Thin-Layer Chromatography

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.

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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Thin-Layer Chromatography

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