Analytical Chemistry

Analytical Chemistry

A Toolkit for Scientists and Laboratory Technicians

Ham, Bryan M.; MaHam, Aihui

John Wiley & Sons Inc

05/2024

688

Dura

Inglês

9781119894452

15 a 20 dias

666

Descrição não disponível.
About the Authors xxiii

Preface xxv

Acknowledgments xxvii

About the Companion Website xxviii

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 2

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 Safety Data Sheet (SDS) 22

3.7 Emergency Eyewash and Face Wash Stations 24

3.8 Emergency Safety Showers 25

3.9 Fire Extinguishers 25

3.10 Clothing Fire in The Laboratory 26

3.11 Spill Cleanup Kits 26

3.12 Chemicals and Solvents 27

3.13 First Aid Kits 29

3.14 Gasses and Cylinders 29

3.15 Sharps Containers and Broken Glass Boxes 30

3.16 Occupational Safety and Health Administration (OSHA) 30

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 96

4.7 Chapter Problems 96

5 Analytical Data Treatment (Statistics) 97

5.1 Errors in the Laboratory 97

5.2 Expressing Absolute and Relative Errors 98

5.3 Precision 98

5.4 The Normal Distribution Curve 98

5.5 Precision of Experimental Data 100

5.6 Normal Distribution Curve of a Sample 101

5.7 ChemTech Statistical Calculations 102

5.8 Student's Distribution t Test for Confidence Limits 105

5.9 Tests of Significance 111

5.10 Treatment of Data Outliers 112

5.11 Chapter Key Concepts 114

5.12 Chapter Problems 114

6 Plotting and Graphing 116

6.1 Introduction to Graphing 116

6.2 Graph Construction 116

6.3 Rectangular Cartesian Coordinate System 117

6.4 Curve Fitting 117

6.5 Redrawn Graph Example 117

6.6 Graphs of Equations 118

6.7 Least-Squares Method 121

6.8 Computer-Generated Curves 122

6.9 Calculating Concentrations 125

6.10 Nonlinear Curve Fitting 126

6.11 Chapter Key Concepts 130

6.12 Chapter Problems 130

7 Using Microsoft Excel (R) in the Laboratory 132

7.1 Introduction to Excel (R) 132

7.2 Opening Excel in ChemTech 132

7.3 The Excel Spreadsheet 132

7.4 Graphing in Excel 134

7.5 Complex Charting in Excel 137

7.6 Statistical Analysis using Excel 139

8 Making Laboratory Solutions 151

8.1 Introduction 151

8.2 Laboratory Reagent Fundamentals 151

8.3 The Periodic Table 151

8.4 Calculating Formula Weights 152

8.5 Calculating The Mole 152

8.6 Molecular Weight Calculator 152

8.7 Expressing Concentration 153

8.8 The Parts PER (PP) Notation 157

8.9 Computer-Based Solution Calculations 157

8.10 Reactions in Solution 161

8.11 Chapter Key Concepts 161

8.12 Chapter Problems 162

9 Acid-Base Theory and Buffer Solutions 163

9.1 Introduction 163

9.2 Acids and Bases in Everyday Life 163

9.3 The Litmus Test 163

9.4 Early Acid-Base Descriptions 164

9.5 Br?nsted-Lowry Definition 164

9.6 The Equilibrium Constant 165

9.7 The Acid Ionization Constant 165

9.8 Calculating the Hydrogen Ion Concentration 165

9.9 The Base Ionization Constant 167

9.10 Ion Product for Water 168

9.11 The Solubility Product Constant (K SP) 168

9.12 The pH of a Solution 170

9.13 Measuring the pH 171

9.14 Buffered Solutions-Description and Preparing 172

9.15 ChemTech Buffer Solution Calculator 174

9.16 Chapter Key Concepts 175

9.17 Chapter Problems 175

10 Titration-A Volumetric Method of Analysis 178

10.1 Introduction 178

10.2 Reacting Ratios 178

10.3 The Equivalence Point 179

10.4 Useful Relationships for Calculations 179

10.5 Deriving the Titration Equation 179

10.6 Titrations in ChemTech 180

10.7 Acid/Base Titration Endpoint (Equivalence Point) 181

10.8 Acid/Base Titration Midpoint 182

10.9 Acid/Base Titration Indicators 182

10.10 Titrations Using Normal Solutions 184

10.11 Polyprotic Acid Titration 184

10.12 ChemTech Calculation of Normal Titrations 185

10.13 Performing a Titration 185

10.14 Primary Standards 186

10.15 Standardization of Sodium Hydroxide 187

10.16 Conductometric Titrations (Nonaqueous Solutions) 189

10.17 Precipitation Titration (MOHR Method for Halides) 190

10.18 Complex Formation with Back Titration (Volhard Method for Anions) 191

10.19 Chapter Key Concepts 196

10.20 Chapter Problems 197

11 Oxidation-Reduction (Redox) Reactions 199

11.1 Introduction 199

11.2 Oxidation and Reduction 199

11.3 The Volt 200

11.4 The Electrochemical Cell 200

11.5 Redox Reaction Conventions 200

11.6 The Nernst Equation 202

11.7 Determining Redox Titration Endpoints 203

11.8 Potentiometric Titrations 204

11.9 Visual Indicators used in Redox Titrations 206

11.10 Pretitration Oxidation-Reduction 207

11.11 Ion-Selective Electrodes 207

11.12 Chapter Key Concepts 207

11.13 Chapter Problems 209

12 Laboratory Information Management System (LIMS) 211

12.1 Introduction 211

12.2 Lims Main Menu 211

12.3 Logging in Samples 213

12.4 Entering Test Results 213

12.5 Add or Delete Tests 214

12.6 Calculations and Curves 214

12.7 Search Wizards 215

12.8 Approving Samples 217

12.9 Printing Sample Reports 217

13 Ultraviolet and Visible (UV/VIS) Spectroscopy 227

13.1 Introduction to Spectroscopy in the Analytical Laboratory 227

13.2 The Electromagnetic Spectrum 227

13.3 Ultraviolet/Visible (UV/VIS) Spectroscopy 227

13.4 UV/Visible Spectrophotometers 236

13.5 Special Topic (Example)-Spectrophotometric Study of Dye Compounds 237

13.6 Chapter Key Concepts 240

13.7 Chapter Problems 242

14 Fluorescence Optical Emission Spectroscopy 244

14.1 Introduction to Fluorescence 244

14.2 Fluorescence and Phosphorescence Theory 245

14.3 Phosphorescence 246

14.4 Excitation and Emission Spectra 247

14.5 Rate Constants 247

14.6 Quantum Yield Rate Constants 248

14.7 Decay Lifetimes 248

14.8 Factors Affecting Fluorescence 249

14.9 Quantitative Analysis and Beer-Lambert Law 252

14.10 Quenching of Fluorescence 253

14.11 Fluorometric Instrumentation 253

14.12 Special Topic-Fluorescence Study of Dye-A007 Complexes 259

14.13 Chapter Key Concepts 261

14.14 Chapter Problems 262

15 Fourier Transform Infrared (FTIR) Spectroscopy 264

15.1 Introduction 264

15.2 Basic IR Instrument Design 264

15.3 The Infrared Spectrum and Molecular Assignment 266

15.4 FTIR Table Band Assignments 267

15.5 FTIR Spectrum Example I 273

15.6 FTIR Spectrum Example II 273

15.7 FTIR Inorganic Compound Analysis 274

15.8 Chapter Key Concepts 274

15.9 Chapter Problems 276

16 Nuclear Magnetic Resonance (NMR) Spectroscopy 280

16.1 Introduction 280

16.2 Frequency and Magnetic Field Strength 280

16.3 Continuous-Wave NMR 281

16.4 The NMR Sample Probe 282

16.5 Pulsed-Field Fourier Transform NMR 282

16.6 Proton NMR Spectra Environmental Effects 284

16.7 Carbon-13 NMR 286

16.8 Special Topic-NMR Characterization of Cholesteryl Phosphate 290

16.9 Chapter Key Concepts 295

16.10 Chapter Problems 296

References 297

17 Atomic Absorption Spectroscopy (AAS) 298

17.1 Introduction 298

17.2 Atomic Absorption and Emission Process 298

17.3 Atomic Absorption and Emission Source 299

17.4 Source Gases and Flames 299

17.5 Block Diagram of AAS Instrumentation 299

17.6 The Light Source 301

17.7 Interferences in AAS 302

17.8 Electrothermal Atomization-Graphite Furnace 302

17.9 Instrumentation 303

17.10 Flame Atomic Absorption Analytical Methods 304

18 Atomic Emission Spectroscopy 306

18.1 Introduction 306

18.2 Elements in Periodic Table 306

18.3 The Plasma Torch 306

18.4 Sample Types 307

18.5 Sample Introduction 308

18.6 ICP-OES Instrumentation 308

18.7 ICP-OES Environmental Application Example 313

19 Atomic Mass Spectrometry 328

19.1 Introduction 328

19.2 Low-Resolution ICP-MS 328

19.3 High-Resolution ICP-MS 331

20 X-Ray Fluorescence (XRF) and X-Ray Diffraction (XRD) 336

20.1 X-Ray Fluorescence Introduction 336

20.2 X-Ray Fluorescence Theory 336

20.3 Energy-Dispersive X-Ray Fluorescence (EDXRF) 337

20.4 Wavelength Dispersive X-Ray Fluorescence (WDXRF) 340

20.5 Applications of XRF 344

20.6 X-Ray Diffraction (XRD) 345

21 Chromatography-Introduction and Theory 354

21.1 Preface 354

21.2 Introduction to Chromatography 354

21.3 Theory of Chromatography 354

21.4 The Theoretical Plate Number N 358

21.5 Resolution Rs 359

21.6 Rate Theory Versus Plate Theory 360

21.7 Retention Factor k' 365

References 365

22 High-Performance Liquid Chromatography (HPLC) 366

22.1 HPLC Background 366

22.2 Design and Components of HPLC 366

23 Solid-Phase Extraction 383

23.1 Introduction 383

23.2 Disposable SPE Columns 383

23.3 SPE Vacuum Manifold 383

23.4 SPE Procedural Bulletin 383

24 Plane Chromatography: Paper and Thin-Layer Chromatography 397

24.1 Plane Chromatography 397

24.2 Thin-Layer Chromatography 398

24.3 Retardation Factor (R F) In TLC 399

24.4 Plate Heights (H) and Counts (N) In TLC 400

24.5 Retention Factor In TLC 401

25 Gas-Liquid Chromatography 402

25.1 Introduction 402

25.2 Theory and Principle of GC 402

25.3 Mobile-Phase Carrier Gasses in GC 404

25.4 Columns and Stationary Phases 405

25.5 Gas Chromatograph Injection Port 407

25.6 The GC Oven 415

25.7 GC Programming and Control 418

25.8 GC Detectors 419

26 Gas Chromatography-Mass Spectrometry (GC-MS) 422

26.1 Introduction 422

26.2 Electron Ionization (EI) 422

26.3 Electron Ionization (EI)/OE Processes 423

26.4 Oleamide Fragmentation Pathways: OE M +? by Gas Chromatography/Electron Ionization Mass Spectrometry 426

26.5 Oleamide Fragmentation Pathways: EE [M+H] + by ESI/ION Trap Mass Spectrometry 427

26.6 Quantitative Analysis by GC/EI-MS 430

26.7 Chapter Problems 432

References 434

27 Special Topics: Strong Cation Exchange Chromatography and Capillary Electrophoresis 436

27.1 Introduction 436

27.2 Strong Ion Exchange HPLC 436

27.3 Cze 436

27.4 Binding Constants by Cation Exchange and CZE 437

27.5 Comparison of Methods 446

27.6 Conclusions 449

References 449

28 Mass Spectrometry 450

28.1 Definition and Description of Mass Spectrometry 450

28.2 Basic Design of Mass Analyzer Instrumentation 450

28.3 Mass Spectrometry of Protein Metabolite and Lipid Biomolecules 452

28.4 Fundamental Studies of Biological Compound Interactions 456

28.5 Mass-to-Charge (m/z) Ratio: How the Mass Spectrometer Separates Ions 457

28.6 Exact Mass Versus Nominal Mass 459

28.7 Mass Accuracy and Resolution 460

28.8 High-Resolution Mass Measurements 462

28.9 Rings Plus Double Bonds (r+db) 464

28.10 The Nitrogen Rule in Mass Spectrometry 465

28.11 Chapter Problems 466

References 466

29 Ionization in Mass Spectrometry 468

29.1 Ionization Techniques and Sources 468

29.2 Chemical Ionization (CI) 468



29.3 Atmospheric Pressure Chemical Ionization (APCI) 472

29.4 Electrospray Ionization (ESI) 474

29.5 Nanoelectrospray Ionization (NANO-ESI) 476

29.6 Atmospheric Pressure Photoionization (APPI) 479

29.7 Matrix-Assisted Laser Desorption Ionization (MALDI) 484

29.8 Fab 486

29.9 Chapter Problems 490

References 490

30 Mass Analyzers in Mass Spectrometry 492

30.1 Mass Analyzers 492

30.2 Magnetic and Electric Sector Mass Analyzer 492

30.3 Time-of-Flight Mass Analyzer (TOF/MS) 496

30.4 Time-of-Flight/Time-of-Flight Mass Spectrometer (TOF-TOF/MS) 498

30.5 Quadrupole Mass Filter 500

30.6 Triple Quadrupole Mass Spectrometer (QQQ/MS) 503

30.7 Three-Dimensional Quadrupole Ion Trap Mass Spectrometer (QIT/MS) 504

30.8 Linear Quadrupole Ion Trap Mass Spectrometer (LTQ/MS) 506

30.9 Quadrupole Time-of-Flight Mass Spectrometer (Q-TOF/MS) 508

30.10 Fourier Transform Ion Cyclotron Resonance Mass Spectrometer (fticr/ms) 509

30.11 Linear Quadrupole Ion Trap Fourier Transform Mass Spectrometer (ltq-ft/ms) 517

30.12 Linear Quadrupole Ion Trap Orbitrap Mass Spectrometer (LTQ-Orbitrap/MS) 519

30.13 Chapter Problems 527

References 528

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 538

31.5 Sterols 542

31.6 Acylglycerols 547

31.7 Esi-Mass Spectrometry of Phosphorylated Lipids 550

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 576

33 Biomolecule Spectral Interpretation: Proteins 577

33.1 Introduction to Proteomics 577

33.2 Protein Structure and Chemistry 577

33.3 Bottom-Up Proteomics: Mass Spectrometry of Peptides 578

33.4 Top-Down Proteomics: Mass Spectrometry of Intact Proteins 588

33.5 PTM of Proteins 592

33.6 Systems Biology and Bioinformatics 610

33.7 Chapter Problems 614

References 616

Appendix I: Chapter Problem Answers 619

Appendix II: Atomic Weights and Isotopic Compositions 625

Appendix III: Fundamental Physical Constants 629

Appendix IV: Redox Half-Reactions 630

Appendix V: Periodic Table of Elements 633

Appendix VI: Installing and Running Programs 635

Index 637
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lab safety; lab glassware; lab basics; laboratory information management systems; LIMS; spectroscopy; theory of light; light absorption; chemtech; laboratory technician; chemist textbook; laboratory math; spectroscopy; instrumental analysis; statistics; chromatography; mass spectrometry; metals analysis; inorganic; organic; calibration; graphing; lab solutions; acid-base analysis; titration; wet chemistry; bench chemistry; pH; redox reactions; oxidation; reduction; UV-Vis; NMR; FTIR; gas chromatography; liquid chromatography