INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY

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1 INDUCTIVELY COUPLED PLASMA MASS SPECTROMETRY Edited by AKBAR MONTASER George Washington University Washington, D.C , USA WILEY-VCH New York Chichester Weinheim Brisbane Singapore Toronto

2 CONTENTS Foreword, xix Preface, xxv Acknowledgments, xxix 1 An Introduction to ICP Spectrometries for Elemental Analysis, Formation, Operation, and Characteristics of the ICP Discharge, An Overview of ICP Spectrometries, Analytical Figures of Merit for ICPAES Spectrometers, Analytical Figures of Merit for ICPMS Spectrometers, 16 Acknowledgments, 28 References, 28 2 The Art and Science of Microwave Sample Preparations for Trace and Ultratrace Elemental Analysis, Introduction, Absorption of Microwave Energy and Heating, Laboratory Microwave Design, Microwave Closed Vessel Digestion, Atmospheric-Pressure Digestion, 41 ix

3 X CONTENTS Microwave Autoclave Digestion, Flow-Through Microwave Digestion, Microwave Reaction Control, Stepwise Development of Microwave Dissolution Procedures, Data Quality Objectives, The Matrix, TheAnalyte, Reaction Properties Defined by the Matrix, Analyte, and Reagents Selected, Methodology and Instrumentation, Acid Chemistry, Introduction to the Primary Dissolution Reagents, Reactions with Nitric Acid, Reactions with Hydrochloric Acid, Reactions with Hydrofluoric Acid, Reactions with Sulfuric Acid, Reactions with Perchloric Acid, Reactions with Hydrogen Peroxide, Dissolution Parameters, Overview of Matrix Digestion Chemistry, Standard Microwave Methods, Microwave Dissolution of Organic Matrices, Microwave Dissolution of Inorganic Matrices, Environmental Applications of Microwave Digestion, Generic Digestion Protocol: The EPA Total Digestion Method 3052, Total Microwave Processing, Achieving Trace and Ultratrace Analysis Through Clean Chemistry and Microwave Dissolution, Microwave Sample Decomposition Safety, Conclusions and Future Trends, 76 References, 78

4 CONTENTS XI 3 Sample Introduction in ICPMS, Introduction, Gaseous Sample Introduction, Hydride Generation Methods, Direct Gaseous Sample Introduction, The Chromatographie Methods, Gaseous Sample Introduction: Conclusions and Future Developments, Liquid Sample Introduction, Common Pneumatic Nebulizers, Ultrasonic Nebulizers, Thermospray Nebulizers, Low Sample Consumption Nebulizers, Discrete Sample Introduction Devices, The Monodisperse Dried Microparticulate Injector, Spray Chambers and Desolvation Systems, Aerosol Desolvation Devices, Liquid Sample Introduction: Conclusions and Future Developments, Solid Sample Introduction, Direct Sample Insertion, Electrothermal Vaporization, Are and Spark Ablation, Laser Ablation, Slurry Nebulization, Other Techniques, Solid Sample Introduction: Conclusions and Future Developments, 221 Acknowledgments, 224 References, 224

5 xii CONTENTS 4 Plasma Generation in ICPMS, Introduction, Nature of the ICP, Historical Background, Types of ICP Generators, The Plasma System Building Blocks, The Oscillator, The Small-Signal Amplifiers, The Power Amplifier, Solid-State Versus Electron Tube Devices, Water-Cooled Versus Air-Cooled Devices, System Requirements, Free-Running Oscillator, Crystal-Controlled Generator, Types of Crystal-Controlled Generators, Solid-State and Electron Tube Generators, Solid-State RF Generators, Computerization and the Plasma System, Impedance Matching Network, Plasma Impedance, The Secondary RF Discharge, Induction Coils, Effect of Frequency, Power Stability, Power Measurements, Electromagnetic Interference, Torches, Conventional and New Models, Gas Flow Systems for Plasma Torches, The Future, 324

6 CONTENTS xiii Acknowledgments, 325 References, Fundamental Aspects of Sample Introduction in ICP Spectrometry, Introduction, Noise and Precision, Key Parameters in Droplet Size Characterization, Droplet Size Distribution and Mean Diameters, Span of a Droplet Size Distribution, Volume Flux of Droplets, Droplet Number Density, Droplet Mean Velocity and Droplet Time of Arrival, Measurement of Droplet Size Distributions, Mechanical Methods, Electrical Methods, Optical Methods, Parameters Influencing the Aerosol Droplet Distribution, Aerosol Ionic Redistribution, Droplet Collisions, Droplet Evaporation, Solvent Load, Analyte Transport Efficiency, Mass Transport Rate, and Acid Effects, Definitions, Measurement Methods, Typical Values of Transport Properties, Acid Effects and Transport Parameters, Typical Droplet Sizes with Various Nebulizers and Gases, Droplet Sizes with Various Nebulizers, Nebulization of Solutions by Different Gases, 397

7 xiv CONTENTS 5.8 Modeling of Nebulizer Systems, Key Parameters in Modeling Nebulizer Systems, Models for Common Nebulizer Systems, Models for Spray Chambers, Models for Nebulizer Systems, Conclusions and Future Directions, 407 Acknowledgments, 408 References, Instrumentation for Low- and High-Resolution ICPMS, Introduction, The ICPMS Interface and Ion Sampling, The Skimmer Aperture as an Ion Source and Transfer Optics, Vacuum Systems, Pumping Systems, Pressure Gauges, The Mass Analyzer, The Radiofrequency Quadrupole Mass Spectrometer, Basic Concepts of High-Resolution ICPMS, Other Mass Analyzers, Detection Systems, Ion Counting, Analogue Collection, Dual Detection Systems, Performance of Low-Resolution and High-Resolution ICP Mass Spectrometers, Interferences in High-Resolution ICPMS, Detection Limits with High-Resolution ICPMS, Isotope Ratio Measurement with High-Resolution ICPMS, Current Limitations and Future Directions, 490

8 CONTENTS xv Acknowledgments, 491 References, Analytical Characteristics of ICPMS, Introduction, Signal Dependence on Instrumental Parameters, ICP Parameters, Interface Parameters, Ion Lens Voltage Settings, Spectral Characteristics of ICPMS, Interelement (Isobaric) Spectral Overlaps, Basic Background Species, Molecular Species Derived from the Sample Matrix, Oxide and Hydroxide Species: Some General Observations and Comments, Control and Manipulation of Spectral Features, Matrix Effects in ICPMS, Quantitative Analysis Using ICPMS, Semiquantitative Analysis, Assessment of Potential Spectral Overlaps, Assessment of Potential Matrix Effects, Internal Standardization and Isotope Dilution, Noise Characteristics of ICPMS Signals, Basic Noise Characteristics, Considerations in Measurements of Precision and Isotope Ratio, Conclusions and Future Directions, 563 Acknowledgments, 564 References, 564 Appendix 7.1 Mass Spectra of Elements, 589 Appendix 7.2 MS InterView and Exercises, 612

9 xvi CONTENTS 8 Fundamental Considerations in ICPMS, Introduction, Properties of the ICP as an Ion Source, Use of Equilibria as a First Approximation for Order-of- Magnitude Estimates, Singly Charged Ions, Doubly Charged Ions, Molecular Ions, Mass Spectrometry Under "Cold Plasma" Conditions, Sampling Ions from the ICP, Introduction to Kinetics of Gases and Plasmas, Flow Properties Upstream of the Sampler, Flow Properties Downstream of the Sampler, The Skimming Process, Ion Kinetic Energies, Deviations from Ideal Behavior, Space Charge Effects, Future Directions, Alternate Mass Analyzers, Speciation, Alternate Ionization Sources, 668 Acknowledgment, 669 References, Novel Applications of ICPMS, Introduction, Types of Analysis, Semiquantitative Analysis, Quantitative Analysis, Analysis of Solid Samples, Chromatographie Speciation Analysis, 709

10 CONTENTS xvii Isotopic Analysis, Applications, Biological Applications, Geological Applications, Environmental Applications, Industrial Applications, Applications in the Semiconductor Industry, Forensic Applications, Applications Using High-Resolution ICPMS, Multicomponent Analysis for Rapid Automated Survey of ICPMS Spectra, Conclusions and Future Directions, 769 Acknowledgments, 770 References, Mass Spectrometry with Mixed-Gas and Helium ICPs, Introduction, Benents and Limitations of ICPMS Operated with Argon Versus Alternative Gases, Instrumentation for Alternative ICP Discharges, Torches, RF Generators, Impedance Matching Networks, and Load Coil Configurations, The MS Interface, The Sample Introduction Systems, Fundamental Properties of Alternative ICP Discharges, Fundamental Parameters of Mixed-Gas Plasmas at Atmospheric Pressure, Fundamental Parameters of Helium ICP Discharges at Atmospheric Pressure, Fundamental Parameters of Low-Pressure ICP Discharges, Analytical Characteristics of Alternative ICP Discharges, 854

11 xviii CONTENTS Mixed-Gas ICP Discharges, Helium ICP Discharges, Low-Pressure ICP Discharges, Conclusions and Future Directions, 874 Acknowledgments, 875 References, Mass Spectrometry with Microwave-Induced Plasmas, Introduction, Instrumentation, Fundamental Properties of Microwave Plasmas, Analytical Characteristics, Helium MIP Discharges, Nitrogen MIP Discharges, Reduced-Pressure MIP Discharges, Soft lonization with Microwave-Based Plasmas, Conclusions and Future Directions, 932 Acknowledgments, 932 References, 933 Index, 941

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