Analytical Chemistry
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Analytical Chemistry
A Toolkit for Scientists and Laboratory Technicians
Ham, Bryan M.; MaHam, Aihui
John Wiley & Sons Inc
05/2024
688
Dura
Inglês
9781119894452
Pré-lançamento - envio 15 a 20 dias após a sua edição
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
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
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
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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