Overview

A comprehensive study of analytical chemistry providing the basics of analytical chemistry and introductions to the laboratory Covers the basics of a chemistry lab including lab safety, glassware, and common instrumentation  Covers fundamentals of analytical techniques such as wet chemistry, instrumental analyses, spectroscopy, chromatography, FTIR, NMR, XRF, XRD, HPLC, GC-MS, Capillary Electrophoresis, and proteomics Includes ChemTech an interactive program that contains lesson exercises, useful calculators and an interactive periodic table Details Laboratory Information Management System a program used to log in samples, input data, search samples, approve samples, and print reports and certificates of analysis

Full Product Details

Author:   BM Ham ,  Aihui MaHam
Publisher:   John Wiley & Sons Inc
Imprint:   John Wiley & Sons Inc
Dimensions:   Width: 21.70cm , Height: 4.00cm , Length: 30.80cm
Weight:   1.756kg
ISBN:  

9781118714843

ISBN 10:   1118714849
Pages:   688
Publication Date:   26 October 2015
Audience:   Professional and scholarly ,  Professional & Vocational
Replaced By:   9781119894452
Format:   Hardback
Publisher's Status:   Active
Availability:   Available To Order  
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Table of Contents

Preface xxiii Author Biographies xxv Acknowledgments xxvii 1 Chemist and Technician in the Analytical Laboratory 1 1.1 Introduction—The Analytical Chemist and Technician 1 1.2 Today’s Laboratory Chemist and Technician 1 1.3 ChemTech—The Chemist and Technician Toolkit Companion 1 1.4 Chapter Layout 2 1.5 Users of ChemTech 6 2 Introduction to the Analytical Laboratory 7 2.1 Introduction to the Laboratory 7 2.2 Laboratory Glassware 7 2.3 Conclusion 18 3 Laboratory Safety 19 3.1 Introduction 19 3.2 Proper Personal Protection and Appropriate Attire 19 3.3 Proper Shoes and Pants 20 3.4 Laboratory Gloves 20 3.5 General Rules to Use Gloves 22 3.6 Material Safety Data Sheet (MSDS) 22 3.7 Emergency Eye Wash and Face Wash Stations 23 3.8 Emergency Safety Showers 24 3.9 Fire Extinguishers 24 3.10 Clothing Fire in the Laboratory 25 3.11 Spill Cleanup Kits 25 3.12 Chemicals and Solvents 27 3.13 First Aid Kits 27 3.14 Gasses and Cylinders 29 3.15 Sharps Containers and Broken Glass Boxes 29 3.16 Occupational Safety and Health Administration (OSHA) 29 4 Basic Mathematics in the Laboratory 83 4.1 Introduction to Basic Math 83 4.2 Units and Metric System 83 4.3 Significant Figures 84 4.4 Scientific Calculators 86 4.5 ChemTech Conversion Tool 89 4.6 Chapter Key Concepts 89 4.7 Chapter Problems 92 5 Analytical Data Treatment (Statistics) 93 5.1 Errors in the Laboratory 93 5.2 Expressing Absolute and Relative Errors 94 5.3 Precision 94 5.4 The Normal Distribution Curve 94 5.5 Precision of Experimental Data 96 5.6 Normal Distribution Curve of a Sample 97 5.7 ChemTech Statistical Calculations 98 5.8 Student’s Distribution t Test for Confidence Limits 101 5.9 Tests of Significance 104 5.10 Treatment of Data Outliers 105 5.11 Chapter Key Concepts 106 5.12 Chapter Problems 107 6 Plotting and Graphing 109 6.1 Introduction to Graphing 109 6.2 Graph Construction 109 6.3 Rectangular Cartesian Coordinate System 110 6.4 Curve Fitting 110 6.5 Redrawn Graph Example 110 6.6 Graphs of Equations 111 6.7 Least-Squares Method 114 6.8 Computer-Generated Curves 115 6.9 Calculating Concentrations 119 6.10 Nonlinear Curve Fitting 119 6.11 Chapter Key Concepts 123 6.12 Chapter Problems 124 7 Using Microsoft Excel® in the Laboratory 125 7.1 Introduction to Excel® 125 7.2 Opening Excel® in ChemTech 125 7.3 The Excel® Spreadsheet 125 7.4 Graphing in Excel® 127 7.5 Charts in Excel® 2010 132 7.6 Complex Charting in Excel® 97-2003 132 7.7 Complex Charting in Excel® 2010 139 7.8 Statistical Analysis Using Excel® 141 8 Making Laboratory Solutions 147 8.1 Introduction 147 8.2 Laboratory Reagent Fundamentals 147 8.3 The Periodic Table 147 8.4 Calculating Formula Weights 148 8.5 Calculating the Mole 148 8.6 Molecular Weight Calculator 148 8.7 Expressing Concentration 148 8.8 The Parts per (PP) Notation 153 8.9 Computer-Based Solution Calculations 153 8.10 Reactions in Solution 157 8.11 Chapter Key Concepts 157 8.12 Chapter Problems 158 9 Acid–Base Theory and Buffer Solutions 159 9.1 Introduction 159 9.2 Acids and Bases in Everyday Life 159 9.3 The Litmus Test 159 9.4 Early Acid–Base Descriptions 160 9.5 Brǿnsted–Lowry Definition 160 9.6 The Equilibrium Constant 161 9.7 The Acid Ionization Constant 161 9.8 Calculating the Hydrogen Ion Concentration 162 9.9 The Base Ionization Constant 163 9.10 Ion Product for Water 164 9.11 The Solubility Product Constant (Ksp) 164 9.12 The pH of a Solution 166 9.13 Measuring the pH 167 9.14 Buffered Solutions—Description and Preparing 168 9.15 ChemTech Buffer Solution Calculator 170 9.16 Chapter Key Concepts 171 9.17 Chapter Problems 172 10 Titration—A Volumetric Method of Analysis 175 10.1 Introduction 175 10.2 Reacting Ratios 175 10.3 The Equivalence Point 176 10.4 Useful Relationships for Calculations 176 10.5 Deriving the Titration Equation 176 10.6 Titrations in ChemTech 177 10.7 Acid/Base Titration Endpoint (Equivalence Point) 178 10.8 Acid/Base Titration Midpoint 179 10.9 Acid/Base Titration Indicators 180 10.10 Titrations Using Normal Solutions 181 10.11 Polyprotic Acid Titration 181 10.12 ChemTech Calculation of Normal Titrations 182 10.13 Performing a Titration 183 10.14 Primary Standards 184 10.15 Standardization of Sodium Hydroxide 185 10.16 Conductometric Titrations (Nonaqueous Solutions) 186 10.17 Precipitation Titration (Mohr Method for Halides) 188 10.18 Complex Formation with Back Titration (Volhard Method for Anions) 189 10.19 Complex Formation Titration with EDTA for Cations 190 10.20 Chapter Key Concepts 194 10.21 Chapter Problems 195 11 Oxidation–Reduction (Redox) Reactions 197 11.1 Introduction 197 11.2 Oxidation and Reduction 197 11.3 The Volt 198 11.4 The Electrochemical Cell 198 11.5 Redox Reaction Conventions 198 11.6 The Nernst Equation 200 11.7 Determining Redox Titration Endpoints 202 11.8 Potentiometric Titrations 202 11.9 Visual Indicators Used in Redox Titrations 204 11.10 Pretitration Oxidation–Reduction 205 11.11 Ion-Selective Electrodes 206 11.12 Chapter Key Concepts 206 11.13 Chapter Problems 207 12 Laboratory Information Management System (LIMS) 209 12.1 Introduction 209 12.2 LIMS Main Menu 209 12.3 Logging in Samples 209 12.4 Entering Test Results 209 12.5 Add or Delete Tests 211 12.6 Calculations and Curves 212 12.7 Search Wizards 214 12.8 Approving Samples 218 12.9 Printing Sample Reports 220 13 Ultraviolet and Visible (UV/Vis) Spectroscopy 221 13.1 Introduction to Spectroscopy in the Analytical Laboratory 221 13.2 The Electromagnetic Spectrum 221 13.3 Ultraviolet/Visible (UV/Vis) Spectroscopy 221 13.4 UV/Visible Spectrophotometers 230 13.5 Special Topic (Example)—Spectrophotometric Study of Dye Compounds 234 13.6 Chapter Key Concepts 236 13.7 Chapter Problems 237 14 Fluorescence Optical Emission Spectroscopy 239 14.1 Introduction to Fluorescence 239 14.2 Fluorescence and Phosphorescence Theory 240 14.3 Phosphorescence 241 14.4 Excitation and Emission Spectra 242 14.5 Rate Constants 243 14.6 Quantum Yield Rate Constants 243 14.7 Decay Lifetimes 244 14.8 Factors Affecting Fluorescence 244 14.9 Quantitative Analysis and Beer–Lambert Law 248 14.10 Quenching of Fluorescence 249 14.11 Fluorometric Instrumentation 249 14.12 Special Topic—Flourescence Study of Dye-A007 Complexes 255 14.13 Chapter Key Concepts 257 14.14 Chapter Problems 258 15 Fourier Transform Infrared (FTIR) Spectroscopy 261 15.1 Introduction 261 15.2 Basic IR Instrument Design 261 15.3 The Infrared Spectrum and Molecular Assignment 263 15.4 FTIR Table Band Assignments 264 15.5 FTIR Spectrum Example I 270 15.6 FTIR Spectrum Example II 270 15.7 FTIR Inorganic Compound Analysis 271 15.8 Chapter Key Concepts 271 15.9 Chapter Problems 273 16 Nuclear Magnetic Resonance (NMR) Spectroscopy 277 16.1 Introduction 277 16.2 Frequency and Magnetic Field Strength 277 16.3 Continuous-Wave NMR 278 16.4 The NMR Sample Probe 280 16.5 Pulsed Field Fourier Transform NMR 280 16.6 Proton NMR Spectra Environmental Effects 280 16.7 Carbon-13 NMR 283 16.8 Special Topic—NMR Characterization of Cholesteryl Phosphate 287 16.9 Chapter Key Concepts 292 16.10 Chapter Problems 293 References 294 17 Atomic Absorption Spectroscopy (AAS) 295 17.1 Introduction 295 17.2 Atomic Absorption and Emission Process 295 17.3 Atomic Absorption and Emission Source 296 17.4 Source Gases and Flames 296 17.5 Block Diagram of AAS Instrumentation 296 17.6 The Light Source 297 17.7 Interferences in AAS 299 17.8 Electrothermal Atomization—Graphite Furnace 299 17.9 Instrumentation 300 17.10 Flame Atomic Absorption Analytical Methods 301 18 Atomic Emission Spectroscopy 303 18.1 Introduction 303 18.2 Elements in Periodic Table 303 18.3 The Plasma Torch 303 18.4 Sample Types 304 18.5 Sample Introduction 304 18.6 ICP-OES Instrumentation 305 18.7 ICP-OES Environmental Application Example 310 19 Atomic Mass Spectrometry 325 19.1 Introduction 325 19.2 Low-Resolution ICP-MS 325 19.3 High-Resolution ICP-MS 328 20 X-ray Fluorescence (XRF) and X-ray Diffraction (XRD) 333 20.1 X-Ray Fluorescence Introduction 333 20.2 X-Ray Fluorescence Theory 333 20.3 Energy-Dispersive X-Ray Fluorescence (EDXRF) 334 20.4 Wavelength Dispersive X-Ray Fluorescence (WDXRF) 337 20.5 Applications of XRF 341 20.6 X-ray Diffraction (XRD) 342 21 Chromatography—Introduction and Theory 351 21.1 Preface 351 21.2 Introduction to Chromatography 351 21.3 Theory of Chromatography 351 21.4 The Theoretical Plate Number N 355 21.5 Resolution RS 356 21.6 Rate Theory versus Plate Theory 357 21.7 Retention Factor k 361 References 362 22 High Performance Liquid Chromatography (HPLC) 363 22.1 HPLC Background 363 22.2 Design and Components of HPLC 363 23 Solid-Phase Extraction 381 23.1 Introduction 381 23.2 Disposable SPE Columns 381 23.3 SPE Vacuum Manifold 381 23.4 SPE Procedural Bulletin 381 24 Plane Chromatography: Paper and Thin-Layer Chromatography 395 24.1 Plane Chromatography 395 24.2 Thin-Layer Chromatography 395 24.3 Retardation Factor (RF) in TLC 398 24.4 Plate Heights (H) and Counts (N) in TLC 398 24.5 Retention Factor in TLC 399 25 Gas-Liquid Chromatography 401 25.1 Introduction 401 25.2 Theory and Principle of GC 401 25.3 Mobile-Phase Carrier Gasses in GC 403 25.4 Columns and Stationary Phases 404 25.5 Gas Chromatograph Injection Port 406 25.6 The GC Oven 415 25.7 GC Programming and Control 417 25.8 GC Detectors 418 26 Gas Chromatography–Mass Spectrometry (GC–MS) 421 26.1 Introduction 421 26.2 Electron Ionization (EI) 421 26.3 Electron Ionization (EI)/OE Processes 422 26.4 Oleamide Fragmentation Pathways: OE M+• by Gas Chromatography/Electron Ionization Mass Spectrometry 425 26.5 Oleamide Fragmentation Pathways: EE [M+H]+ by ESI/Ion Trap Mass Spectrometry 426 26.6 Quantitative Analysis by GC/EI–MS 429 26.7 Chapter Problems 431 References 433 27 Special Topics: Strong Cation Exchange Chromatography and Capillary Electrophoresis 435 27.1 Introduction 435 27.2 Strong Ion Exchange HPLC 435 27.3 CZE 435 27.4 Binding Constants by Cation Exchange and CZE 436 27.5 Comparison of Methods 446 27.6 Conclusions 448 References 448 28 Mass Spectrometry 449 28.1 Definition and Description of Mass Spectrometry 449 28.2 Basic Design of Mass Analyzer Instrumentation 449 28.3 Mass Spectrometry of Protein Metabolite and Lipid Biomolecules 451 28.4 Fundamental Studies of Biological Compound Interactions 455 28.5 Mass-to-Charge (m/z) Ratio: How the Mass Spectrometer Separates Ions 457 28.6 Exact Mass versus Nominal Mass 458 28.7 Mass Accuracy and Resolution 460 28.8 High-Resolution Mass Measurements 461 28.9 Rings Plus Double Bonds (r + db) 463 28.10 The Nitrogen Rule in Mass Spectrometry 464 28.11 Chapter Problems 465 References 465 29 Ionization in Mass Spectrometry 467 29.1 Ionization Techniques and Sources 467 29.2 Chemical Ionization (CI) 467 29.3 Atmospheric Pressure Chemical Ionization (APCI) 471 29.4 Electrospray Ionization (ESI) 472 29.5 Nanoelectrospray Ionization (Nano-ESI) 474 29.6 Atmospheric Pressure Photo Ionization (APPI) 477 29.7 Matrix Assisted Laser Desorption Ionization (MALDI) 483 29.8 FAB 485 29.9 Chapter Problems 489 References 489 30 Mass Analyzers in Mass Spectrometry 491 30.1 Mass Analyzers 491 30.2 Magnetic and Electric Sector Mass Analyzer 491 30.3 Time-of-Flight Mass Analyzer (TOF/MS) 496 30.4 Time-of-Flight/Time-of-Flight Mass Analyzer (TOF–TOF/MS) 497 30.5 Quadrupole Mass Filter 500 30.6 Triple Quadrupole Mass Analyzer (QQQ/MS) 502 30.7 Three-Dimensional Quadrupole Ion Trap Mass Analyzer (QIT/MS) 503 30.8 Linear Quadrupole Ion Trap Mass Analyzer (LTQ/MS) 506 30.9 Quadrupole Time-of-Flight Mass Analyzer (Q-TOF/MS) 507 30.10 Fourier Transform Ion Cyclotron Resonance Mass Analyzer (FTICR/MS) 508 30.11 Linear Quadrupole Ion Trap Fourier Transform Mass Analyzer (LTQ–FT/MS) 517 30.12 Linear Quadrupole Ion Trap Orbitrap Mass Analyzer (LTQ–Orbitrap/MS) 518 30.13 Chapter Problems 527 References 527 31 Biomolecule Spectral Interpretation: Small Molecules 529 31.1 Introduction 529 31.2 Ionization Efficiency of Lipids 529 31.3 Fatty Acids 530 31.4 Wax Esters 537 31.5 Sterols 542 31.6 Acylglycerols 548 31.7 ESI-Mass Spectrometry of Phosphorylated Lipids 551 31.8 Chapter Problems 556 References 557 32 Macromolecule Analysis 559 32.1 Introduction 559 32.2 Carbohydrates 559 32.3 Nucleic Acids 565 32.4 Chapter Problems 576 References 577 33 Biomolecule Spectral Interpretation: Proteins 579 33.1 Introduction to Proteomics 579 33.2 Protein Structure and Chemistry 579 33.3 Bottom-up Proteomics: Mass Spectrometry of Peptides 580 33.4 Top-Down Proteomics: Mass Spectrometry of Intact Proteins 590 33.5 PTM of Proteins 594 33.6 Systems Biology and Bioinformatics 614 33.7 Chapter Problems 618 References 619 Appendix I: Chapter Problem Answers 621 Appendix II: Atomic Weights and Isotopic Compositions 627 Appendix III: Fundamental Physical Constants 631 Appendix IV: Redox Half Reactions 633 Appendix V: Periodic Table of Elements 637 Appendix VI: Installing and Running Programs 639 Index 641

Reviews

This book intends to combine theoretical and practical aspects of analytical chemistry, and generally, it can be considered a success: both the concepts and analytical techniques and the focus on the laboratory aspects of this field are chosen didactically well, offering not only a detailed overview but also demonstrating connections of different techniques. (Analytical and Bioanalytical Chemistry 2016)

"""This book intends to combine theoretical and practical aspects of analytical chemistry, and generally, it can be considered a success: both the concepts and analytical techniques and the focus on the laboratory aspects of this field are chosen didactically well, offering not only a detailed overview but also demonstrating connections of different techniques."" (Analytical and Bioanalytical Chemistry 2016)"

Author Information

BRYAN M. HAM, Ph.D., has worked in analytical chemistry laboratories for over 25 years including petroleum, chemical, environmental, foodstuff, and life science research, and has a doctorate in analytical chemistry. He has published 15 research papers in peer reviewed journals and two books: Even Electron Mass Spectrometry with Biomolecule Applications (Wiley, 2008), and Proteomics of Biological Systems: Protein Phosphorylation Using Mass Spectrometry Techniques (Wiley, 2012). He is currently working for the Department of Homeland Security at the U.S. Customs and Border Protection New York Laboratory. He is a member of the American Society of Mass Spectrometry (ASMS) and the American Chemical Society (ACS). AIHUI MAHAM, Ph.D., is an expert in nano-materials including the synthesis and characterization of chemical and biological nano-sensors. She is also an expert in the field of inorganic materials chemistry, and their characterization utilizing methodologies such as SEM, XRD, XRF and OES. She has published numerous research papers including a recent review entitled Protein-Based Nanomedicine Platforms for Drug Delivery (Small, 2009), which has been cited over 170 times by other researchers. She is currently working for the Department of Homeland Security at the U.S. Customs and Border Protection New York Laboratory.

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