Thin-Layer Chromatography,9780854045358

Thin-Layer Chromatography

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ISBN13: 9780854045358
ISBN10: 085404535X
Format: Hardcover
Pub. Date: 2005-11-01
Publisher(s): Royal Society of Chemistry
List Price: $140.00

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Summary

Thin-Layer Chromatography (TLC) is a modern, reliable tool that complements other chromatographic techniques. This book provides a practical guide to the basic principles, procedures, and pitfalls on the practical application of TLC. Thin Layer Chromatography: A Modern Practical Approach offers a sequence of chapters following the steps of the technique as the chromatographer would follow them. The chapters provide a choice of sorbent best suited to the separation intended, followed by pre-treatment required for the sample, applying the sample to the sorbent layer, development procedure, visualisation and detection, and finally quantification. Imaging and hyphenation techniques are described. The reasons why recommendations are made for specific and more general methods are covered. The book also provides an overview of some recent developments in the field. This practical guide is an invaluable introduction to Thin-Layer Chromatography, and will be welcomed by undergraduate students and the practising chromatographer in industry and academia.

Table of Contents

Chapter 1 Introduction and History 1(5)
1 Introduction to Thin-layer Chromatography
1(1)
2 History of TLC
2(2)
3 References
4(2)
Chapter 2 Sorbents and TLC Layers 6(53)
1 Sorbent Selection
6(34)
1.1 Introduction
6(1)
1.2 Silica Based Sorbents
7(28)
1.2.1 Silica Gel
7(5)
1.2.2 Silica Gel Bonded Phases
12(23)
1.3 Non-silica Sorbents
35(5)
1.3.1 Cellulose
35(2)
1.3.2 Cellulose Bonded Phases
37(1)
1.3.3 Aluminium Oxide
37(1)
1.3.4 Kieselguhr
38(1)
1.3.5 Polyamide
39(1)
1.3.6 Miscellaneous Stationary Phases
39(1)
1.3.7 Mixed Stationary Phases
40(1)
1.3.8 Dual Phases
40(1)
2 Preparation of TLC Sheets and Plates
40(37)
2.1 "Home made" TLC Plates
40(1)
2.2 Pre-coated TLC/HPTLC Sheets and Plates
41(1)
3 Cutting TLC/HPTLC Sheets and Plates
41(1)
4 Humidity Effects with TLC Plates
42(1)
5 Pre-washing TLC Plates
43(1)
6 Use of Phosphorescent/Fluorescent Indicators
44(1)
7 Channelled TLC Layers
44(1)
8 Concentration Zone TLC/HPTLC Plates
45(1)
9 HPTLC Pre-coated Plates
45(3)
9.1 HPTLC Spherical Silica Gel 60
48(1)
10 Improving Resolution with Buffers and Complexing Reagents
49(1)
10.1 Impregnation of Sorbent before Layer Coating
49(1)
10.2 Impregnation of the Ready Coated Layer
50(1)
11 Silver Nitrate Impregnation
50(1)
12 Charge Transfer TLC
51(3)
13 Preparative Layer Chromatography (PLC)
54(1)
14 References
55(4)
Chapter 3 Sample Pre-treatment 59(6)
1 Introduction
59(1)
2 Extractions from Solid Samples
60(1)
3 Solid Phase Extraction Systems (SPE)
61(3)
3.1 Diatomaceous Earth
61(1)
3.2 Bonded Silica Gels and Polymers
61(2)
3.3 Sorbent Conditioning
63(1)
3.4 Sample Injection
63(1)
3.5 Cleaning
63(1)
3.6 Recovery of Analytes
63(1)
4 References
64(1)
Chapter 4 Sample Application 65(21)
1 Introduction
65(1)
2 Selecting the Sample Solvent
65(1)
3 Theoretical Determination of Spot Size
66(6)
3.1 Spot Size and Loading Equations
66(2)
3.2 Spot Capacity Equation
68(4)
4 Sample Loading
72(3)
4.1 Layer Damaging Effects
74(1)
4.2 Humidity Considerations
75(1)
5 Sample Application Methods
75(7)
5.1 Manual Methods
76(1)
5.2 Instrumental Methods
77(3)
5.2.1 Manual Instrumental Techniques
77(1)
5.2.2 Automated Techniques
78(2)
5.3 Large Sample Application
80(10)
5.3.1 Contact Spotting
80(1)
5.3.2 Use of Concentration Zone TLC/HPTLC
81(1)
6 Choice of Band or Spot Application
82(3)
7 References
85(1)
Chapter 5 Development Techniques 86(48)
1 Introduction
86(1)
2 The Theory of Solvent Migration
86(4)
3 Mechanisms of TLC Separation
90(2)
3.1 Introduction
90(1)
3.2 Adsorption Separations
90(1)
3.3 Partition Separations
91(1)
3.4 Ion-exchange Separations
91(1)
4 Solvent Selection
92(8)
4.1 Eluotropic Series and Solvent Optimisation
93(7)
4.1.1 Selectivity Triangles
96(3)
4.1.2 PRISMA Model
99(1)
5 Development Chambers
100(12)
5.1 N-Chambers and Chamber Saturation Effects
100(5)
5.2 Twin-trough Chamber
105(1)
5.3 Sandwich, Horizontal and U-chambers
105(3)
5.4 Automatic Developing Chamber (ADC)
108(1)
5.5 Forced-flow Development (OPLC)
109(1)
5.6 Vario Chambers
110(2)
6 Multiple Development Techniques
112(9)
6.1 Single Mobile Phase Multiple and Continuous Development
112(3)
6.2 Two-dimensional Development
115(3)
6.3 Manual Gradient Development
118(1)
6.4 Automated Multiple Development (AMD)
118(3)
7 Mobile Phase Additives
121(11)
7.1 Use of Buffers and pH
121(3)
7.2 Acid or Base Additives
124(1)
7.3 Ion-pairing Reagents
124(2)
7.4 Chiral Additives
126(6)
7.4.1 Cyclodextrins
127(2)
7.4.2 Bovine Serum Albumin (BSA)
129(1)
7.4.3 Other Chiral Selectors
129(3)
7.5 Argentation (Silver Nitrate) TLC
132(1)
8 References
132(2)
Chapter 6 Detection and Visualisation 134(20)
1 Introduction
134(1)
2 Non-destructive Techniques
135(4)
2.1 Visible Detection
135(1)
2.2 Ultra-violet Detection
135(2)
2.3 Reversible Reactions
137(1)
2.3.1 Iodine Vapour
137(1)
2.3.2 Ammonia Vapour
138(1)
2.4 Non-reversible Reactions
138(2)
2.4.1 Fluorescent Dyes
138(1)
2.4.2 pH Indicators
139(1)
3 Destructive Techniques
139(2)
3.1 Charring Reactions
140(1)
3.2 Thermochemical Activation
140(1)
4 Derivatisation Reactions
141(12)
4.1 Post-chromatographic Visualisation
141(10)
4.1.1 Universal Chemical Reagents
143(3)
4.1.2 Group Specific Reagents
146(3)
4.1.3 Sequencing Reactions
149(2)
4.2 Pre-chromatographic Visualisation
151(2)
5 References
153(1)
Chapter 7 Quantification and Video Imaging 154(12)
1 Introduction
154(1)
2 Densitometry
155(5)
2.1 Mode of Operation of Spectrodensitometers
155(3)
2.2 Theory of Spectrodensitometry
158(2)
3 Video Imaging and Densitometry
160(3)
4 Future Trends – Spectrodensitometry or Video Imaging?
163(1)
5 References
164(2)
Chapter 8 TLC Coupling Techniques 166(11)
1 Introduction
166(1)
2 TLC/HPTLC and HPLC
167(1)
3 TLC and MS
167(4)
4 TLC Coupled with FTIR
171(2)
4.1 On-line TLC – FTIR
172(1)
4.2 Off-line TLC – FTIR
172(1)
5 TLC and Raman Spectroscopy
173(1)
6 References
174(3)
Subject Index 177

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