CHEMICAL SEPARATION TECHNIQUES. SYLLABUS ~ Autumn 2017 MWF 2:30-3:20 PM Bagley Hall 261

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1 CHEM 429 / 529 CHEMICAL SEPARATION TECHNIQUES SYLLABUS ~ Autumn 2017 MWF 2:30-3:20 PM Bagley Hall 261 INSTRUCTOR: OFFICE HOURS: TEXTBOOKS: LECTURE NOTES: PROBLEM SETS: Professor Robert E. Synovec Chemistry Library Bldg , synovec@chem.washington.edu By appointment only (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 and supplemental information will be available on the class WEB site posted on Canvas. 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

2 CHEM 429 COURSE GRADING: Grades are calculated based on your final percentage (100% possible). There will be two mid-term quizzes (25% of grade each), and a final exam (50% of grade). 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% of grade each), and a final exam (40% of grade). For graduate students, a special topic report (20% of grade) 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. All quizzes are graded on a 50 point scale, while the final is graded on a 100 point scale. For CHEM 529 (only) the special topic report is graded on a 50 point scale.

3 CHEM 529 Special Topic Report Technology Development, Separation Fundamentals, Key Applications The special topic report 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 can relate to stationary phase and instrumentation design, detection, 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 three research groups, and at least one publication (since 2005) from each research group must be critically evaluated. The report must contain at least 10 references overall (some references older than 2005 are acceptable, and even encouraged to provide historical context). The report should demonstrate the development of the state-of-the-art in Chemical Separation Techniques, 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 Nov 17, The due date is Thursday, Dec 14 at 5:00 PM, submitted electronically as a pdf. Each day the report is late is a 5 point deduction on the 50 point scale. 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.

4 COURSE SCHEDULE Chemistry 429 / 529: concepts and topics (Autumn 2017) page 4 Lectures Sept 27 Sept 29 Oct 2,4 Oct 6 Oct 9,11 Oct 13 Oct 16 Oct 18 Oct 20 Topic(s) Introduction to course and separation science issues. Chromatography illustration of separation mechanism, instrumentation, data and band broadening (BB), with thermodynamics and mass transfer kinetics. Motivations to study band broadening (BB): C(t), S(t), LOD, Rs and N. Column and stationary phase materials. BB Theory molecular basis: define H, and contributions to H, stationary phase materials, fluid dynamics: convection and diffusion. Comprehensive BB equation (Giddings), fluid mechanics for separations, separation performance: Gas vs. Liquid mobile phase behavior. Separation trade-offs and optimization chemical selectivity (w.r.t. resolution), instrumental performance and analysis time. Liquid Chromatography: Normal Phase (NP-LC) and Reversed Phase (RP-LC) Modes; Bonded Phase HPLC; RP-LC mechanism. 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. Oct 23 Quiz 1: Lectures Sept 27 Oct 16 Oct 25 Oct 27 Oct 30 Nov 1 Nov 3 Nov 6 Nov 8 Detection methods for LC, GC and CE; univariate and multichannel detection approaches Gas Chromatography: instrumentation, separation theory for capillary (Golay equation), GC-MS (mass spectrometry detection) Resistively heated GC-on-a-chip, high-speed GC 2D Separations, GC x GC, LC x LC Supercritical Fluid Chromatography: SF behavior as mobile phase, instrumentation, LC with water: theory and examples Size Exclusion Chromatography: stationary phase design, separation mechanism, theory, data analysis for molecular weight determination. Monolithic stationary phases; Chiral stationary phases & separations

5 COURSE SCHEDULE Chemistry 429 / 529: concepts and topics (Autumn 2017) page 5 Lecture Nov 13 Nov 15 Topic(s) Ion Chromatography: stationary phase design, ion-exchange theory, selectivity and separation of anions Nov 17 Quiz 2: Lectures Oct 18 Nov 8 Nov 20 Nov 22 Nov 27 Nov 29 Dec 1 Dec 4 Dec 6 Dec 8 Special Topic: Fuels Analysis using GC x GC TOFMS with Chemometrics No Lecture Ion Chromatography Detection and Instrument Development: conductivity detection, micromembrane suppression 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 Sample Preparation: Solvent Extraction, Solid Phase Extraction (SPE), Solid Phase Microextraction (SPME) with applications to HPLC, GC and Ion Chromatography Electrophoresis: electrophoretic migration, capillary electrophoresis (CE), electroosmotic flow, BB behavior and separation optimization State-of-the-art CE: Theory vs. Experiment, CE-on-a-chip FINAL EXAM: 2:30 4:20 P.M., Tuesday, Dec 12, 2017, Comprehensive CHEM 529 Report: 5:00 P.M., Thursday, Dec 14, 2017, pdf

CHEM 429 / 529 Chemical Separation Techniques

CHEM 429 / 529 Chemical Separation Techniques Robert E. Synovec, Professor Department of Chemistry University of Washington Lecture 1 Course Introduction Goal Chromatography and Related Techniques Obtain