as possible to concepts presented in the course. Include and discuss salient data
results (eg., figures and tables, citing source references) for how the new
technology performs.

Page 6. Future prospectus: What are the challenges and/or shortcomings that
still need to be addressed by the technology? Is there room for improvement, and if
so, how? References: also on page 6, list references cited in text using numbers.
COURSE SCHEDULE
Chemistry 429 / 529: concepts and topics (Autumn 2015) page 4

Lectures Topic(s)

Sept 30 Introduction to course and separation science issues.

Oct 2 Chromatography – illustration of separation mechanism,

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

Oct 5,7 Motivations to study band broadening (BB): C(t), S(t), LOD, Rs and N.
Column and stationary phase materials.

Oct 9 BB Theory – molecular basis: define H, and contributions to H,

stationary phase materials, fluid dynamics: convection and diffusion.

Oct 12, 14, 16 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.

Oct 19 Liquid Chromatography: Normal Phase (NP-LC) and Reversed

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

Oct 21 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.

October 23 Review

Monday, October 26 Quiz 1 Lectures Sept 30 – Oct 23 (50 pts, 25% / 20%)

Oct 28 Detection methods for LC, GC and CE; univariate and multichannel
detection approaches

Oct 30 Gas Chromatography: instrumentation, separation theory for capillary

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

Nov 2 Resistively heated GC-on-a-chip, high-speed GC

Nov 4 2D Separations, GC x GC, LC x LC

COURSE SCHEDULE
Chemistry 429 / 529: concepts and topics (Autumn 2015) page 5

Lecture Topic(s)

Nov 6 Special Topic: GC x GC – TOFMS data analysis and forensics

Nov 9 Supercritical Fluid Chromatography: SF behavior as mobile phase,

instrumentation, LC with water: theory and examples

Nov 13 Size Exclusion Chromatography: stationary phase design, separation

mechanism, theory, data analysis for molecular weight determination.

Nov 16 Monolithic stationary phases; Chiral stationary phases & separations

Nov 18 Review

Friday, Nov 20 Quiz 2 Lectures Oct 28 – Nov 18 (50 pts, 25% / 20%)

Nov 23 Ion Chromatography: stationary phase design, ion-exchange

theory, selectivity and separation of anions

Nov 25 Special Topic: Advanced Sample Preparation and Method Validation

Nov 30 Ion Chromatography – Detection and Instrument Development:

conductivity detection, micromembrane suppression

Dec 2 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

Dec 4 Electrophoresis: electrophoretic migration, capillary electrophoresis

(CE), electro-osmotic flow, BB behavior and separation optimization

Dec 7 State-of-the-art CE: Theory vs. Experiment, CE-on-a-chip

Dec 9 SDS-PAGE for protein separations: separation mechanism and

data analysis; Capillary Gel Electrophoresis for DNA sequencing

Dec 11 Review

FINAL EXAM: 2:30 – 4:20 P.M., Tuesday, Dec 15, 2015 (100 pts, 50% / 40%),
Lectures Nov 23 – Dec 11 (30 pts) and Comprehensive Review (70 pts)

CHEM 529 Report: 5:00 P.M., Thursday, Dec 17, 2015, email pdf (50 pts, 20%)