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CHROMATOGRAPHY AND
SEPARATION SCIENCE
 This is Volume 4 of
SEPARATION SCIENCE AND TECHNOLOGY
A reference series edited by Satinder Ahuja
CHROMATOGRAPHY
AND SEPARATION
SCIENCE

Satinder Ahuja
Ahuja Consulting
Calabash, North Carolina

Amsterdam Boston London New York Oxford Paris San Diego

San Francisco Singapore Sydney Tokyo
This book is printed on acid-free paper. 1 s
Copyright ß 2003 Elsevier Science (USA)

All rights reserved.

No part of this publication may be reproduced or transmitted in any form or by any means,
electronic or mechanical, including photocopy, recording, or any information storage and
retrieval system, without permission in writing from the Publisher.

The appearance of the code at the bottom of the first page of a chapter in this book indicates the
Publisher’s consent that copies of the chapter may be made for personal or internal use of specific
clients. This consent is given on the condition, however, that the copier pay the stated per copy fee
through the Copyright Clearance Center, Inc. (222 Rosewood Drive, Danvers, Massachusetts
01923), for copying beyond that permitted by Sections 107 or 108 of the U.S. Copyright Law. This
consent does not extend to other kinds of copying, such as copying for general distribution, for
advertising or promotional purposes, for creating new collective works, or for resale. Copy fees for
pre-2003 chapters are as shown on the title pages. If no fee code appears on the title page, the copy fee
is the same as for current chapters. $35.00

Explicit permission from Academic Press is not required to reproduce a maximum of two figures
or tables from an Academic Press chapter in another scientific or research publication provided
that the material has not been credited to another source and that full credit to the Academic
Press chapter is given.

ACADEMIC PRESS
An Elsevier Science Imprint
525 B Street, Suite 1900, San Diego, California 92101-4495, USA
http://www.academicpress.com

International Standard Book Number: 0-12-044981-1

Printed in the United States of America

02 03 04 05 06 07 08 MM 9 8 7 6 5 4 3 2 1
CONTENTS

PREFACE ix

1 Relating Chromatography to Separations

I. Defining Separation 2
II. Evolution of Chromatography 3
III. Separations in Everyday Life 6
IV. Basis of Separations 7
V. Modes of Chromatography 13
VI. Unified Separation Science 14
VII. Selectivity and Detectability 15
References 16
Questions for Review 16

2 Simple Separation Methods

I. Evaporation 18
II. Precipitation 18
III. Crystallization 19
IV. Filtration 19
V. Membrane Separations 21
VI. Distillation 24
VII. Extraction 26
References 35
Questions for Review 35

v
vi CONTENTS

3 Equilibrium Processes in Separations

I. Molecular Interactions 38
II. Separation Thermodynamics 38
References 48
Questions for Review 48

4 The Molecular Basis of Separation

I. Molecular Interactions 49
II. Solubility Parameter Theory 60
III. Group Interactions 65
References 67
Questions for Review 67

5 MassTransport and Separation

I. Types of Diffusion 70
II. Modeling Diffusion 71
III. Chromatographic Implications 72
IV. Diffusion Rates in Various Media 74
V. Mass Transfer 77
References 79
Questions for Review 79

6 Chromatographic Methods
I. General Classification of Chromatographic Methods 84
II. Classification Based on Retention Mode 87
III. Classification Based on Sample Introduction 90
IV. Separation Characteristics of Chromatographic Methods 93
V. Basic Chromatographic Theory 95
References 99
Questions for Review 100

7 Paper Chromatography
I. Chromatography Paper 102
II. Sample Preparation 103
III. Sample Cleanup 104
IV. Derivatization 105
V. Mobile Phases and Stationary Phases 106
VI. Development of Chromatograms 110
VII. Detection 111
VIII. Quantitation 112
References 112
Questions for Review 112
CONTENTS vii

8 Thin-Layer Chromatography
I. Stationary Phases for TLC 114
II. TLC of Enantiomeric Compounds 117
III. Sample Application 119
IV. Mobile Phases 123
V. Development of Chromatograms 124
VI. Detection and Quantitation 125
VII. Applications 126
References 131
Questions for Review 131

9 Gas Chromatography
I. Equipment 134
II. Separation Process 135
III. Columns 136
IV. Gas Chromatographic Detectors 142
V. Recording and Analysis 145
VI. Resolution 146
VII. Selection of a Stationary Phase 147
References 152
Questions for Review 152

10 High-Pressure Liquid Chromatography

I. Evolution of HPLC 154
II. Advantages over Gas Chromatography (GC) 155
III. Separation Process 157
IV. Retention Parameters in HPLC 160
V. Resolution and Retention Time 163
VI. Equipment 167
VII. Separation Mechanism in HPLC 168
VIII. Stationary Phase Effects 179
IX. A Case Study of Retention Mechanism Investigations 180
X. Molecular Probes/Retention Index 182
XI. Mobile Phase Selection and Optimization 185
References 205
Questions for Review 208

11 Evolving Methods and Method Selection

I. Evolving Methodologies 211
II. Selection of a Separation Method 220
III. Chiral Separations 223
IV. Comparison of GC, SFC, HPLC, and CEC for a Selective Separation 239
References 240
Questions for Review 241

Index 243

vii
This Page Intentionally Left Blank
PREFACE

For more than 25 years, I led a group in Analytical R&D in a major

pharmaceutical company (Novartis), and also taught a course on chemical
separations at Pace University. I had the pleasure of succeeding Lloyd Snyder,
who had taught this course before me. We used Karger, Snyder, and Horvath’s
An Introduction to Separation Science (Wiley) as a text for this course. I also
taught graduate courses on separations and advanced biochemical analysis at
Rutgers University and a course on modern methods of chemical analysis at
Polytechnic University. I found that I had to use at least a dozen books
to convey the subject of chromatography and separation science to the
students. All of those books and more are adequately referenced in this
text to enable the reader to seek more details. The books that were found
especially useful, besides the one mentioned above, were Pecosk, Shields,
Cairns, and McWilliam’s Modern Chemical Analysis (Wiley), Stahl’s, Thin-
Layer Chromatography (Springer-Verlag), Snyder and Kirkland’s Introduction
to Modern Liquid Chromatography (Wiley), Poole and Poole’s Chromatog-
raphy Today (Elsevier), McNair and Miller’s Basic Gas Chromatography
(Wiley), Miller’s Separation Methods in Chemical Analysis (Wiley), Giddings’s
Dynamics of Chromatography (Marcel Dekker) and Unified Separation
Science (Wiley), and books by me, entitled Selectivity and Detectability
Optimizations in HPLC (Wiley), Trace and Ultratrace Analysis by HPLC
(Wiley), and Chiral Separations by Chromatography (Oxford). I am indebted
to the valuable contributions made by these scientists.
After several years of dealing with this number of books, it occurred to
me to plan a text that would cover this subject of chromatography and
separation science in a concise manner and avoid burdening the reader with
a lot of details and mathematical equations. This book is designed for
students and separation scientists who are not averse to learning a few

ix
x PREFACE

equations dealing with physicochemical processes that influence chromatog-

raphy and separations. The main objectives of this book are as follows:
. Provide basic information on chromatography and separation science.
. Describe the relationship between these important fields.
. Cover how simple extraction or partition processes provide the basis
for development of chromatography and separation science.
. Describe the role of chromatography and separation science in various
fields.
. Discuss the role of chromatography and separation science in
development of new methodology.
. Cover new evolving methods and show how to select an optimum
method.
Separation can be defined as an operation in which a mixture is divided
into at least two fractions having different composition, molecular mass, or
stereochemical structure. An actual separation is usually achieved by physical
process, although chemical reactions may occasionally be involved in this
process. It is important to learn the fundamental physical and chemical
phenomena involved in the achievement of separations, as well as those with
the development and application of various separation processes. This
continually evolving discipline is called separation science.
Chromatography derives its name from chroma and graphy, meaning
color writing. It is essentially a physical method of separation in which
components to be separated are distributed between two phases.
Chromatography is a powerful technique concerned with separations of a
large variety of complex compounds. The contributions of chromatography
to various scientific disciplines and the benefits that chromatography provide
to mankind are unparalelled. For example, the progress made in the
biological sciences such as biotechnology, clinical pharmacology/therapeutics,
and toxicology provides an excellent testimony to the contributions of
chromatography. Examples from these and other fields are included
throughout this textbook.
This book will provide the necessary information to improve the
comprehension of separation science. It will show how chromatography
relates to separation science and describe how simple separation methods
have led to highly useful chromatographic techniques that provide high
resolution (Chapters 1 and 2). To provide a better understanding of transport
phenomena and thermodynamics, an elementary discussion is included in
Chapters 3 to 5.
The discussion on chromatography should help improve the under-
standing of the principles involved in various modes of chromatography such
as paper chromatography, thin-layer chromatography, gas chromatography,
and high-pressure liquid chromatography (Chapters 6 to 10).
This book relates simple separation techniques—such as extraction—to
chromatography. And it lets us see how chromatography in turn relates to
capillary electrophoresis or field flow fractionation (Chapter 11).
PREFACE xi

I believe that both theory and many interesting applications of various

chromatographic and separation techniques included in this book will be
found useful by the readers.

November 6, 2002 Satinder Ahuja

This Page Intentionally Left Blank
1 RELATING CHROMATOGRAPHY TO
SEPARATIONS
I. DEFINING SEPARATION
II. EVOLUTION OF CHROMATOGRAPHY
A. Definition of Chromatography
B. Similarity of Chromatography to Separation Methods
III. SEPARATIONS IN EVERYDAY LIFE
IV. BASIS OF SEPARATIONS
A. Physicochemical Phenomena
B. Utilizing a Desirable Physical Property
V. MODES OF CHROMATOGRAPHY
A. AdsorptionVersus Absorption
B. Partition or Distribution
C. Exclusion
D. Ion Exchange
VI. UNIFIED SEPARATION SCIENCE
VII. SELECTIVITYAND DETECTABILITY
A. Selectivity
B. Detectability
REFERENCES
QUESTIONS FOR REVIEW

A chromatographic method can be considered simply a physical method of

separation in which components to be separated are distributed between two
phases. However, it should be recognized that chromatographic methods
have evolved into complex and elegant methods that utilize a variety of
physicochemical approaches to provide the desired separation of complex
molecules (see Chapters 6–10). Chromatography can be related directly to
some of the simple nonchromatographic separation methods by the same
common basic physicochemical principles employed in these methodologies
to achieve the desired results. We will see from the discussion in Sections I
and II that separation is a broad term that can include nonchromatographic
methods as well as all of the chromatographic methods, and it should be
recognized at the very outset that this does not imply that all separation
methods are chromatographic.
Chromatography provides a variety of powerful methods that can help
separate a large number of different compounds. As a matter of fact, it can be

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