A Practical Guide to Graphite Furnace Atomic

Jacket Design/Illustration: Keithley & Associates Inc.

DAVID J. BUTCHER, PhD, is Associate Professor of Chemistry at Western Carolina University, Cullowhee, North Carolina.<br> <br> SNEDDON, PhD, is Professor of Chemistry at McNeese State University, Lake Charles, Louisiana.

Preface

ix

(2)

Acknowledgments

xi

(2)

Cumulative Listing of Volumes in Series

xiii

CHAPTER 1 INTRODUCTION

1

(2)

CHAPTER 2 THEORY

3

(28)

2.1 Spectroscopy

3

(1)

2.2 Introduction to Atomic Spectroscopy

4

(2)

2.3 Quantitative Considerations of Transitions

6

(2)

2.3.1 Population of Atoms in a State: The Boltzmann Distribution

6

(1)

2.3.2 Einstein Coefficients

7

(1)

2.4 Electronic States of Atoms

8

(4)

2.4.1 Quantum Numbers for Electrons

9

(1)

2.4.2 Coupling Schemes, Term Symbols, and Selection Rules

10

(1)

2.4.3 Atomic Spectra

11

(1)

2.5 Measures of Transition Strengths: Transition Probabilities and Oscillator Strengths

12

(1)

2.6 Spectral Profiles of Absorption Lines

13

(2)

2.7 GFAAS Analytical Signal: Absorbance

15

(2)

2.8 Intensity of Absorbance in Terms of Fundamental Parameters

17

(2)

2.9 Nature of the Transient GFAAS Signal: Mechanism of Atom Formation in a Graphite Furnace

19

(7)

2.9.1 Surface Processes

20

(1)

2.9.2 Heterogeneous Solid-Gas Interactions

21

(2)

2.9.3 Gas-Phase Chemistry

23

(1)

2.9.4 Processes by Which Analyte Is Lost from the Tube

24

(1)

2.9.5 Monte Carlo Simulations of Atomization Processes

25

(1)

References

26

(5)

CHAPTER 3 QUANTITATIVE GFAAS: CALIBRATION

31

(8)

3.1 General Analytical Methodology

31

(1)

3.2 Calibration Graphs

32

(3)

3.3 Method of Standard Additions

35

(1)

3.4 Method of Internal Standardization

36

(1)

3.5 Absolute Analysis

37

(1)

References

38

(1)

CHAPTER 4 INSTRUMENTATION

39

(66)

4.1 Light Sources

39

(6)

4.1.1 Hollow Cathode Lamps

40

(3)

4.1.2 Electrodeless Discharge Lamps

43

(1)

4.1.3 Xenon Arc Lamps

43

(1)

4.1.4 Semiconductor Diode Lasers

44

(1)

4.2 Graphite Furnace

45

(12)

4.2.1 Graphite Tube Material and Design

46

(3)

4.2.2 Furnace Heating Cycle

49

(5)

4.2.3 Methods of Atomization

54

(3)

4.3 Wavelength Selectors

57

(3)

4.3.1 Monochromators

59

(1)

4.3.2 Echelle Monochromators

60

(1)

4.4 Detectors

60

(2)

4.5 Signal Processing, Readout, and Instrument Control

62

(2)

4.6 Background Correction

64

(26)

4.6.1 Nearby Line (Two-Line) Method

64

(2)

4.6.2 Continuum Source Method

66

(3)

4.6.3 Self-Reversal (Smith-Hieftje) Method

69

(4)

4.6.4 Zeeman Effect Method

73

(11)

4.6.4.1 Inverse Longitudinal ac Zeeman

77

(6)

4.6.4.2 Inverse Transverse ac Zeeman

83

(1)

4.6.4.3 Inverse Transverse dc Zeeman

84

(1)

4.6.5 Comparison of Background Correction Systems

84

(6)

4.7 Graphite Furnace Atomic Emission Spectrometry

90

(2)

4.8 Spectrometer Designs

92

(7)

4.8.1 Single-Element Instruments

93

(1)

4.8.2 Multielement Instruments

94

(5)

References

99

(6)

CHAPTER 5 INTERFERENCE-FREE ANALYSIS

105

(14)

5.1 Spectral Interferences

105

(8)

5.1.1 Spectral Overlaps

105

(2)

5.1.2 Background Attenuation

107

(6)

5.2 Chemical Interferences

113

(3)

5.3 Physical Interferences

116

(1)

References

117

(2)

CHAPTER 6 SAMPLE PREPARATION AND INTRODUCTION

119

(56)

6.1 Liquids

119

(3)

6.2 Gases

122

(3)

6.3 Solids

125

(18)

6.3.1 Wet Decomposition

125

(8)

6.3.2 Combustion

133

(1)

6.3.3 Fusion

133

(1)

6.3.4 Summary of Digestion Procedures

134

(1)

6.3.5 Solids Analysis with Slurry Sampling

134

(5)

6.3.6 Direct Solid Sampling

139

(3)

6.3.7 Laser Ablation

142

(1)

6.4 Preconcentration/Separation Methods

143

(18)

6.4.1 Extraction

144

(2)

6.4.2 Chromatography

146

(3)

6.4.3 Flow Injection Analysis

149

(10)

6.4.4 Other Preconcentration/Separation Methods

159

(2)

6.5 Metal Speciation

161

(5)

References

166

(9)

CHAPTER 7 PRACTICAL HINTS ON THE DETERMINATION OF ELEMENTS BY GFAAS

175

(22)

7.1 Applicability

175

(1)

7.2 Sampling, Sample Storage, and Sample Preparation

176

(7)

7.3 Quality Control Procedures

183

(2)

7.4 Development of GFAAS Methods

185

(3)

7.5 Troubleshooting

188

(7)

References

195

(2)

CHAPTER 8 COMMERCIAL GFAAS INSTRUMENTATION: TYPES, COSTS, AND TRAINING

197

(6)

8.1 Types and Costs of GFAAS Instrumentation

197

(3)

8.2 Consumables

200

(1)

8.3 Service and Maintenance

200

(1)

8.4 Training

201

(2)

CHAPTER 9 FUTURE OF GFAAS

203

(2)

APPENDIX A HISTORICAL BACKGROUND

205

(4)

A.1 Early Work in Atomic Spectroscopy (Before 1955)

205

(1)

A.2 Flame Atomic Absorption Spectrometry

205

(1)

A.3 Graphite Furnace Atomic Absorption Spectrometry

205

(2)

References

207

(2)

APPENDIX B GFAAS LITERATURE

209

(6)

B.1 Books

209

(1)

B.2 Periodicals

210

(1)

B.3 Reviews

210

(1)

B.4 Internet Resources

211

(1)

B.5 Applications of GFAAS

211

(1)

References

212

(3)

APPENDIX C CONDITIONS FOR GFAAS

215

(12)

APPENDIX D GLOSSARY

227

(14)

Index

241

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A Practical Guide to Graphite Furnace Atomic Absorption Spectrometry

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