Practical Inductively Coupled Plasma

The book provides an up-to-date account of inductively coupled plasmas and their use in atomic emission spectroscopy and mass spectrometry. Specific applications of the use of these techniques are highlighted including applications in environmental, food and industrial analysis. It is written in a distance learning / open learning style; suitable for self study applications. It contains contain self-assessment and discussion questions, worked examples and case studies that allow the reader to test their understanding of the presented material.

John R. Dean took his first degree in Chemistry at UMIST, followed by an M.Sc. in Analytical Chemistry and Instrumentation at Loughborough University of Technology and finally a Ph.D. and D.I.C. in Physical Chemistry at Imperial College. He then spent 2 years as a postdoctoral research fellow at the Food Science Laboratory of the Ministry of Agriculture, Fisheries and Food in Norwich in conjunction with Polytechnic South West in Plymouth. The work was focused on the development of directly coupled high performance liquid chromatography inductively coupled plasma mass spectrometry methods for trace element speciation in foodstuffs. This was followed by a temporary lectureship in Inorganic Chemistry at Huddersfield Polytechnic. In 1988 he was appointed to a lectureship in Inorganic/Analytical Chemistry at Newcastle Polytechnic (now Northumbria University). This was followed by promotion to Senior Lecturer (1990), Reader (1994) and Principal Lecturer (1998). In 1998 he was awarded a D.Sc. (London) in Analytical and Environmental Science and was the recipient of the 23rd SAC Silver Medal in 1995. He has published extensively in analytical and environmental science. He is an active member of the Royal Society of Chemistry Analytical Division having served as a member of the atomic spectroscopy group for 15 years (10 as honorary secretary) as well as a past chairman (1997-99). He has served on Analytical Division council for three terms and is currently its vice-president (2002-04) as well as chairman of the North East Region (2001-03).

Series Preface

xi

Preface

xiii

Acknowledgements

xvii

Acronyms, Abbreviations and Symbols

xix

About the Author

xiii

Methodology for Trace Elemental Analysis

1

(16)

Introduction

1

(2)

Analytical Terms and their Definitions

3

(5)

Units

8

(1)

Calibration Strategies

8

(2)

Presentation of Data: Tables

10

(1)

Presentation of Data: Graphs

11

(2)

Calculations: Dilution Factors

13

(1)

Quality Assurance and the Use of Certified Reference Materials

13

(4)

Sample Preparation for Inductively Coupled Plasma Spectroscopy

17

(22)

Introduction

18

(1)

Aqueous Samples

18

(4)

Liquid--Liquid Extraction

18

(2)

Ion-Exchange

20

(2)

Co-Precipitation

22

(1)

Solid Samples

22

(7)

Decomposition Techniques

22

(2)

Microwave Digestion

24

(4)

Dry Ashing

28

(1)

Fusion

29

(1)

Extraction Procedures

29

(10)

Single Extraction Procedures

31

(2)

Sequential Extraction Procedures

33

(3)

Enzymatic Digestion Procedures

36

(2)

References

38

(1)

Sample Introduction Procedures for Inductively Coupled Plasmas

39

(18)

Introduction

39

(1)

Nebulizers

40

(4)

Spray Chambers and Desolvation Systems

44

(3)

Discrete Sample Introduction

47

(5)

Continuous Sample Introduction

52

(2)

Hydride and Cold Vapour Techniques

54

(3)

References

56

(1)

The Inductively Coupled Plasma and Other Sources

57

(8)

Introduction

57

(1)

Inductively Coupled Plasma

58

(3)

Direct-Current Plasma

61

(1)

Microwave-Induced Plasma

62

(1)

Glow Discharge

63

(2)

References

64

(1)

Inductively Coupled Plasma--Atomic Emission Spectroscopy

65

(24)

Fundamentals of Spectroscopy

66

(6)

Origins of Atomic Spectra

67

(2)

Spectral Line Intensity

69

(1)

Spectral Line Broadening

70

(2)

Plasma Spectroscopy

72

(3)

Spectrometers

75

(7)

Sequential

77

(1)

Simultaneous

77

(5)

Detectors

82

(3)

Photomultiplier Tube

82

(2)

Charge-Transfer Devices

84

(1)

Interferences

85

(4)

References

87

(2)

Inductively Coupled Plasma-Mass Spectrometry

89

(34)

Fundamentals of Mass Spectrometry

90

(2)

Atomic Structure

90

(1)

Terminology

91

(1)

Inorganic Mass Spectrometry

92

(2)

Ion Source: ICP

94

(1)

Interface

94

(2)

Mass Spectrometer

96

(6)

Quadrupole Mass Spectrometer

96

(2)

Sector-Field Mass Spectrometer

98

(2)

Ion-Trap Mass Spectrometer

100

(1)

Time-of-Flight Mass Spectrometer

101

(1)

Detectors

102

(2)

Interferences

104

(10)

Isobaric Interferences

105

(1)

Molecular Interferences

105

(4)

Remedies for Molecular Interferences

109

(4)

Non-Spectral Interferences: Matrix-Induced

113

(1)

Isotope Dilution Analysis

114

(3)

Mass Spectral Interpretation

117

(6)

References

122

(1)

Selected Applications of Inductively Coupled Plasma Technology

123

(26)

Forensic Science: Document Analysis

124

(3)

Industrial Analysis: Coal

127

(3)

Clinical/Biological Analysis: Whole Blood and Urine

130

(4)

Materials Analysis: Gadolinium Oxide

134

(2)

Environmental Analysis: Soil

136

(5)

Food Analysis: Milk Products

141

(5)

Pharmaceutical Analysis

146

(3)

References

146

(3)

Further Information: Recording of Data and Selected Resources

149

(14)

Recording of Information in the Laboratory

149

(6)

Introduction

149

(2)

Examples of Data Sheets

151

(4)

Selected Resources

155

(8)

Keeping `Up-to-Date'

155

(1)

Basic Understanding of Inductively Coupled Plasma Spectroscopy (and Related Issues)

155

(8)

Responses to Self-Assessment Questions

163

(10)

SI Units and Physical Constants

173

(4)

Periodic Table

177

(2)

Index

179

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Practical Inductively Coupled Plasma Spectroscopy

Summary

Author Biography

Table of Contents

Supplemental Materials