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

Preface xxiiiAuthor Biographies xxvAcknowledgments xxvii1 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 11.4 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 Material Safety Data Sheet (MSDS) 223.7 Emergency Eye Wash and Face Wash Stations 233.8 Emergency Safety Showers 243.9 Fire Extinguishers 243.10 Clothing Fire in the Laboratory 253.11 Spill Cleanup Kits 253.12 Chemicals and Solvents 273.13 First Aid Kits 273.14 Gasses and Cylinders 293.15 Sharps Containers and Broken Glass Boxes 293.16 Occupational Safety and Health Administration (OSHA) 294 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 894.7 Chapter Problems 925 Analytical Data Treatment (Statistics) 935.1 Errors in the Laboratory 935.2 Expressing Absolute and Relative Errors 945.3 Precision 945.4 The Normal Distribution Curve 945.5 Precision of Experimental Data 965.6 Normal Distribution Curve of a Sample 975.7 ChemTech Statistical Calculations 985.8 Student's Distribution t Test for Confidence Limits 1015.9 Tests of Significance 1045.10 Treatment of Data Outliers 1055.11 Chapter Key Concepts 1065.12 Chapter Problems 1076 Plotting and Graphing 1096.1 Introduction to Graphing 1096.2 Graph Construction 1096.3 Rectangular Cartesian Coordinate System 1106.4 Curve Fitting 1106.5 Redrawn Graph Example 1106.6 Graphs of Equations 1116.7 Least-Squares Method 1146.8 Computer-Generated Curves 1156.9 Calculating Concentrations 1196.10 Nonlinear Curve Fitting 1196.11 Chapter Key Concepts 1236.12 Chapter Problems 1247 Using Microsoft Excel® in the Laboratory 1257.1 Introduction to Excel® 1257.2 Opening Excel® in ChemTech 1257.3 The Excel® Spreadsheet 1257.4 Graphing in Excel® 1277.5 Charts in Excel® 2010 1327.6 Complex Charting in Excel® 97-2003 1327.7 Complex Charting in Excel® 2010 1397.8 Statistical Analysis Using Excel® 1418 Making Laboratory Solutions 1478.1 Introduction 1478.2 Laboratory Reagent Fundamentals 1478.3 The Periodic Table 1478.4 Calculating Formula Weights 1488.5 Calculating the Mole 1488.6 Molecular Weight Calculator 1488.7 Expressing Concentration 1488.8 The Parts per (PP) Notation 1538.9 Computer-Based Solution Calculations 1538.10 Reactions in Solution 1578.11 Chapter Key Concepts 1578.12 Chapter Problems 1589 Acid-Base Theory and Buffer Solutions 1599.1 Introduction 1599.2 Acids and Bases in Everyday Life 1599.3 The Litmus Test 1599.4 Early Acid-Base Descriptions 1609.5 Brÿnsted-Lowry Definition 1609.6 The Equilibrium Constant 1619.7 The Acid Ionization Constant 1619.8 Calculating the Hydrogen Ion Concentration 1629.9 The Base Ionization Constant 1639.10 Ion Product for Water 1649.11 The Solubility Product Constant (Ksp) 1649.12 The pH of a Solution 1669.13 Measuring the pH 1679.14 Buffered Solutions--Description and Preparing 1689.15 ChemTech Buffer Solution Calculator 1709.16 Chapter Key Concepts 1719.17 Chapter Problems 17210 Titration--A Volumetric Method of Analysis 17510.1 Introduction 17510.2 Reacting Ratios 17510.3 The Equivalence Point 17610.4 Useful Relationships for Calculations 17610.5 Deriving the Titration Equation 17610.6 Titrations in ChemTech 17710.7 Acid/Base Titration Endpoint (Equivalence Point) 17810.8 Acid/Base Titration Midpoint 17910.9 Acid/Base Titration Indicators 18010.10 Titrations Using Normal Solutions 18110.11 Polyprotic Acid Titration 18110.12 ChemTech Calculation of Normal Titrations 18210.13 Performing a Titration 18310.14 Primary Standards 18410.15 Standardization of Sodium Hydroxide 18510.16 Conductometric Titrations (Nonaqueous Solutions) 18610.17 Precipitation Titration (Mohr Method for Halides) 18810.18 Complex Formation with Back Titration (Volhard Method for Anions) 18910.19 Complex Formation Titration with EDTA for Cations 19010.20 Chapter Key Concepts 19410.21 Chapter Problems 19511 Oxidation-Reduction (Redox) Reactions 19711.1 Introduction 19711.2 Oxidation and Reduction 19711.3 The Volt 19811.4 The Electrochemical Cell 19811.5 Redox Reaction Conventions 19811.6 The Nernst Equation 20011.7 Determining Redox Titration Endpoints 20211.8 Potentiometric Titrations 20211.9 Visual Indicators Used in Redox Titrations 20411.10 Pretitration Oxidation-Reduction 20511.11 Ion-Selective Electrodes 20611.12 Chapter Key Concepts 20611.13 Chapter Problems 20712 Laboratory Information Management System (LIMS) 20912.1 Introduction 20912.2 LIMS Main Menu 20912.3 Logging in Samples 20912.4 Entering Test Results 20912.5 Add or Delete Tests 21112.6 Calculations and Curves 21212.7 Search Wizards 21412.8 Approving Samples 21812.9 Printing Sample Reports 22013 Ultraviolet and Visible (UV/Vis) Spectroscopy 22113.1 Introduction to Spectroscopy in the Analytical Laboratory 22113.2 The Electromagnetic Spectrum 22113.3 Ultraviolet/Visible (UV/Vis) Spectroscopy 22113.4 UV/Visible Spectrophotometers 23013.5 Special Topic (Example)--Spectrophotometric Study of Dye Compounds 23413.6 Chapter Key Concepts 23613.7 Chapter Problems 23714 Fluorescence Optical Emission Spectroscopy 23914.1 Introduction to Fluorescence 23914.2 Fluorescence and Phosphorescence Theory 24014.3 Phosphorescence 24114.4 Excitation and Emission Spectra 24214.5 Rate Constants 24314.6 Quantum Yield Rate Constants 24314.7 Decay Lifetimes 24414.8 Factors Affecting Fluorescence 24414.9 Quantitative Analysis and Beer-Lambert Law 24814.10 Quenching of Fluorescence 24914.11 Fluorometric Instrumentation 24914.12 Special Topic--Flourescence Study of Dye-A007 Complexes 25514.13 Chapter Key Concepts 25714.14 Chapter Problems 25815 Fourier Transform Infrared (FTIR) Spectroscopy 26115.1 Introduction 26115.2 Basic IR Instrument Design 26115.3 The Infrared Spectrum and Molecular Assignment 26315.4 FTIR Table Band Assignments 26415.5 FTIR Spectrum Example I 27015.6 FTIR Spectrum Example II 27015.7 FTIR Inorganic Compound Analysis 27115.8 Chapter Key Concepts 27115.9 Chapter Problems 27316 Nuclear Magnetic Resonance (NMR) Spectroscopy 27716.1 Introduction 27716.2 Frequency and Magnetic Field Strength 27716.3 Continuous-Wave NMR 27816.4 The NMR Sample Probe 28016.5 Pulsed Field Fourier Transform NMR 28016.6 Proton NMR Spectra Environmental Effects 28016.7 Carbon-13 NMR 28316.8 Special Topic--NMR Characterization of Cholesteryl Phosphate 28716.9 Chapter Key Concepts 29216.10 Chapter Problems 293References 29417 Atomic Absorption Spectroscopy (AAS) 29517.1 Introduction 29517.2 Atomic Absorption and Emission Process 29517.3 Atomic Absorption and Emission Source 29617.4 Source Gases and Flames 29617.5 Block Diagram of AAS Instrumentation 29617.6 The Light Source 29717.7 Interferences in AAS 29917.8 Electrothermal Atomization--Graphite Furnace 29917.9 Instrumentation 30017.10 Flame Atomic Absorption Analytical Methods 30118 Atomic Emission Spectroscopy 30318.1 Introduction 30318.2 Elements in Periodic Table 30318.3 The Plasma Torch 30318.4 Sample Types 30418.5 Sample Introduction 30418.6 ICP-OES Instrumentation 30518.7 ICP-OES Environmental Application Example 31019 Atomic Mass Spectrometry 32519.1 Introduction 32519.2 Low-Resolution ICP-MS 32519.3 High-Resolution ICP-MS 32820 X-ray Fluorescence (XRF) and X-ray Diffraction (XRD) 33320.1 X-Ray Fluorescence Introduction 33320.2 X-Ray Fluorescence Theory 33320.3 Energy-Dispersive X-Ray Fluorescence (EDXRF) 33420.4 Wavelength Dispersive X-Ray Fluorescence (WDXRF) 33720.5 Applications of XRF 34120.6 X-ray Diffraction (XRD) 34221 Chromatography--Introduction and Theory 35121.1 Preface 35121.2 Introduction to Chromatography 35121.3 Theory of Chromatography 35121.4 The Theoretical Plate Number N 35521.5 Resolution RS 35621.6 Rate Theory versus Plate Theory 35721.7 Retention Factor k 361References 36222 High Performance Liquid Chromatography (HPLC) 36322.1 HPLC Background 36322.2 Design and Components of HPLC 36323 Solid-Phase Extraction 38123.1 Introduction 38123.2 Disposable SPE Columns 38123.3 SPE Vacuum Manifold 38123.4 SPE Procedural Bulletin 38124 Plane Chromatography: Paper and Thin-Layer Chromatography 39524.1 Plane Chromatography 39524.2 Thin-Layer Chromatography 39524.3 Retardation Factor (RF) in TLC 39824.4 Plate Heights (H) and Counts (N) in TLC 39824.5 Retention Factor in TLC 39925 Gas-Liquid Chromatography 40125.1 Introduction 40125.2 Theory and Principle of GC 40125.3 Mobile-Phase Carrier Gasses in GC 40325.4 Columns and Stationary Phases 40425.5 Gas Chromatograph Injection Port 40625.6 The GC Oven 41525.7 GC Programming and Control 41725.8 GC Detectors 41826 Gas Chromatography-Mass Spectrometry (GC-MS) 42126.1 Introduction 42126.2 Electron Ionization (EI) 42126.3 Electron Ionization (EI)/OE Processes 42226.4 Oleamide Fragmentation Pathways: OE M+* by Gas Chromatography/Electron Ionization Mass Spectrometry 42526.5 Oleamide Fragmentation Pathways: EE [M+H]+ by ESI/Ion Trap Mass Spectrometry 42626.6 Quantitative Analysis by GC/EI-MS 42926.7 Chapter Problems 431References 43327 Special Topics: Strong Cation Exchange Chromatography and Capillary Electrophoresis 43527.1 Introduction 43527.2 Strong Ion Exchange HPLC 43527.3 CZE 43527.4 Binding Constants by Cation Exchange and CZE 43627.5 Comparison of Methods 44627.6 Conclusions 448References 44828 Mass Spectrometry 44928.1 Definition and Description of Mass Spectrometry 44928.2 Basic Design of Mass Analyzer Instrumentation 44928.3 Mass Spectrometry of Protein, Metabolite, and Lipid Biomolecules 45128.4 Fundamental Studies of Biological Compound Interactions 45528.5 Mass-to-Charge (m/z) Ratio: How the Mass Spectrometer Separates Ions 45728.6 Exact Mass versus Nominal Mass 45828.7 Mass Accuracy and Resolution 46028.8 High-Resolution Mass Measurements 46128.9 Rings Plus Double Bonds (r + db) 46328.10 The Nitrogen Rule in Mass Spectrometry 46428.11 Chapter Problems 465References 46529 Ionization in Mass Spectrometry 46729.1 Ionization Techniques and Sources 46729.2 Chemical Ionization (CI) 46729.3 Atmospheric Pressure Chemical Ionization (APCI) 47129.4 Electrospray Ionization (ESI) 47229.5 Nanoelectrospray Ionization (Nano-ESI) 47429.6 Atmospheric Pressure Photo Ionization (APPI) 47729.7 Matrix Assisted Laser Desorption Ionization (MALDI) 48329.8 FAB 48529.9 Chapter Problems 489References 48930 Mass Analyzers in Mass Spectrometry 49130.1 Mass Analyzers 49130.2 Magnetic and Electric Sector Mass Analyzer 49130.3 Time-of-Flight Mass Analyzer (TOF/MS) 49630.4 Time-of-Flight/Time-of-Flight Mass Analyzer (TOF-TOF/MS) 49730.5 Quadrupole Mass Filter 50030.6 Triple Quadrupole Mass Analyzer (QQQ/MS) 50230.7 Three-Dimensional Quadrupole Ion Trap Mass Analyzer (QIT/MS) 50330.8 Linear Quadrupole Ion Trap Mass Analyzer (LTQ/MS) 50630.9 Quadrupole Time-of-Flight Mass Analyzer (Q-TOF/MS) 50730.10 Fourier Transform Ion Cyclotron Resonance Mass Analyzer (FTICR/MS) 50830.11 Linear Quadrupole Ion Trap Fourier Transform Mass Analyzer (LTQ-FT/MS) 51730.12 Linear Quadrupole Ion Trap Orbitrap Mass Analyzer (LTQ-Orbitrap/MS) 51830.13 Chapter Problems 527References 52731 Biomolecule Spectral Interpretation: Small Molecules 52931.1 Introduction 52931.2 Ionization Efficiency of Lipids 52931.3 Fatty Acids 53031.4 Wax Esters 53731.5 Sterols 54231.6 Acylglycerols 54831.7 ESI-Mass Spectrometry of Phosphorylated Lipids 55131.8 Chapter Problems 556References 55732 Macromolecule Analysis 55932.1 Introduction 55932.2 Carbohydrates 55932.3 Nucleic Acids 56532.4 Chapter Problems 576References 57733 Biomolecule Spectral Interpretation: Proteins 57933.1 Introduction to Proteomics 57933.2 Protein Structure and Chemistry 57933.3 Bottom-up Proteomics: Mass Spectrometry of Peptides 58033.4 Top-Down Proteomics: Mass Spectrometry of Intact Proteins 59033.5 PTM of Proteins 59433.6 Systems Biology and Bioinformatics 61433.7 Chapter Problems 618References 619Appendix I: Chapter Problem Answers 621Appendix II: Atomic Weights and Isotopic Compositions 627Appendix III: Fundamental Physical Constants 631Appendix IV: Redox Half Reactions 633Appendix V: Periodic Table of Elements 637Appendix VI: Installing and Running Programs 639Index 641