CHE 526

THE UNIVERSITY OF KENTUCKY

DEPARTMENT OF CHEMISTRY

CHE 526 Chemical Separations

Spring Semester, 1998


Course Description: An advanced study of the theory, instrumentation, and analytical applications of chemical separation methods. Prereq: CHE 440G or CHE 444G or consent of instructor.

Course Information

Exams and Grading

Tests:

     Midterm Exam:            Tuesday, March 5, 7:00 p.m.
     Final Exam:              Tuesday, May 5, 1:00 p.m.
     Term paper (optional)    Due 5:00 p.m., Thursday, April 23.
                              No late papers will be accepted.
                              Need to let me know by April 9.

Grading Procedure

    Component      Option A    Option B
    Midterm Exam     40%         20%
    Term Paper                   20%
    Final Exam       60%         60%

Grades:

Usually, "A" corresponds to >90%, "B" to 80-89.9%, etc.

Important Dates

Academic Dishonesty

Academic dishonesty or cheating of any kind will not be tolerated. This is a serious offense and the instructor will make every effort to ensure that the punishment is immediate and severe. This is also the official policy of the Department of Chemistry.


Course Syllabus, CHE 526

I.	History and Introduction to Separations

II.	Mass Transport Processes
	A.	Diffusion and Fick's laws
	B.	Mass transfer through interfaces
	C.	Flow through tubes and packed columns
	D.	Compressible flow

III.	Thermodynamic and Molecular Basis of Equilibrium Separations
	A.	Thermodynamics of phase distributions
	B.	Intermolecular interactions
	C.	Predicting the distribution process

IV.	Introduction to Chromatography and Theory of Retention
	A.	Classification of chromatographic methods
	B.	Sorption isotherms
	C.	Dependence of chromatographic peak shape on sorption isotherms
	D.	Retention parameters and chromatographic symbols
	E.	Peak resolution
	F.	Optimizing the separation

V.	Kinetic Processes in Chromatography
	A.	Band-broadening mechanisms
	B.	The rate theory (van Deemter plot)
	C.	Comparison of gas, liquid, and supercritical fluid mobile phases 

VI. 	Chromatography on Planar Surfaces
	A.	Thin layer chromatography (TLC)
	B.	High performance TLC
	C.	Cellulosic sorbents
	D.	Chemically bonded phases in TLC
	E.	Modification of TLC plates
	F.	Equipment and apparatus

VII.	HPLC Instrumentation
	A.	From LC to HPLC
	B.  The HPLC Instrument
	C.	The HPLC columns
	D.	Mobile phase preparation
	E.	Pumps
	F.	Injection systems
	G. 	Guard and scavenger columns
	H. 	Detectors
	I.	Gradient Elution

VIII.	Adsorption Chromatography (Liquid-Solid Chromatography)
	A.	General remarks
	B.	Stationary phases
	C.	Choice of mobile phase
	D.	Flash chromatography

IX.	Partition Chromatography
	A.	Choice of solid support;  bonded phase packing material
	B.	Normal phase chromatography
	C.	Reverse phase chromatography
	D.	Columns for biomolecules
	E.	Determination of void volume
	F.	Chromatographic calibration
	G.	Bonded phases for flash chromatography
	H.	Secondary equilibria

X.	Ion-Exchange Chromatography - Ion Chromatography
	A.	Ion-exchange chromatography
	B.	Ion chromatography
	C.	Structure and properties of ion-exchange materials
	D.	Elution techniques

XI.	Size-Exclusion Chromatography 
	A.	Principle
	B.	Packing material
	C.	Practical concerns

XII.	Affinity Chromatography
	A.	Principles
	B.	Supports and immobilization procedures
	C.	Spacer arm concept

XIII.	Chiral Chromatography
	A.	General comments
	B.	Chromatographic behavior of stereoisomers
	C.	Chiral stationary phases

XIV.	Gas Chromatography
	A. 	Basic Instrumentation
	B.	Classification of GC methods
	C.	Stationary phase
	D.	Carrier Gas
	E.	Detectors
	F.	Temperature effect	
	G.	"Hyphenated methods": GC-MS, GC-FTIR


XV.	Electrophoresis
	A.	Principles
	B. 	SDS-PAGE
	C.	Capillary electrophoresis

XVI.	Supercritical Fluid Chromatography
	A. 	Supercritical fluids
	B.	Instrumentation

XVII.	Other Important Separation Topics (if time permits)

Resource Materials

Books on Reserve in the Library

1.	Giddings, Unified Separation Science, Wiley, 1991 
	QD63.S4 G53
2.	Poole and Schuette, "Contemporary Practice of Chromatography"
	QD79.C4 P66
3.	Karger, Snyder, and Horváth, "An Introduction to Separation Science"
	544 K1455C
4.	"High Performance Liquid Chromatography",  (Horváth, Ed),  Vol. 1 and 2,1980
	QD79.C454 H534
5.	Snyder and Kirkland, "Introduction to Modern Liquid Chromatography"
	QD79.C454 S58
6.	Scott, "Techniques and Practice of Chromatography"
	QD79.C4 S384

Bibliography

I.	History and Introduction to Separations
1.	Ettre, In "High Performance Liquid Chromatography",  (Horváth, Ed),  Vol. 1, 1980
2.	Berezkin, Chem. Rev., 89, 279-285 (1989)
3.	Ettre, J. Chromatogr., 535, 3-12 (1990)
4.	Scott, "Techniques and Practice of Chromatography", Chapter 1

II.	Mass Transport Processes
1.	Karger, Snyder, and Horváth, "An Introduction to Separation Science", Chapter 3
2.	Laub, In "Inorganic Chromatographic Analysis", Chemical Analysis Vol. 78, pp. 84-97, 1985
3.	Giddings, "Unified Separation Science", Chapters 3.5-3.6, 4

III.	Thermodynamic and Molecular Basis of Equilibrium Separation
1.	Karger, Snyder, and Horváth, "An Introduction to Separation Science", Chapter 2
2.	Dorsey, Chromatography, June 1987, p.37
3.	Giddings, "Unified Separation Science", Chapter 2
4.	Scott, "Techniques and Practice of Chromatography", Chapter 2

IV.	Introduction to chromatography and theory of retention
1.	Poole and Schuette, "Contemporary Practice of Chromatography", Chapter 1
2.	Karger, Snyder, and Horváth, "An Introduction to Separation Science", Chapter 5
3.	Snyder, J. Chromatogr. Sci., 10, 200-212 (1972)
4.	Giddings, "Unified Separation Science", Chapter 10
5.	Ettre, Pure Appl. Chem., 65, 819-872 (1993)
6.	Dolan, LC.GC, 12, 368-370 and 446-450 (1994)
7.	Scott, "Techniques and Practice of Chromatography", Chapters 4, 5

V. 	Kinetic processes in chromatography
1.	Poole and Schuette, "Contemporary Practice of Chromatography", Chapter 1
2.	Giddings, "Unified Separation Science", Chapters 11, 12
3.	Hawkes, J. Chem. Ed., 60, 393-398 (1983)
4.	Palmieri, J. Chem. Ed., 65, A254-A259 (1988)
5.	Scott, "Techniques and Practice of Chromatography", Chapter 3

VI.	Chromatography on planar surfaces
1.	Poole and Schuette, "Contemporary Practice of Chromatography", Chapter 9
2.	Donovan, Gould and Majors, LC.GC, 5, 1024 (1987)
3.	Hauck and Mack, LC.GC, 8, 88-96 (1990)
4.	Kalász, Ettre and Báthori, LC.GC, 15, 1044-1050 (1997)
5.	Vogel's Textbook of Practical Organic Chemistry, 5th Edition, 199-209
6.	Scott, "Techniques and Practice of Chromatography", Chapters 14, 15

VII. Adsorption chromatography (liquid-solid chromatography)
1.	Poole and Schuette, "Contemporary Practice of Chromatography", Chapter 4.10
2.	Engelhardt and Elgass, In "High Performance Liquid Chromatography", (Horváth, Ed), Vol. 2, 1980
3.	Still, Kahn and Mitra, J. Org. Chem., 43, 2923-2925 (1978)
4.	Vogel's Textbook of Practical Organic Chemistry, 5th Edition, 217-220

VIII. HPLC Instrumentation
1.	Poole and Schuette, "Contemporary Practice of Chromatography", Chapters 4.4 and 5
2.	Dolan, LC.GC, 15, 110-113 (1997)
3.	Dolan, LC.GC, 9, 344-348 (1991)
4.	Warner, Anal. Chem., 66, 601A-606A (1994)
5.	Niessen and Tinke, J. Chromatogr., 703, 37-57 (1995)
6.	Volmer and Vollmer, LC.GC, 14, 236-242 (1996)
7.	Freeman, Daunert and Bachas, LC.GC, 10, 112-118 (1992)
8.	Scott, "Techniques and Practice of Chromatography", Chapters 10-12

IX. 	Partition chromatography
1.	Poole and Schuette, "Contemporary Practice of Chromatography", Chapter 4
2.	Meyer, "Practical High-Performance Liquid Chromatography", 2nd Ed., 1994
3.	Sadek, Carr, and Bowers, LC, 3, 590-592 (1985)
4.	Foley, Chromatography, June 1987, 43

X.	Ion-exchange chromatography - ion chromatography
1.	Poole and Schuette, "Contemporary Practice of Chromatography", Chapter 4.14, 4.15
2.	Fritz, Anal. Chem., 59, 335A-344A (1987)
3.	Small and Miller, Anal. Chem., 54, 462-469 (1982)
4.	Dasgupta, Anal. Chem., 64, 775A-782A (1992)
5.	Noble, Anal. Chem., 67, 205A-208A (1995)

XI.	Size-exclusion chromatography - gel filtration
1.	Poole and Schuette, "Contemporary Practice of Chromatography", Chapter 4.13
2.	Dolan, LC-GC, 8, 290-294 (1990)
3.	Ettre, Pure Appl. Chem., 65, 819-872 (1993), Section 6

XII.	Affinity chromatography
1.	Parikh and Cuatrecasas, C&EN, August 26, 1985, 17-32 (1985)

XIII. Chiral Chromatography
1.	Poole and Poole, "Chromatography Today", Chapter 8.15
2.	Dappen, Arm and Meyer, J. Chromatogr., 373, 1-20 (1986)
3.	Armstrong and Han, CRC Critical Rev. Anal. Chem., 19, 175-224 (1988)

XIV. Gas chromatography
1.	Poole and Schuette, "Contemporary Practice of Chromatography", Chapters 2 and 3
2.	Klee, LC-GC, 5, 774-782 (1987)
3.	Westmoreland and Rhodes, Pure Appl. Chem., 61, 1147-1160 (1989)

XV. Electrophoresis
1.	Jorgenson, Anal. Chem., 58, 743A-760A (1986)
2.	Ewing et al., Anal. Chem., 61, 292A-303AA (1989)
3.	Warner, Anal. Chem., 66, 1137A-1141A (1994)


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