Intuitively organized textbook aligned to common analytical instrumentation courses for undergraduate students
Through an analytical approach, Essential Methods of Instrumental Analysis provides an expansive overview of common instruments and methods and their applications for undergraduate students, integrating experimental protocols with real result examples to deliver a well-rounded understanding of the inner workings of the instruments and enabling students to evaluate the success of their experiments and create scientific figures.
In addition to detailed coverage of specific instruments, the book discusses analytical laboratory practices, instrument maintenance, statistics, and real-world lab experiments with previous student results. Each analytical method section includes extensive sample preparation information, rather than a simple stand-alone chapter offering generic discussions not connected to specific methods.
This book conveniently organizes content by analyte class (inorganic and organic) in a way that is intuitive to a student and aligned with relevant courses. Ancillaries including .mp4 videos, instructor PowerPoint slides, and animations are included on a companion website.
Written by an experienced professor and tested and refined over years in his courses since 2008, Essential Methods of Instrumental Analysis includes information on sample topics such as:
Proper laboratory protocols for analytical instrumentation, covering chemical reagents, glassware, calibration techniques, and figures of merit Optical physics, covering the interaction of electromagnetic radiation with instrument components and sample molecules, relaxation processes, reflection, diffraction, dispersion, and refraction Flame atomic absorption and flame emission spectrometry, covering optical radiation sources, mirrors, choppers, burner heads, and doppler broadening Gas and liquid chromatography, covering gaseous, liquid, soil-sediment, and biological samples, analyte recovery, chromatography theory, injectors, columns and ovens, common detectors, and mass spectrometers
Focusing on contrasts and comparisons across multiple types of instruments in a way distinct from similar texts, Essential Methods of Instrumental Analysis is an essential textbook for students in advanced undergraduate courses in related programs of study.
About the Authors xv Preface xix About the Companion Website xxi 1 Proper Laboratory Protocols for Analytical Instrumentation 1 1.1 Laboratory Preliminaries 1 1.2 Standard Practices 11 1.3 Questions 13 1.4 Problems 14 2 Statistical Analysis 17 2.1 Introduction 17 2.2 Linear Least-squares Analysis 18 2.3 Student’s t-test Equations 20 2.4 Assignments 24 Further Reading 24 3 A Review of Optical Physics 25 3.1 Introduction 25 3.2 Interaction of Electromagnetic Radiation with Sample Molecules 26 3.3 Interaction of Electromagnetic Radiation with Surfaces 32 3.4 Detectors in UV–visible Spectrometry 41 3.5 Summary 48 Reference 49 3.6 Questions 49 Supporting Information 51 4 Analytical Molecular Spectrometry 53 4.1 Introduction 53 4.2 Basic UV–Vis Spectrometer 53 4.3 From Simple to Complex UV–Visible Spectrometers 54 4.4 Fluorescence and Phosphorescence Instruments 55 4.5 Instrument Maintenance 57 4.6 Summary 57 4.7 Case Study: Quantitation of Riboflavin by UV–Vis and Fluorescence Spectrometry by Nate Boland 60 5 Flame Atomic Absorption and Flame Emission Spectrometry 61 5.1 Introduction and History of Atomic Absorption Spectrometry (AAS) 61 5.2 Components of a Flame Atomic Absorption/Emission Spectrometer System 61 5.3 Specialized Sample Introduction Techniques and Analysis 73 5.4 General Operation of FAAS and FAES Instruments 76 5.5 Maintenance 76 5.6 Summary 76 5.7 Questions 77 Supporting Information 78 6 Inductively Coupled Plasma 79 6.1 Introduction and History 79 6.2 Atomic Emission Spectrometry Theory 79 6.3 Components of an Inductively Coupled Plasma: Atomic Emission Spectrometry System (ICP–AES) 80 6.4 Interferences 90 6.5 Maintenance 90 6.6 Case Study: Quantitation of Heavy Metals in Consumer Products by Dan Burgard 90 6.7 Summary 91 6.8 Questions 92 Supporting Information 92 References 93 7 Inductively Coupled Plasma–Mass Spectrometry 95 7.1 Introduction and History 95 7.2 Components of a Mass Spectrometer 95 7.3 Summary 112 7.4 Questions 113 Supporting Information 115 Reference 115 Further Reading 115 8 Contrasts and Comparisons of Instrumentation 117 8.1 Introduction 117 8.2 Figures of Merit 117 8.3 Questions 120 9 Chromatography Introduction, Chromatography Theory, and Instrument Calibration 121 9.1 Introduction 121 9.2 Chromatographic Theory 122 9.3 Case Study 129 9.4 Optimization of Chromatographic Conditions 131 9.5 Calibration of an Instrument/Detector 133 9.6 Evolution of Peak Integration 135 Supporting Information 136 References 136 10 Gas Chromatography 137 10.1 Introduction and History 137 10.2 Types of Samples and Sample Introduction 137 10.3 Gas Chromatography 143 10.4 Advanced GC Systems 152 10.5 Applications/Case Studies 152 10.6 Summary 160 10.7 Questions 161 Supporting Information 162 Reference 162 11 High-performance Liquid Chromatography 163 11.1 Introduction and History 163 11.2 Types of Analytes, Samples, and Sample Introduction 165 11.3 Liquid Chromatography 166 11.4 Advanced and Specialty LC Systems 173 11.5 Applications/Case Studies 177 11.6 Summary 180 11.7 Questions 180 Supporting Information 182 References 182 12 Capillary Electrophoresis by Nicole James 185 12.1 Introduction 185 12.2 Electrophoresis and Capillary Electrophoresis 185 12.3 Samples 190 12.4 Methods of Operation 192 12.5 Detectors 195 12.6 Application/Case Studies 199 12.7 Summary 202 References 202 13 Mass Spectrometry 203 13.1 Introduction and History 203 13.2 Sample Introduction from GC and Analyte Ionization 204 13.3 Introduction of Samples from HPLC 210 13.4 Introduction of Samples from a Capillary Electrophoresis System 214 13.5 Common Mass Filters (Mass Analyzers) 216 13.6 Ion Detectors 238 13.7 Three-dimensional Aspects of GC–MS 239 13.8 Summary 239 13.9 Questions 240 Supporting Information 242 References 242 Further Reading 242 14 Fragmentation and Interpretation of Spectra 245 14.1 Introduction 245 14.2 Creation of the Spectra 246 14.3 Identifying the Molecular Ion Peak 247 14.4 Use of the Molecular Ion 249 14.5 Identification of Analytes Using Isotopic Ratios 252 14.6 Fragmentation 255 14.7 Rearrangements 257 14.8 Identification of Compounds 257 14.9 Fragmentation of Hydrocarbons 258 14.10 Fragmentation of Alcohols 262 14.11 Fragmentation of Ketones and Aldehydes 265 14.12 Fragmentation of Carboxylic Acids 270 14.13 Fragmentation of Ethers 271 14.14 Fragmentation of Esters 273 14.15 Fragmentation of Amines 276 14.16 Fractionation of Amides 278 14.17 Fragmentation of Nitriles 279 14.18 Reviewing General Principles 280 14.19 Searchable Databases 284 15 Common Radiochemical Detection Methods in Analytical Chemistry 285 15.1 Introduction 285 15.2 Common Sources of Radiation 285 15.3 Detection of Alpha, Beta, and Gamma Emission 286 15.4 Case Studies 290 Reference 290 16 Instrumental Laboratory Experiments with Results 291 16.1 Introduction 291 16.2 A Typical Glassware Inventory for an Instrumental Methods Course 291 16.3 Maintaining a Legally Defensible Laboratory Notebook 291 16.4 Solutions, Weights, and Laboratory Techniques 293 16.5 Determination of a Surrogate Toxic Metal (Ca) in a Simulated Hazardous Waste Sample by a Variety of Techniques 295 16.6 Identification of Components in Liquors and Distilled Spirits 306 16.7 Identification of Fragrances 311 16.8 GC–MS Analysis of Synthetic and Natural Fragrances by Evan Bowman, Annika Mayo, and Aurora Anderson 316 16.9 SPME–GC–MS Analysis of Wine Headspace by Bailey Arend 324 16.10 Quantitative Determination of the Presence of Captan on Organic and Nonorganic Strawberries by Peter Mullin, Eric Ying, Jon Na, Sharon Ndayambaje, and Soren Sandeno 330 16.11 Determination of Nicotine in Human Urine Using HPLC–MS by Ashley Nguyen, Lea Molacek, Maxwell Brown 333 16.12 Analysis of Caffeine in Urine Samples Using GC–FID by Elsa Nader, Ralph Huang, Aaron Lieberman, Jane Duncan, and Matt Sousa 336 16.13 Caffeine in the Walla Walla (WA) Wastewater Effluent by MacKenzie Cummings, Mia Groff, Roya Nasseri, Noah Willis, and Clara Wheeler 338 16.14 Gasoline Analysis by GC–FID and GC–MS by Theodore Pierce and Austin Shaff 340 16.15 GC–MS as an Effective Instrument for Detecting Cocaine on US Currency by Jessica Boyers and Kacey Godwin 343 16.16 Analytical Quantification of CBD-A Content in Cannabis sativa (Hemp) Using GC–FID and GC–MS by Lauren Yumibe, Sam Weiss, Maddie Bowers, Tori Li, Asher Bachtold, and Brandon Neifert 347 16.17 Results and Discussion 349 16.18 Conclusions 350 References 351 Further Reading 354 Index 357
Frank M. Dunnivant, PhD is a Professor in the Department of Chemistry at Whitman College. He has worked for several labs including the Oak Ridge National Laboratory, the Idaho National Engineering Laboratory, and the University of Zurich (ETH) and the Swiss Federal Institute for Water and Waste Water Pollution (EAWAG). Jake W. Ginsbach, PhD is a Principal Consultant at Kaiser Permanente. At Stanford and Whitman College, his research included lab analyses of environmental chemicals and contaminants, studying the activation of dioxygen at copper active sites in metalloenzymes, along with helping develop two e-textbooks.
