COURSE BOOK
for
Analytical Chemistry for Third Stage
Course name: Separation Methods
Academic Year: 2013-2014
Lecture's name: Dr. Azad T. Faizullah
Department of Chemistry
College of Science
University of Salahaddin
Email: drazad53@yahoo.com
Course Objective
“Separation Science”, is a senior level of undergraduate
course within the analytical chemistry lecture series. It is
concerned with all aspects of the chemical and physical
separation of substances, with particular emphasis on
separation as
a
tool for chemical identification and
measurement.
Throughout this course, lecture topics will be illustrated
with examples from biological, pharmaceutical, food &
drink, environmental sample analysis. This will give a sense
of the scope and impact of separation science on society, as
well as providing concrete examples on how to identify
appropriate separation and analysis strategies depending on
the target analyte(s) and sample matrix.
Course Syllabus:
2
There are 2 hr lectures weekly. The following provides an overview of
the topics covered during the semester:
1- Introduction
Important total analysis process steps:
 Sampling
 Methods
 Separation
 Quantitation
 Evaluation
2- Separation Science
-Definition of Separation Science
-Classification and Application of Separations
I- Separation by Phase-Formation methods
 Volatilization Methods (conversion of Solid to Gas)

Distillation Methods (conversion of Liquid to Gas)

Separation by Precipitation
II- Separation by Phase- transformation methods
 Extraction
1Solvent extraction (Liquid Extraction)
1.1.
The equilibrium constant
1.2.
Efficiency of extraction
1.3.
Selectivity of extraction
1.4.
Nature of partition forces
1.4.1. Dispersion interaction
1.4.2. Dipole-Dipole interaction
1.4.3. Induction interaction
1.4.4. 4-Hydrogen bonding
1.5. Extraction system
1.5.1. Extraction of Covalent, Neutral
Molecules
1.5.1.1. pH effect
1.5.1.2. Effect of complex formation
1.5.1.3. Effect of association
1.6. Methods of Extraction
1.6.1. Batch extraction
1.6.2. Continuous extraction
1.6.3. Multistage extraction
2- Solid-Phase Extraction (Liquid-Solid Extraction)
 Chromatographic Methods
1- Introduction and some important definition in Chromatography
3
2- Chromatographic Methods
2.1. Plate theory
2.2. Rate theory
3- Chromatographic resolution
4- Classifications of chromatographic Methods
5- Adsorption Chromatography
6- Partition Chromatography
7- Plane Chromatography
7.1. Paper Chromatography (PC)
7.1.1. Techniques of Paper Chromatography
7.1.2. Preparative paper chromatography
7.1.3. Qualitative and Quantitative application of PC
8- Thin Layer Chromatography (TLC)
9- Liquid Chromatography (LC)
10- High performance Liquid Chromatography (HPLC)
10.1. Bonded-Phase Column
10.2. Elution System
11- Ion-Pair Chromatography
12- Ion Exchange Chromatography (IEC)
13- Affinity Chromatography
14- Gas-Chromatography (GC)
Evaluation, Examination and Marking Scheme
Students will be expected to make full use of the
supplementary materials and case studies made available
through both lecture handouts and reference books.
4
Familiarity with the basic principles and calculations
employed
in
extraction,
general
separation
and
chromatography will be assumed. Students should consult
the
available
notes
and
supplemental
examples
for
specimen calculations and problems.
The students are required to do two closed exams and one
optional exam during the course period. All exams have
15% marks; the quiz tests have 5% marks, the attendance,
classroom, activities, absence count 5% marks. So that the
final grade will be based upon the following criteria:
Exams (closed and optional): 15%
The quiz tests and homework: 5%
Classroom participation and assignments: 5%
Practical Course 15%
Final Exam: 60% which include 45% for theoretical and
15% for practical.
Course Material
The student can find additional information and examples
in the following references
1- Modern Analytical Chemistry; by David Harvey.
5
2-
Ion Exchange and Solvent Extraction; Volume 13,
by
Jacob A. Marinsky and Yizhak Marcus.
3-
Fundamentals of Analytical Chemistry; Eighth Edition,
by Douglas A. Skoog, Donald M. West, F. James
Holler and Stanley R. Crouch.
4-
Chromatography and Separation Science; by Satinder
Ahuja.
5-
Chromatography : Concepts and Contrasts, by James
M. Miller.
6-
Chromatography: Fundamentals and Applications of
Chromatography and Related Differential Migration
Methods
Part
A:
Fundamentals
and
Techniques;
Journal of Chromatography Library — Volume 69A;
Sixth Edition, by E. Heftmann.
7-
Chemical
Separations :Principles,
Techniques,
and
Experiments; by Clifton E. Meloan.
8-
A Century of Separation Science; by Haleem J. Issaq.
9-
Solvent Extraction Principle and Practice;
Edition,
by
Jan
Rydberg,Claude
Second
Musikas
and
Gregory R. Choppin.
10- Quantitative Chromatographic Analysis; by Thomas E.
Beesley, Benjamin Buglio and Raymond P. W. Scott.
Course Program (Separation Methods)
Week 1:
1- Introduction
Important total analysis process steps:
 Sampling
6




Methods
Separation
Quantitation
Evaluation
2- Separation Science
-Definition of Separation Science
-Classification and Application of Separations
Week 2:
I- Separation by Phase-Formation methods
 Volatilization Methods (conversion of Solid to Gas)
 Distillation Methods (conversion of Liquid to Gas)
 Separation by Precipitation
II- Separation by Phase- transformation methods
 Extraction
Week 3:
1. Solvent extraction (Liquid extraction)
1.5. The equilibrium constant
1.6. Efficiency of extraction
1.7. Selectivity of extraction
1.8. Nature of partition forces
1.8.1.
Dispersion interaction
1.8.2.
Dipole-Dipole interaction
1.8.3.
Induction interaction
1.8.4. 4-Hydrogen bonding
Week 4:
1.5. Extraction system
1.5.1. Extraction of Covalent, Neutral
Molecules
1.5.1.1. pH effect
1.5.1.2. Effect of complex formation
1.5.1.3. Effect of association
1.6. Methods of Extraction
7
1.6.1. Batch extraction
1.6.2. Continuous extraction
1.6.3. Multistage extraction
2. Solid-Phase Extraction (Liquid-Solid Extraction)
Week 5:
First Examination
Week 6:
 Chromatographic Methods
1. Introduction and some important definition in
Chromatography
2. Chromatographic Methods
2.2. Plate theory
2.2. Rate theory
3. Chromatographic resolution
4. Classifications of chromatographic Methods
Week 7:
5. Adsorption Chromatography
6. Partition Chromatography
Week 8:
7. Plane Chromatography
7.1. Paper Chromatography (PC)
7.1.1. Techniques of Paper Chromatography
7.1.2. Preparative paper chromatography
7.1.3. Qualitative and Quantitative application of
PC
Week 9:
8- Thin Layer Chromatography (TLC)
Week 10:
9- Liquid Chromatography (LC)
10- High performance Liquid Chromatography (HPLC)
8
10.1. Bonded-Phase Column
10.2. Elution System
Week 11:
Second Examination
Week 12:
11- Ion-Pair Chromatography
12- Ion Exchange Chromatography (IEC)
13- Affinity chromatography
Week 13
13- Gas-Chromatography (GC)
Week 14:
Optional Examination
Week 15:
Seminar
9