Inorganic Mass Spectrometry

Johanna Sabine Becker; Since 1997- Deputy Head of Central Department for Analytical Chemistry, Research Centre Jülich.

• Foreword xiiiPreface xviiAcknowledgements xixIntroduction to Mass Spectrometry 11 History of Mass Spectrometric Techniques 7References 222 Ion Sources 252.1 Inductively Coupled Plasma Ion Source 282.1.1 Laser Ablation Coupled to an Inductively Coupled Plasma Ion Source 382.1.2 Electrothermal Vaporization Coupled to an Inductively Coupled Plasma Ion Source 432.1.3 Hydride Generation and Cold Vapour Technique Coupled to an Inductively Coupled Plasma Source 432.2 Spark Ion Source 442.3 Laser Ion Source 462.3.1 Laser Plasma Ionization 462.3.2 Resonant Laser Ionization 502.4 Glow Discharge Ion Source 512.5 Thermal Surface Ionization Source 562.6 Ion Sources for Secondary Ion Mass Spectrometry (SIMS) and Sputtered Neutral Mass Spectrometry (SNMS) 602.7 Electron Ionization Source 652.8 Matrix Assisted Laser Desorption/Ionization Source 692.9 Electrospray Ionization Source 70References 733 Ion Separation 773.1 Sector Field Analyzer 783.1.1 Magnetic Sector Field Analyzer 783.1.2 Electric Sector Field Analyzer 813.1.3 Combination of Magnetic and Electric Sector Fields – Double-focusing Sector Field Mass Spectrometer 833.2 Dynamic Mass Separation Systems 873.2.1 Quadrupole Mass Analyzer 873.2.2 Time-of-flight Analyzer 913.2.3 Ion Trap Mass Analyzer 943.2.4 Ion Cyclotron Resonance Mass Analyzer 953.3 Mass Resolution and Abundance Sensitivity 98References 1014 Ion Detection Systems 1034.1 Faraday Cup 1034.2 Secondary Electron Multiplier 1054.3 Combination of Faraday Cup and Secondary Electron Multiplier 1074.4 Channel Electron Multiplier and Microchannel Plates 1084.5 Daly Detector 1094.6 Multiple Ion Collection System 1114.7 Fluorescence Screen and Photographic Ion Detection 113References 1145 Instrumentation 1175.1 Inductively Coupled Plasma Mass Spectrometers (ICP-MS) 1205.1.1 Quadrupole Based ICP Mass Spectrometers (ICP-QMS) 1215.1.2 ICP Mass Spectrometers with Collision or Dynamic Reaction Cell or Collision Reaction Interface 1235.1.3 Double-focusing Sector Field ICP Mass Spectrometers with Single Ion Collector (ICP-SFMS) 1315.1.4 Time-of-flight Mass Spectrometers (ToF-MS) 1335.1.5 Multiple Ion Collector ICP Mass Spectrometers (mc-icp-ms) 1355.1.6 Solution Introduction Systems in ICP-MS 1415.1.7 Hydride Generation and Cold Vapour Technique 1465.1.8 Flow Injection and Hyphenated Techniques 1475.1.9 Laser Ablation Inductively Coupled Plasma Mass Spectrometers (la-icp-ms) 1505.2 Spark Source Mass Spectrometers (SSMS) 1535.3 Laser Ionization Mass Spectrometers (LIMS) 1545.4 Resonance Ionization Mass Spectrometers (RIMS) 1555.5 Glow Discharge Mass Spectrometers (GDMS) 1575.6 Thermal Ionization Mass Spectrometers (TIMS) 1605.7 Secondary Ion Mass Spectrometers (SIMS) and Sputtered Neutral Mass Spectrometers (SNMS) 1615.8 Accelerator Mass Spectrometers (AMS) 1675.9 Electron Ionization Mass Spectrometers for Stable Isotope Ratio Measurements 1695.10 Knudsen Effusion Mass Spectrometers 170References 1716 Analytical and Practical Considerations 1776.1 Qualitative Analysis 1776.1.1 Isotopic Pattern 1786.1.2 Mass Determination 1806.1.3 Interference Problems 1806.2 Quantification Procedures 1876.2.1 Semi-quantitative Analysis 1886.2.2 One Point Calibration in Solid-state Mass Spectrometry Using a Certified Reference Material 1896.2.3 Quantification of Analytical Data via Calibration Curves in Mass Spectrometry Using Certified Reference Materials or Defined Standard Solutions 1936.2.4 Isotope Dilution Technique 1966.2.5 Quantification in Solid-state Mass Spectrometry Using Synthetic Laboratory Standards 1996.2.6 Solution Based Calibration in LA-ICP-MS 2016.3 Sample Preparation and Pretreatment 2086.3.1 Sample Preparation for Analysis of Solids 2096.3.2 Sample Preparation for ICP-MS 2096.3.3 Trace Matrix Separation and Preconcentration Steps 211References 2127 Mass Spectrometric Techniques for Analysis of Gaseous Materials and Volatile Compounds 2157.1 Sampling and Sample Preparation of Gases and Volatile Compounds 2157.2 Applications of Inorganic Mass Spectrometry for Analysis of Gases and Volatile Compounds 2167.3 Stable Isotope Ratio Measurements of Gases and Volatile Compounds 220References 2218 Isotope Ratio Measurements and their Application 2238.1 Capability of Inorganic Mass Spectrometry in Isotope Ratio Measurements 2268.2 Limits for Precision and Accuracy of Isotope Ratio Measurements and How to Solve the Problems 2288.3 Isotope Ratio Measurements by Gas Source Mass Spectrometry 2328.4 Isotope Ratio Measurements by Quadrupole based ICP-MS 2328.5 Isotope Ratio Measurements by Laser Ablation ICP-MS 2348.6 Multiple Ion Collector Mass Spectrometry for High Precision Isotope Ratio Measurements 2378.7 Applications of Isotope Dilution Mass Spectrometry 2398.8 Isotope Ratio Measurement of Long-Lived Radionuclides 2418.9 Applications of Isotope Ratio Measurements in Geochemistry and Geochronology 246References 2509 Fields of Application in Trace, Ultratrace and Surface Analysis 2559.1 Materials Science 2569.1.1 Trace and Ultratrace (Bulk) Analysis of Metals and Alloys 2609.1.2 Semiconductors 2689.1.3 Ceramics, Glasses, Polymers and Other Non-conductors 2729.1.4 Thin and Thick Film Analysis 2779.1.5 Analysis of Surface Contamination and of Process Chemicals Used in Semiconductor Technology 2879.1.6 Microlocal Analysis in Materials Research 2919.1.7 Imaging by Inorganic Mass Spectrometry in Materials Science 292References I 2939.2 Environmental Science and Environmental Control 2989.2.1 Analysis of Water Samples 3009.2.2 Analysis of Air Samples, Particles and Smoke 3049.2.3 Multi-elemental Analysis of Environmental Samples for Environmental Control 3069.2.4 Environmental Monitoring of Selected Elements, Group Elements and Trace Element Species 3069.2.5 Isotope Ratio Measurements in Environmental Samples 3089.2.6 Monitoring of Radionuclides in the Environment 311References II 3139.3 Biology 3179.3.1 Analysis of Trace Elements in Biological Samples 3189.3.2 Elemental Speciation in Biological Samples 3229.3.3 Analysis of Phosphorus, Metals and Metalloids Bonded to Proteins 3269.3.4 Isotope Ratio Measurements of Biological Systems 3319.3.5 Trace and Imaging Analysis on Biological Tissues and Single Cells 333References III 3369.4 Bioengineering 3389.4.1 Activities in Bioengineering and Analytics 3399.4.2 Nanobiotechnology 340References IV 3439.5 Medicine 3449.5.1 Sampling, Sample Handling and Storage of Medical Samples 3449.5.2 Body Fluids 3459.5.3 Hair, Nail, Tooth and Bone Analysis 3499.5.4 Microanalysis of Small Amounts of Medical Samples 3529.5.5 P, S, Se and Metal Determination in Proteins 3539.5.6 Analysis of Tissues 3629.5.7 Imaging Mass Spectrometry of Medical Tissues 3669.5.8 Single Cell Analysis 3729.5.9 Ultrafine Particles and Health 375References V 3759.6 Food Analysis 3809.6.1 Determination of Trace Elements and Species in Foodstuffs 3819.6.2 Analysis of Mineral and Bottled Water 3859.6.3 Fingerprinting of Foods by Trace Analysis and Isotope Ratio Measurements 385References VI 3869.7 Geology and Geochemistry 3889.7.1 Sample Preparation Techniques for Geological Samples 3889.7.2 Fractionation Effects in LA-ICP-MS 3909.7.3 Multi-element Analysis of Geological Samples 3919.7.4 Trace Analysis of Selected Elements in Geological Materials 3969.7.5 Isotope Analysis Including Age Determination of Minerals and Rocks by Mass Spectrometry 3989.7.6 Mass Spectrometric Microlocal and Imaging Analysis of Geological Samples 407References VII 4079.8 Cosmochemistry, Planetary and Space Science 4109.8.1 Cosmochemical Trace Analysis 4109.8.2 Isotope Analysis in Cosmochemistry 4129.8.3 Cosmogenic Radionuclides and Age Dating 413References VIII 4149.9 Determination of Long-lived Radionuclides 4159.9.1 Determination of Half-life of Long-lived Radionuclides 4189.9.2 Methodological Developments and Applications of ICP-MS for Determination of Long-lived Radionuclides Including Trace/Matrix Separation 4199.9.3 Ultratrace Analysis of Long-lived Radionuclides in Very Small Sample Volumes 4249.9.4 Determination of Long-lived Radionuclides by LA-ICP-MS and Etv-icp-ms 4279.9.5 Particle Analysis by Inorganic Mass Spectrometry 430References IX 4319.10 Forensic Analysis 4339.10.1 Fingerprinting in Forensic Studies 4349.10.2 Multi-element Analysis for Forensic Studies 4359.10.3 Trace Element Analysis of Selected Elements and Speciation 4369.10.4 Nuclear Forensic Studies 4379.10.5 Forensic Investigations by Isotope Ratio Measurements 438References X 4399.11 Study of Cluster and Polyatomic Ion Formation by Mass Spectrometry 4409.11.1 Carbon and Boron Nitride Cluster Ion Formation 4419.11.2 Formation of Selected Heteronuclear Cluster Ions 4469.11.3 Clusters From Metal Oxide/Graphite Mixtures 4469.11.4 Argon Diatomic Ions 4509.11.5 Oxide Ion Formation of Long-lived Radionuclides in Icp-ms 453References XI 4559.12 Further Applications 4569.12.1 Pharmaceutical Applications and Analysis of Drugs 4579.12.2 Archaeology 457References XII 45810 Future Developments and Trends in Inorganic Mass Spectrometry 459AppendicesAppendix I 463Appendix II 470Appendix III 473Appendix IV 478Appendix V 481Index 483

"This book fits very well into the curriculum for graduate courses in inorganic analysis and inorganic mass spectrometry … It is a pleasure to recommend this up-to-date and thorough book." (Angewandte Chemie International Edition, May 2008) "A volume that belongs on the shelf of every practicing mass spectrometrist and worthy of consideration for any graduate level course dealing with the subject … .It is far more coherent and cohesive than most other volumes that are merely edited collections of individually written chapters." (International Journal of Mass Spectrometry)"Standing ovations for this book! It is very homogenous, well written, excellently illustrated, and well rounded." (Analytical & Bioanalytical Chemistry, September 2008)This overview would benefit researchers in all of these fields…may provide them with some useful answers would be well advised to secure a copy of this text. (Journal of the American Chemical Society, July 2, 2008)"This book fits very well into the curriculum for graduate courses in inorganic analysis and inorganic mass spectrometry. It will also server as an easy-to-use and extremely valuable source of information for all practitioners in the board field of mass spectrometry. It is a pleasure to recommend this up-to-date and thorough book." (Angewandte Chemie, 2008-47/23)