Analytical Separation Science.

Format:

Book

Author/Creator:

Pirok, Bob W. J.

Contributor:

Schoenmakers, Peter J.

Language:

English

Subjects (All):

Chromatographic analysis.

Analytical chemistry.

Physical Description:

1 online resource (0 pages)

Edition:

1st ed.

Place of Publication:

Cambridge : Royal Society of Chemistry, The, 2025.

Summary:

Students and practising analysts will find the majority of all the important aspects of analytical separation sciences in this teaching textbook.

Contents:

Intro

Chapter 1: Fundamentalsof Chromatography

1.1 Chromatography (B)

1.1.1 Chromatographic Separation

1.1.2 Thin-layer Chromatography

1.1.3 Column Chromatography

1.2 Retention (B)

1.3 Selectivity (B

1.4 Efficiency (B)

1.4.1 Diffusion

1.4.3 The Plate Number

1.4.4 The van Deemter Equation

1.4.5 Peak Dilution

1.5 Resolution and Peak Capacity (B)

1.5.1 Resolution

1.5.2 Peak Capacity

1.6 Equilibria and Migration (M)

1.6.1 Thermodynamics of Retention

1.6.2 Phase Ratio

1.6.3 Flow Profiles

1.6.4 Column Permeability

1.7 Band Broadening (M)

1.7.1 Revisiting the van Deemter Equation

1.7.2 Effect of Diffusion Coefficient and Particle Size

1.7.3 Reduced Plate-height Equations

1.7.4 Plate-height Theory - A Closer Look

1.7.5 Extra-column Band Broadening

1.7.6 Heat Dissipation

1.7.7 Open-tubular Columns - The Golay Equation

1.7.8 Applicability of Open-tubular Columns in Liquid Chromatography

1.8 Adsorption Isotherms (M)

Acknowledgements

References

Chapter 2: Gas Chromatography

2.1 Introduction to Gas Chromatography (B)

2.1.1 Basic Instrumentation and Operation

2.1.2 Selectivity

2.1.3 Retention Indices

2.1.4 Stationary Phas

2.1.5 Open-tubular Columns

2.1.6 Basic Gas Chromatography-Mass Spectrometry

2.2 Retention (M)

2.3 The Mobile Phase (M)

2.4 Injectors for Gas Chromatography (M)

2.4.1 Split/Splitless Injector

2.4.2 On-column Injector

2.4.3 Programmed-temperature Vaporizer Injector

2.4.4 Headspace Injec

2.4.5 Thermal Desorption

2.5 Detectors for Gas Chromatography (B)

2.5.1 Flame-ionization Detector

2.5.2 Thermal Conductivity Detector

2.5.3 Photoionization Detecto

2.5.4 Element-specific Detecto

2.5.5 Atomic-emission Detector

2.5.6 Infrared Spectroscopy

2.5.7 Ultraviolet Spectroscopy.

2.5.8 Olfactometry

2.6 Gas Chromatography-Mass Spectrometry(M)

2.6.1 Ionization Methods

2.6.2 Mass Analyzers

2.7 Controlling Flow and Temperature (A)

2.7.1 Flow Control

2.7.2 Temperature Control

2.8 Column Characterization (A)

2.9 Correcting for Mobile-phase Compressibility (A)

2.10 Practical Tips and Troubleshooting for GC (M)

2.10.1 Carrier Gases

2.10.2 GC Columns

2.10.3 Poor Peak Shapes

2.10.4 Flow Control

2.10.5 Bleeding Septa

Chapter 3: Liquid Chromatography

3.1 Basics of Liquid Chromatography (B)

3.1.1 Introduction

3.1.2 Basic Instrumentation and Operation

3.1.3 Retention in LC

3.1.4 Determining the Hold-up Volume in Liquid Chromatography

3.2 Stationary-phase Materials (B)

3.2.1 Column Packing

3.2.2 Silica

3.2.3 Alternatives to Silica

3.2.4 Monolithic Columns

3.2.5 New Column Technol

3.3 Instrumentation (B)

3.3.1 Hardware

3.3.2 Ultra-high-pressure Liquid Chromatography

3.3.3 Extra-column Band Broadening

3.3.4 High-temperature Liquid Chromatogra

3.3.5 Miniaturization

3.4 Gradient Elution (M)

3.4.1 Introduction to Gradient Elution

3.4.2 Retention Times Under Gradient-elution Conditions

3.5 Reversed-phase Liquid Chromatography(B)

3.5.1 Introduction to Reversed-phase LiquidChromatography

3.5.2 Mobile-phase Viscosity

3.5.3 Iso-eluotropic Mixtures

3.5.4 Mobile-phase pH

3.5.5 Injection Solvents

3.5.6 Column Testing

3.6 Normal-phase Liquid Chromatography (B)

3.6.1 Classical Normal-phase Liquid Chromatography

3.6.2 Hydrophilic-interaction Liquid Chromatography

3.7 Separation of Ions (M)

3.7.1 Ion-exchange Chromatography

3.7.2 Ion Chromatography

3.7.3 Ion-pair Chromatography

3.7.4 Ion-exclusion Chromatography

3.8 Retention Models (M).

3.8.1 Usefulness of Retention Models

3.8.2 Quantitative Structure-Retention Relationships

3.8.3 Single-variable Models

3.8.4 Multi-variable Models

3.9 LC Detectors (B)

3.9.1 Refractive Index Detection

3.9.2 UV-Vis Detection

3.9.3 Fluorescence Detection

3.9.4 Evaporative Light-scattering Detection

3.9.5 Electrical Detection

3.9.6 Comparison of Main Detection Methods

3.9.7 Other LC Detectors

3.10 Hyphenation and LC-MS (M)

3.10.1 LC-MS

3.10.2 Spectroscopy Hyphenated with LC

3.11 LC Troubleshooting (M)

3.11.1 Introduction

3.11.2 Test Mixture

3.11.3 Pressure Traces

3.11.4 Peak Shapes

3.11.5 Other Issues

3.12 Preparative LC (A)

3.12.1 Introduction to Preparative LC

3.12.2 Counter-current Chromatography

3.12.3 Simulated Moving Bed Chromatography

3.13 Chiral Recognition (A)

3.14 Micellar Liquid Chromatography (A)

3.15 Specific Protein-separation Methods (A)

3.15.1 Hydrophobic-interaction Chromatography

3.15.2 Affinity Chromatography

3.15.3 Metal-ion Affinity Chromatography

3.15.4 Chromatofocussing

3.16 Kinetic Plots (A)

3.17 Gradient Elution - A Closer Look (A)

3.17.1 Deriving Retention Equations

3.17.2 Gradient Scanning

3.17.3 Multi-segment Gradients

3.17.4 Gradient Deformation

Chapter 4: Separation of Large Molecules

4.1 Introduction (B)

4.1.1 Characteristics of Large Molecules

4.2 Size-exclusion Chromatography (B)

4.2.1 Fundamental Concept

4.2.2 SEC Columns

4.3.2 Gradient Liquid Chromatography of Polymers

4.4 Hydrodynamic Chromatography (A)

4.5 Field-flow Fractionation (A)

4.5.1 Concept and Modes

4.5.2 Asymmetric Flow Field-flow Fractionation (AF4)

4.6 Detection Techniques for Large Molecules (A)

4.6.1 Static Light Scattering Detection

4.6.2 Dynamic Light Scattering Detection.

4.6.3 Viscometric Detection

4.6.4 Universal Calibration

Recommended Reading

Chapter 5: Capillary Electrophoresis

5.1 Principles of Capillary Electrophoresis (M)

5.1.1 Basic Theory

5.1.2 Electro-osmotic Flow

5.1.3 Band Broadening in Capillary Electrophoresis (B)

5.1.4 Electromigration Methods

5.2 Instrumentation for Capillary Electrophoresis (B)

5.2.1 General Instrumentation

5.2.2 Injection Methods

5.2.3 Detection Methods

5.2.4 Microfluidics

5.3 Capillary Electrophoresis-Mass Spectrometry (M)

5.4 Micellar Electrokinetic Chromatography(A)

5.4.1 Retention and Selectivity

5.4.2 Analyte Focussing

Chapter 6: Supercritical Fluid Chromatography

6.1 Introduction (M)

6.1.1 Supercritical Fluids

6.1.2 Why SFC?

6.1.3 Retention in SFC

6.1.4 Viscosity and Pressure Drop

6.1.5 Diffusion Coefficients

6.2 Packed-column SFC (B)

6.2.1 Setup

6.2.2 The Roles of Modifiers

6.3 Open-tubular-column SFC (M)

6.4 Enhanced Fluidity Liquid Chromatography (A)

Chapter 7: Multi-dimensional Separations

7.1 General Principles (M)

7.1.1 Introduction to Multi-dimensional Separations

7.1.2 Modes of Separations

7.1.3 Hardware for 2D Separations

7.1.4 Rationale for Two-dimensional Separations

7.1.5 Key Concepts of Comprehensive 2D Chromatography

7.1.6 Dilution Factors in LC×LC

7.2 Two-dimensional Gas Chromatography (M)

7.2.1 Heart-cut Two-dimensional Gas Chromatography(GC-GC)

7.2.2 Hardware for GC-GC

7.2.3 Comprehensive Two-dimensional Gas Chromatography (GC×GC)

7.2.4 Modulation

7.2.5 Selectivity in GC×GC

7.2.6 Structured Chromatograms

7.3 Two-dimensional Liquid Chromatography (M)

7.3.1 Introduction.

7.3.2 Target Applications of LC-LC and LC×LC

7.3.3 Instrumentation

7.3.4 Modulation

7.3.5 Mobile Phase Composition Programs for LC×LC

7.3.6 Achieving Selectivity

7.4 LC Hyphenated with GC (LC-GC) (A)

7.5 Other 2D Techniques (A)

7.5.1 Two-dimensional Electrophoresis

7.5.2 Coupling Liquid Chromatography with Electromigration

7.5.3 Combinations of Supercritical-fluid Chromatography and Liquid Chromatography

Chapter 8: Sample Preparation

8.1 Introduction to Sample Preparation (B)

8.1.1 Aim of Sample Preparation

8.1.2 Sampling and Sample Pre-treatment

8.2 Extraction Methods (B)

8.2.1 Extractions with Liquids or Supercritical Fluids

8.2.2 Solid-phase Extraction

8.2.3 Micro-extraction Methods

8.2.4 Overview of Extraction Techniques

8.2.5 Alternatives to Extraction

8.3 Derivatization and Fragmentation (B)

8.3.1 Derivatization

8.3.2 Derivatization Reactions to Improve Sampling and Sample Preparation

8.3.3 Derivatization Reactions to Improve Liquidphase Separations

8.3.4 Derivatization Reactions to Improve GC

8.3.5 Breaking Down Molecules

Chapter 9: Data Analysis: Chemometrics and Statistics

9.1 Introduction to Quantitative Analysis (B)

9.1.1 The Need for Chemometrics and Statistics in Separation Science

9.1.2 Variables and Data Order

9.1.3 Calibration Curve

9.1.4 Peak Height Versus Peak Area

9.1.5 Internal Standard

9.1.6 Detector Linearity

9.2 Repeated Measurements (B)

9.2.1 Errors

9.2.2 Descriptive Statistics.

9.2.3 Confidence Intervals.

Notes:

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ISBN:

1-83767-483-3

1-83767-482-5

OCLC:

1524434703