Detailed reference covering all aspects of working in laboratories, including safety, fundamentals of analytical techniques, lab instrumentation, and more

About the Authors xxiiiPreface xxvAcknowledgments xxviiAbout the Companion Website xxviii1 Chemist and Technician in the Analytical Laboratory 11.1 Introduction--The Analytical Chemist and Technician 11.2 Today's Laboratory Chemist and Technician 11.3 ChemTech--The Chemist and Technician Toolkit Companion 21.4 Chapter Layout 21.5 Users of ChemTech 62 Introduction to the Analytical Laboratory 72.1 Introduction to the Laboratory 72.2 Laboratory Glassware 72.3 Conclusion 183 Laboratory Safety 193.1 Introduction 193.2 Proper Personal Protection and Appropriate Attire 193.3 Proper Shoes and Pants 203.4 Laboratory Gloves 203.5 General Rules to Use Gloves 223.6 Safety Data Sheet (SDS) 223.7 Emergency Eyewash and Face Wash Stations 243.8 Emergency Safety Showers 253.9 Fire Extinguishers 253.10 Clothing Fire in The Laboratory 263.11 Spill Cleanup Kits 263.12 Chemicals and Solvents 273.13 First Aid Kits 293.14 Gasses and Cylinders 293.15 Sharps Containers and Broken Glass Boxes 303.16 Occupational Safety and Health Administration (OSHA) 304 Basic Mathematics in the Laboratory 834.1 Introduction to Basic Math 834.2 Units and Metric System 834.3 Significant Figures 844.4 Scientific Calculators 864.5 ChemTech Conversion Tool 894.6 Chapter Key Concepts 964.7 Chapter Problems 965 Analytical Data Treatment (Statistics) 975.1 Errors in the Laboratory 975.2 Expressing Absolute and Relative Errors 985.3 Precision 985.4 The Normal Distribution Curve 985.5 Precision of Experimental Data 1005.6 Normal Distribution Curve of a Sample 1015.7 ChemTech Statistical Calculations 1025.8 Student's Distribution t Test for Confidence Limits 1055.9 Tests of Significance 1115.10 Treatment of Data Outliers 1125.11 Chapter Key Concepts 1145.12 Chapter Problems 1146 Plotting and Graphing 1166.1 Introduction to Graphing 1166.2 Graph Construction 1166.3 Rectangular Cartesian Coordinate System 1176.4 Curve Fitting 1176.5 Redrawn Graph Example 1176.6 Graphs of Equations 1186.7 Least-Squares Method 1216.8 Computer-Generated Curves 1226.9 Calculating Concentrations 1256.10 Nonlinear Curve Fitting 1266.11 Chapter Key Concepts 1306.12 Chapter Problems 1307 Using Microsoft Excel(r) in the Laboratory 1327.1 Introduction to Excel(r) 1327.2 Opening Excel in ChemTech 1327.3 The Excel Spreadsheet 1327.4 Graphing in Excel 1347.5 Complex Charting in Excel 1377.6 Statistical Analysis using Excel 1398 Making Laboratory Solutions 1518.1 Introduction 1518.2 Laboratory Reagent Fundamentals 1518.3 The Periodic Table 1518.4 Calculating Formula Weights 1528.5 Calculating The Mole 1528.6 Molecular Weight Calculator 1528.7 Expressing Concentration 1538.8 The Parts PER (PP) Notation 1578.9 Computer-Based Solution Calculations 1578.10 Reactions in Solution 1618.11 Chapter Key Concepts 1618.12 Chapter Problems 1629 Acid-Base Theory and Buffer Solutions 1639.1 Introduction 1639.2 Acids and Bases in Everyday Life 1639.3 The Litmus Test 1639.4 Early Acid-Base Descriptions 1649.5 Brÿnsted-Lowry Definition 1649.6 The Equilibrium Constant 1659.7 The Acid Ionization Constant 1659.8 Calculating the Hydrogen Ion Concentration 1659.9 The Base Ionization Constant 1679.10 Ion Product for Water 1689.11 The Solubility Product Constant (K SP) 1689.12 The pH of a Solution 1709.13 Measuring the pH 1719.14 Buffered Solutions--Description and Preparing 1729.15 ChemTech Buffer Solution Calculator 1749.16 Chapter Key Concepts 1759.17 Chapter Problems 17510 Titration--A Volumetric Method of Analysis 17810.1 Introduction 17810.2 Reacting Ratios 17810.3 The Equivalence Point 17910.4 Useful Relationships for Calculations 17910.5 Deriving the Titration Equation 17910.6 Titrations in ChemTech 18010.7 Acid/Base Titration Endpoint (Equivalence Point) 18110.8 Acid/Base Titration Midpoint 18210.9 Acid/Base Titration Indicators 18210.10 Titrations Using Normal Solutions 18410.11 Polyprotic Acid Titration 18410.12 ChemTech Calculation of Normal Titrations 18510.13 Performing a Titration 18510.14 Primary Standards 18610.15 Standardization of Sodium Hydroxide 18710.16 Conductometric Titrations (Nonaqueous Solutions) 18910.17 Precipitation Titration (MOHR Method for Halides) 19010.18 Complex Formation with Back Titration (Volhard Method for Anions) 19110.19 Chapter Key Concepts 19610.20 Chapter Problems 19711 Oxidation-Reduction (Redox) Reactions 19911.1 Introduction 19911.2 Oxidation and Reduction 19911.3 The Volt 20011.4 The Electrochemical Cell 20011.5 Redox Reaction Conventions 20011.6 The Nernst Equation 20211.7 Determining Redox Titration Endpoints 20311.8 Potentiometric Titrations 20411.9 Visual Indicators used in Redox Titrations 20611.10 Pretitration Oxidation-Reduction 20711.11 Ion-Selective Electrodes 20711.12 Chapter Key Concepts 20711.13 Chapter Problems 20912 Laboratory Information Management System (LIMS) 21112.1 Introduction 21112.2 Lims Main Menu 21112.3 Logging in Samples 21312.4 Entering Test Results 21312.5 Add or Delete Tests 21412.6 Calculations and Curves 21412.7 Search Wizards 21512.8 Approving Samples 21712.9 Printing Sample Reports 21713 Ultraviolet and Visible (UV/VIS) Spectroscopy 22713.1 Introduction to Spectroscopy in the Analytical Laboratory 22713.2 The Electromagnetic Spectrum 22713.3 Ultraviolet/Visible (UV/VIS) Spectroscopy 22713.4 UV/Visible Spectrophotometers 23613.5 Special Topic (Example)--Spectrophotometric Study of Dye Compounds 23713.6 Chapter Key Concepts 24013.7 Chapter Problems 24214 Fluorescence Optical Emission Spectroscopy 24414.1 Introduction to Fluorescence 24414.2 Fluorescence and Phosphorescence Theory 24514.3 Phosphorescence 24614.4 Excitation and Emission Spectra 24714.5 Rate Constants 24714.6 Quantum Yield Rate Constants 24814.7 Decay Lifetimes 24814.8 Factors Affecting Fluorescence 24914.9 Quantitative Analysis and Beer-Lambert Law 25214.10 Quenching of Fluorescence 25314.11 Fluorometric Instrumentation 25314.12 Special Topic--Fluorescence Study of Dye-A007 Complexes 25914.13 Chapter Key Concepts 26114.14 Chapter Problems 26215 Fourier Transform Infrared (FTIR) Spectroscopy 26415.1 Introduction 26415.2 Basic IR Instrument Design 26415.3 The Infrared Spectrum and Molecular Assignment 26615.4 FTIR Table Band Assignments 26715.5 FTIR Spectrum Example I 27315.6 FTIR Spectrum Example II 27315.7 FTIR Inorganic Compound Analysis 27415.8 Chapter Key Concepts 27415.9 Chapter Problems 27616 Nuclear Magnetic Resonance (NMR) Spectroscopy 28016.1 Introduction 28016.2 Frequency and Magnetic Field Strength 28016.3 Continuous-Wave NMR 28116.4 The NMR Sample Probe 28216.5 Pulsed-Field Fourier Transform NMR 28216.6 Proton NMR Spectra Environmental Effects 28416.7 Carbon-13 NMR 28616.8 Special Topic--NMR Characterization of Cholesteryl Phosphate 29016.9 Chapter Key Concepts 29516.10 Chapter Problems 296References 29717 Atomic Absorption Spectroscopy (AAS) 29817.1 Introduction 29817.2 Atomic Absorption and Emission Process 29817.3 Atomic Absorption and Emission Source 29917.4 Source Gases and Flames 29917.5 Block Diagram of AAS Instrumentation 29917.6 The Light Source 30117.7 Interferences in AAS 30217.8 Electrothermal Atomization--Graphite Furnace 30217.9 Instrumentation 30317.10 Flame Atomic Absorption Analytical Methods 30418 Atomic Emission Spectroscopy 30618.1 Introduction 30618.2 Elements in Periodic Table 30618.3 The Plasma Torch 30618.4 Sample Types 30718.5 Sample Introduction 30818.6 ICP-OES Instrumentation 30818.7 ICP-OES Environmental Application Example 31319 Atomic Mass Spectrometry 32819.1 Introduction 32819.2 Low-Resolution ICP-MS 32819.3 High-Resolution ICP-MS 33120 X-Ray Fluorescence (XRF) and X-Ray Diffraction (XRD) 33620.1 X-Ray Fluorescence Introduction 33620.2 X-Ray Fluorescence Theory 33620.3 Energy-Dispersive X-Ray Fluorescence (EDXRF) 33720.4 Wavelength Dispersive X-Ray Fluorescence (WDXRF) 34020.5 Applications of XRF 34420.6 X-Ray Diffraction (XRD) 34521 Chromatography--Introduction and Theory 35421.1 Preface 35421.2 Introduction to Chromatography 35421.3 Theory of Chromatography 35421.4 The Theoretical Plate Number N 35821.5 Resolution Rs 35921.6 Rate Theory Versus Plate Theory 36021.7 Retention Factor k' 365References 36522 High-Performance Liquid Chromatography (HPLC) 36622.1 HPLC Background 36622.2 Design and Components of HPLC 36623 Solid-Phase Extraction 38323.1 Introduction 38323.2 Disposable SPE Columns 38323.3 SPE Vacuum Manifold 38323.4 SPE Procedural Bulletin 38324 Plane Chromatography: Paper and Thin-Layer Chromatography 39724.1 Plane Chromatography 39724.2 Thin-Layer Chromatography 39824.3 Retardation Factor (R F) In TLC 39924.4 Plate Heights (H) and Counts (N) In TLC 40024.5 Retention Factor In TLC 40125 Gas-Liquid Chromatography 40225.1 Introduction 40225.2 Theory and Principle of GC 40225.3 Mobile-Phase Carrier Gasses in GC 40425.4 Columns and Stationary Phases 40525.5 Gas Chromatograph Injection Port 40725.6 The GC Oven 41525.7 GC Programming and Control 41825.8 GC Detectors 41926 Gas Chromatography-Mass Spectrometry (GC-MS) 42226.1 Introduction 42226.2 Electron Ionization (EI) 42226.3 Electron Ionization (EI)/OE Processes 42326.4 Oleamide Fragmentation Pathways: OE M +s by Gas Chromatography/Electron Ionization Mass Spectrometry 42626.5 Oleamide Fragmentation Pathways: EE [M+H] + by ESI/ION Trap Mass Spectrometry 42726.6 Quantitative Analysis by GC/EI-MS 43026.7 Chapter Problems 432References 43427 Special Topics: Strong Cation Exchange Chromatography and Capillary Electrophoresis 43627.1 Introduction 43627.2 Strong Ion Exchange HPLC 43627.3 Cze 43627.4 Binding Constants by Cation Exchange and CZE 43727.5 Comparison of Methods 44627.6 Conclusions 449References 44928 Mass Spectrometry 45028.1 Definition and Description of Mass Spectrometry 45028.2 Basic Design of Mass Analyzer Instrumentation 45028.3 Mass Spectrometry of Protein Metabolite and Lipid Biomolecules 45228.4 Fundamental Studies of Biological Compound Interactions 45628.5 Mass-to-Charge (m/z) Ratio: How the Mass Spectrometer Separates Ions 45728.6 Exact Mass Versus Nominal Mass 45928.7 Mass Accuracy and Resolution 46028.8 High-Resolution Mass Measurements 46228.9 Rings Plus Double Bonds (r+db) 46428.10 The Nitrogen Rule in Mass Spectrometry 46528.11 Chapter Problems 466References 46629 Ionization in Mass Spectrometry 46829.1 Ionization Techniques and Sources 46829.2 Chemical Ionization (CI) 46829.3 Atmospheric Pressure Chemical Ionization (APCI) 47229.4 Electrospray Ionization (ESI) 47429.5 Nanoelectrospray Ionization (NANO-ESI) 47629.6 Atmospheric Pressure Photoionization (APPI) 47929.7 Matrix-Assisted Laser Desorption Ionization (MALDI) 48429.8 Fab 48629.9 Chapter Problems 490References 49030 Mass Analyzers in Mass Spectrometry 49230.1 Mass Analyzers 49230.2 Magnetic and Electric Sector Mass Analyzer 49230.3 Time-of-Flight Mass Analyzer (TOF/MS) 49630.4 Time-of-Flight/Time-of-Flight Mass Spectrometer (TOF-TOF/MS) 49830.5 Quadrupole Mass Filter 50030.6 Triple Quadrupole Mass Spectrometer (QQQ/MS) 50330.7 Three-Dimensional Quadrupole Ion Trap Mass Spectrometer (QIT/MS) 50430.8 Linear Quadrupole Ion Trap Mass Spectrometer (LTQ/MS) 50630.9 Quadrupole Time-of-Flight Mass Spectrometer (Q-TOF/MS) 50830.10 Fourier Transform Ion Cyclotron Resonance Mass Spectrometer (fticr/ms) 50930.11 Linear Quadrupole Ion Trap Fourier Transform Mass Spectrometer (ltq-ft/ms) 51730.12 Linear Quadrupole Ion Trap Orbitrap Mass Spectrometer (LTQ-Orbitrap/MS) 51930.13 Chapter Problems 527References 52831 Biomolecule Spectral Interpretation: Small Molecules 52931.1 Introduction 52931.2 Ionization Efficiency of Lipids 52931.3 Fatty Acids 53031.4 Wax Esters 53831.5 Sterols 54231.6 Acylglycerols 54731.7 Esi-Mass Spectrometry of Phosphorylated Lipids 55031.8 Chapter Problems 556References 55732 Macromolecule Analysis 55932.1 Introduction 55932.2 Carbohydrates 55932.3 Nucleic Acids 56532.4 Chapter Problems 576References 57633 Biomolecule Spectral Interpretation: Proteins 57733.1 Introduction to Proteomics 57733.2 Protein Structure and Chemistry 57733.3 Bottom-Up Proteomics: Mass Spectrometry of Peptides 57833.4 Top-Down Proteomics: Mass Spectrometry of Intact Proteins 58833.5 PTM of Proteins 59233.6 Systems Biology and Bioinformatics 61033.7 Chapter Problems 614References 616Appendix I: Chapter Problem Answers 619Appendix II: Atomic Weights and Isotopic Compositions 625Appendix III: Fundamental Physical Constants 629Appendix IV: Redox Half-Reactions 630Appendix V: Periodic Table of Elements 633Appendix VI: Installing and Running Programs 635Index 637