Analytical chemistry: a chemist and laboratory technician's toolkit
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| Main Authors: | , |
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| Format: | Book |
| Language: | English |
| Published: |
Hoboken, New Jersey
Wiley
2016
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| Subjects: | |
| Online Access: | Inhaltsverzeichnis Klappentext |
| Physical Description: | xxiv, 652 Seiten Illustrationen CD-ROM (12 cm) |
| ISBN: | 9781118714843 |
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| 245 | 1 | 0 | |a Analytical chemistry |b a chemist and laboratory technician's toolkit |c Bryan M. Ham, Aihui MaHam |
| 264 | 1 | |a Hoboken, New Jersey |b Wiley |c 2016 | |
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| adam_text | 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
1.2.1 Computers in the Laboratory, 1
1.2.2 Laboratory Information Management Systems (LIMS), 1
1.3 ChemTech—The Chemist and Technician Toolkit Companion, 1
1.3.1 Introduction to ChemTech, 1
1.3.1.1 Opening ChemTech, 2
1.3.1.2 Interactive Periodic Table, 2
1.4 Chapter Layout, 2
1.4.1 Glassware, Chemicals, and Safety, 2
1.4.2 Basic Math and Statistics, 2
1.4.3 Graphing and Plotting, 4
1.4.4 Making Laboratory Solutions, 4
1.4.5 Titrimetric Analysis, 4
1.4.6 Electrochemistry, 5
1.4.7 Laboratory Information Management System (or Software) LIMS, 5
1.4.8 Instrumental Analyses—Spectroscopy, 5
1.4.9 Instrumental Analyses—Chromatography, 5
1.4.10 Instrumental Analyses—Mass Spectrometry, 5
1.4.10.1 Mass Analyzers, 5
1.4.10.2 Mass Ionization, 5
1.4.11 Small Molecule and Macromolecule Analysis, 5
1.5 Users of ChemTech, 6
2 Introduction to the Analytical Laboratory 7
2.1 Introduction to the Laboratory, 7
2.1.1 The Scientific Method, 7
2.2 Laboratory Glassware, 7
2.2.1 Volumetric Flasks, 7
viii
CONTENTS
2.2.2 Beakers and Erlenmeyer Flasks, 7
2.2.3 Graduated Cylinders, 8
2.2.4 Pipettes, 8
2.2.4.1 Steps for Using Pipette Bulb (a), 8
2.2.4.2 Steps for Using Pipette Bulb (b and c), 10
2.2.4.3 Autopipettes, 11
2.2.5 Evaporating Dishes, 11
2.2.6 Flames and Furnaces in the Laboratory, 11
2.2.6.1 Bunsen Burners, 11
2.2.6.2 Crucibles, 11
2.2.6.3 Ashing Samples, 11
2.2.6.4 Muffle Furnaces, 14
2.2.7 Laboratory Fume Hoods, 14
2.2.8 Drying Ovens, 15
2.2.9 Balances, 15
2.2.10 Refrigerators and Freezers, 16
2.2.11 Test Tubes, 16
2.2.12 Soxhlet Extractions, 16
2.2.13 Vacuum Pumps, 18
2.3 Conclusion, 18
3 Laboratory Safety 19
3.1 Introduction, 19
3.2 Proper Personal Protection and Appropriate Attire, 19
3.2.1 Proper Eye Protection, 19
3.2.2 Proper Laboratory Coats, 20
3.3 Proper Shoes and Pants, 20
3.4 Laboratory Gloves, 20
3.4.1 Natural Rubber (Latex), 21
3.4.2 Nitrile, 22
3.4.3 Neoprene, 22
3.4.4 Butyl, 22
3.4.5 Polyvinyl Chloride (PVC), 22
3.4.6 Polyvinyl Alcohol (PVA), 22
3.4.7 Viton, 22
3.4.8 Silver Shield/4H, 22
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
3.9.1 Types of Fires, 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
4.2.1 Introduction to the Metric System, 83
4.2.2 Units of the Metric System, 83
4.2.3 Converting the SI Units, 84
4.3 Significant Figures, 84
4.3.1 Significant Figure Rules, 84
4.4 Scientific Calculators, 86
4.4.1 Example Calculator, 86
4.4.2 Window’s Calculator, 86
4.4.2.1 Windows’Scientific versus Standard Calculator, 86
4.5 ChemTech Conversion Tool, 89
4.5.1 Using the Conversion Tool, 89
4.5.2 Closing the Conversion Tool, 89
4.6 Chapter Key Concepts, 89
4.7 Chapter Problems, 92
5 Analytical Data Treatment (Statistics)
5.1 Errors in the Laboratory, 93
5.1.1 Systematic Errors, 93
5.1.2 Random Errors, 93
5.2 Expressing Absolute and Relative Errors, 94
5.3 Precision, 94
5.3.1 Precision versus Accuracy, 94
5.4 The Norma! Distribution Curve, 94
5.4.1 Central Tendency of Data, 95
5.4.1.1 The Arithmetic Mean, 95
5.4.1.2 The Median, 95
5.4.1.3 The Mode, 95
5.4.1.4 Sticking with the Mean, 95
5.5 Precision of Experimental Data, 96
5.5.1 The Range, 96
5.5.2 The Average Deviation, 96
5.5.3 The Standard Deviation, 97
5.5.3.1 Root Mean Square, 97
5.5.3.2 Sample Standard Deviation, 97
5.5.3.3 Comparison of the Three Methods, 97
5.5.3.4 Using the Scientific Calculator, 97
5.5.3.5 Coefficient of Variation, 97
5.6 Normal Distribution Curve of a Sample, 97
5.7 ChemTech Statistical Calculations, 98
5.7.3 Introduction to ChemTech Statistics, 98
5.7.2 ChemTech Chapter 5, 98
5.7.2.1 Entering Data, 100
5.7.2.2 Calculating the Statistics, 100
5.7.2.3 The Results Output, 100
5.7.2.4 Results not Expected, 100
5.7.2.5 Using ChemTech for Large Value Set, 101
5.7.2.6 The Results Page, 101
5.7.2.7 Resetting the Page, 101
5.8 Student’s Distribution t Test for Confidence Limits, 101
5.8.1 Accuracy, 101
5.8.2 The Student’s t Test, 102
5.8.3 Calculating the Student’s t Value, 102
5.8.4 Probability Level, 103
5.8.5 Sulfate Concentration Confidence Limits, 103
5.8.6 Sulfate t Distribution Curve, 103
5.8.7 Determining Types of Error, 103
5.8.7.1 Glucose Content, 104
5.8.8 Determining Error in Methodology, 104
5.8.8.1 Magnesium Primary Standard, 104
X
CONTENTS
5.9 Tests of Significance, 104
5.9.1 Difference in Means, 104
5.9.2 Null Hypothesis, 105
5.10 Treatment of Data Outliers, 105
5.10.1 The Q Test, 105
5.10.2 The Tn Test, 106
5.11 Chapter Key Concepts, 106
5.12 Chapter Problems, 107
6 Plotting and Graphing
6.1 Introduction to Graphing, 109
6.1.1 The Invention of the Graph, 109
6.1.2 Importance of Graphing, 109
6.2 Graph Construction, 109
6.2.1 Axis and Quadrants, 110
6.3 Rectangular Cartesian Coordinate System, 110
6.4 Curve Fitting, 110
6.5 Redrawn Graph Example, 110
6.6 Graphs of Equations, 111
6.6.1 Introduction, 111
6.6.2 Copper Sulfate Data, 111
6.6.3 Plotting the Data, 111
6.6.4 Best Fit Line, 111
6.6.5 Point-Slope Equation of a Line, 112
6.6.6 Finding the Slope (m), 112
6.6.7 Finding the y-Intercept (b 112
6.6.8 Solving for x, 113
6.6.9 Estimating the Slope and Intercept, 113
6.6.10 Deriving the Equation from the Slope and Intercept, 113
6.7 Least-Squares Method, 114
6.7.1 Plotting Data with Scatter, 114
6.7.2 Linear Regression, 114
6.7.3 Curve Fitting the Data, 114
6.8 Computer-Generated Curves, 115
6.8.1 Using ChemTech to Plot Data, 115
6.8.2 Entering the Data, 115
6.8.3 Plotting the Data, 116
6.8.4 Linear Regression of the Data, 116
6.8.5 Adding the Best Fit Line, 118
6.8.6 Entering a Large Set of Data, 118
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
7.1 Introduction to Excel®, 125
7.2 Opening Excel® in ChemTech, 125
7.3 The Excel® Spreadsheet, 125
7.3.1 Spreadsheet Menus and Quick Access Toolbars, 127
7.4 Graphing in Excel®, 127
7.4.1 Making Column Headings, 127
7.4.2 Entering Data into Columns, 128
7.4.3 Saving the Spreadsheet, 129
7.4.4 Constructing the Graph, 129
7.4.5 The Chart Wizard, 130
109
125
7.4.6 The Chart Source Data, 130
7.4.7 Chart Options, 131
7.5 Charts in Excel0* 2010, 132
7.6 Complex Charting in Excel05 97-2003, 132
7.6.1 Calcium Atomic Absorption (AAS) Data, 132
7.6.2 Entering Ca Data into Spreadsheet. 135
7.6.3 Average and Standard Deviation, 135
7.6.4 Constructing the Calibration Curve, 135
7.6.5 Entering the Chart Options, 136
7.6.6 Error Bars, 137
7.6.7 Trendline, 138
7.7 Complex Charting in Excel09 2010, 139
7.7.1 Entering the Data, 139
7.7.2 Using the Formula Search Function, 139
7.7.3 Inserting the Chart, 140
7.7.4 Formatting the Chart, 140
7.8 Statistical Analysis Using Excel00, 141
7.8.1 Open and Save Excel00 StatExp.xls, 141
7.8.2 Sulfate Data, 141
7.8.3 Excel00 Confidence Function, 142
7.8.4 Excel00 Student’s / Test, 142
7.8.4.1 Spreadsheet Calculation I, 142
7.8.4.2 Spreadsheet Calculation II, 143
7.8.5 Excel00 Tools Data Analysis. 143
7.8.5.1 Analysis ToolPak, 143
7.8.5.2 ToolPak Functions, 143
7.8.5.3 Data Analysis /-Test: Two-Sample Assuming Unequal
Variances, 144
7.8.5.4 Analysis ToolPak F-test, 145
7.8.5.5 Analysis ToolPak Statistical Summary, 145
Making Laboratory Solutions
8.1 Introduction. 147
8.2 Laboratory Reagent Fundamentals, 147
8.3 The Periodic Table, 147
8.3.1 Periodic Table Descriptive Windows, 148
8.4 Calculating Formula Weights, 148
8.5 Calculating the Mole, 148
8.6 Molecular Weight Calculator, 148
8.7 Expressing Concentration, 148
8.7.1 Formal (F) Solutions, 149
8.7.1.1 Formal (F) Solution Example, 149
8.7.2 Molal (m) Solutions, 149
8.7.2.1 Molal (m) Solution—Simple Example, 149
8.7.2.2 Molal (m) Solution—Complex Example. 149
8.7.3 Molar (M) Solutions, 150
8.7.3.1 Molar (Af) Solution Example, 150
8.7.3.2 Molar (M) Solution of K2CO3, 151
8.7.4 Normal (N) Solutions. 151
8.7.4.1 Normal (AO Solution Calculation Example. 152
8.8 The Parts per (PP) Notation, 153
8.9 Computer-Based Solution Calculations, 153
8.9.1 Computer-Based Concentration Calculation—Molarity I, 154
8.9.2 Computer-Based Concentration Calculation—Molarity II, 154
8.9.3 Computer-Based Concentration Calculation—Normality I, 155
8.9.4 Computer-Based Concentration Calculation—Normality II, 156
xii
CONTENTS
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 Brdnsted-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
9.9.1 OH- Ion Concentration Example, 163
9.9.2 Percent Ionization Example, 164
9.10 Ion Product for Water, 164
9.11 The Solubility Product Constant (Ksp), 164
9.11.1 Solubility of Silver(I) Thiocyanate, 164
9.11.2 Solubility of Lithium Carbonate, 166
9.12 The pH of a Solution, 166
9.13 Measuring the pH, 167
9.13.1 The Glass Electrode, 167
9.14 Buffered Solutions—Description and Preparing, 168
9.14.1 Le Chatelier’s Principle, 169
9.14.2 Titration Curve of a Buffer, 169
9.14.3 Natural Buffer Solutions, 169
9.14.4 Calculating Buffer pH, 170
9.14.5 Buffer pH Calculation I, 170
9.15 ChemTech Buffer Solution Calculator, 170
9.16 Chapter Key Concepts, 3 71
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
10.5.1 Titration Calculation Example, 176
10.6 Titrations in ChemTech, 177
10.6.1 Acid/Base Titrations Using Molar Solutions, 177
10.6.2 Titration Calculation Example, 177
10.7 Acid/Base Titration Endpoint (Equivalence Point), 178
10.8 Acid/Base Titration Midpoint, 179
10.9 Acid/Base Titration Indicators, 180
10.9.1 The Ideal Indicator, 180
10.10 Titrations Using Normal Solutions, 181
10.10.1 Normal Solution Titration Example, 181
10.11 Polyprotic Acid Titration, 181
10.12 ChemTech Calculation of Normal Titrations, 182
10.13 Performing a Titration, 183
10.13.1 Titration Glassware, 183
10.13.2 Titration Steps, 183
10.14 Primary Standards, 184
10.15 Standardization of Sodium Hydroxide, 185
10.15.1 NaOH Titrant Standardization Example, 185
10.16 Conductometric Titrations (Nonaqueous Solutions), 186
10.17 Precipitation Titration (Mohr Method for Halides), 188
10.17.1 Basic Steps in Titration, 188
10.17.2 Important Considerations, 189
10.18 Complex Formation with Back Titration
(Volhard Method for Anions), 189
10.18.1 Iron(III) as Indicator, 189
10.18.2 Chloride Titration, 189
10.18.3 The General Calculation, 189
10.18.4 Chloride Titration, 190
10.18.4.1 Volhard Chloride
Analysis Example, 190
10.18.4.2 The Titration Steps, 190
10.19 Complex Formation Titration with EDTA for Cations, 190
10.19.1 EDTA-Metal Ion Complex Formation, 191
10.19.2 The Stability Constant, 191
10.J9.3 Metal Ions Titrated, 191
10.19.4 Influence of pH, 191
10.19.5 Buffer and Hydroxide Complexation, 192
10.19.6 Visual Indicators, 193
10.20 Chapter Key Concepts, 194
10.21 Chapter Problems, 195
11 Oxidation-Reduction (Redox) Reactions
11.1 Introduction, 197
11.2 Oxidation and Reduction, 197
11.3 The Volt, 198
11A The Electrochemical Cell, 198
11.5 Redox Reaction Conventions, 198
11.5.1 Electrode Potential Tables, 198
11.5.2 The Standard Hydrogen Electrode (SHE), 199
11.5.3 The SHE Half-Reaction, 199
11.5.4 Writing the Standard Electrode Potentials, 199
11.5.5 Drawing a Galvanic Cell, 199
11.5.6 Calculating the Cell Potential, 200
11.5.6.1 Iron and Zinc Cell, 200
11.5.6.2 Nickel and Silver Cell, 200
11.6 The Nemst Equation, 200
11.6.1 Nemst Equation Example I, 201
11.6.2 Nemst Equation Example II, 201
11.6.3 Nemst Equation Example III, 201
11.7 Determining Redox Titration Endpoints, 202
11.8 Potentiometric Titrations, 202
11.8.1 Detailed Potentiometer, 202
11.8.2 Half-Reactions, 202
11.8.3 The Nemst Equation, 203
11.8.4 Assumed Reaction Completion, 203
11.8.5 Calculated Potentials of Ce4+, 204
11.9 Visual Indicators Used in Redox Titrations, 204
11.10 Pretitration Oxidation-Reduction, 205
11.10.1 Reducing Agents, 205
11.10.2 Oxidizing Agents, 205
11.11 Ion-Selective Electrodes, 206
xiv
CONTENTS
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
12.7.1 Searching Archived Samples, 214
12.7.2 General Search, 214
12.7.3 Viewing Current Open Samples, 216
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
13.3.1 Wave and Particle Theory of Light, 222
13.3.2 Light Absorption Transitions, 223
13.3.3 The Color Wheel, 224
13.3.4 Pigments, 224
13.3.5 Inorganic Elemental Analysis, 224
13.3.6 The Azo Dyes, 225
13.3.7 UV-Visible Absorption Spectra, 228
13.3.8 Beer’s Law, 228
13.4 UV/Visible Spectrophotometers, 230
13.5 Special Topic (Example)—Spectrophotometric Study of Dye Compounds, 234
13.5.1 Introduction, 234
13.5.2 Experimental Setup for Special Topic Discussion, 235
13.5.3 UV/Vis Study of the Compounds and Complexes, 235
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
14.2.1 Radiant Energy Absorption, 240
14.2.2 Fluorescence Principle—Jabloriski Diagram, 240
14.2.3 Excitation and Electron Spin States, 240
14.2.3.1 Quantum Numbers, 241
14.2.3.2 Electron Spin States, 241
14.3 Phosphorescence, 241
14.4 Excitation and Emission Spectra, 242
14.5 Rate Constants, 243
14.5.1 Emission Times, 243
14.5.2 Relative Rate Constants (k), 243
14.6 Quantum Yield Rate Constants, 243
14.7 Decay Lifetimes, 244
14.8 Factors Affecting Fluorescence, 244
14.8.1 Excitation Wavelength (Instrumental), 244
14.8.2 Light Source (Instrumental), 244
14.8.3 Filters, Optics, and Detectors (Instrumental), 245
CONTENTS xv
14.8.4 Cuvettes and Cells (Instrumental), 245
14.8.5 Structure (Sample), 246
14.8.5.1 Fluorescein and Beta-(ß)-Carotene, 246
14.8.5.2 Diatomic Oxygen Molecular Orbital Diagram, 246
14.8.5.3 Examples of Nonfluorescent and Fluorescent Compounds, 247
14.8.5.4 Other Structural Influences, 247
14.8.5.5 Scattering (Sample), 248
14.9 Quantitative Analysis and Beer-Lambert Law, 248
14.10 Quenching of Fluorescence, 249
14.11 Fluorometric Instrumentation, 249
14.11.1 Spectrofluorometer, 249
14.11.1.1 Light Source, 250
14.11.1.2 Monochromators, 250
14.11.1.3 Photomultiplier tube (PMT), 251
14.11.2 Multidetection Microplate Reader, 252
14.11.3 Digital Fluorescence Microscopy, 252
14.11.3.1 Light Source, 252
14.11.3.2 Filter Cube, 253
14.11.3.3 Objectives and Grating, 253
14.11.3.4 Charged-Coupled Device (CCD), 254
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
16.6.1 Chemical Shift, 281
16.6.2 Spin-Spin Splitting (Coupling), 281
16.6.3 Interpretation of NMR Spectra, 283
16.6.3.1 2-Amino-3-Methyl-Pentanoic Acid, 283
16.6.3.2 Unknown I, 283
16.7 Carbon-13 NMR, 283
16.7.1 Introduction, 283
16.7.2 Carbon-13 Chemical Shift, 284
16.7.3 Carbon-13 Splitting, 286
16.7.4 Finding the Number of Carbons, 286
16.7.5 Carbon-13 NMR Examples, 286
16.8 Special Topic—NMR Characterization of Cholesteryl Phosphate, 287
16.8.1 Synthesis of Cholesteryl Phosphate, 288
16.8.2 Single-Stage and High-Resolution Mass Spectrometry, 288
16.8.3 Proton Nuclear Magnetic Resonance (’H-NMR), 289
XVI
CONTENTS
16.8.4 Theoretical NMR Spectroscopy, 289
16.8.5 Structure Elucidation, 289
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
18.6.1 Radially Viewed System, 306
18.6.2 Axially Viewed System, 308
18.6.3 Ergonomic Sample Introduction System, 309
18.6.4 Innovative Optical Design, 310
18.6.5 Advanced CID Camera Technology, 310
18.7 ICP-OES Environmental Application Example, 310
19 Atomic Mass Spectrometry 325
19.1 Introduction, 325
19.2 Low-Resolution ICP-MS, 325
19.2.1 The PerkinElmer NexION® 350 ICP-MS, 325
19.2.2 Interface and Quadrupole Ion Deflector (QID), 325
19.2.3 The Collision/Reaction Cell, 325
19.2.4 Quadrupole Mass Filter, 328
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
20.3.1 EDXRF Instrumentation, 334
20.3.1.1 Basic Components, 334
20.3.1.2 X-Ray Sources, 334
20.3.1.3 Detectors, 335
20.3.2 Commercial Instrumentation, 337
20.4 Wavelength Dispersive X-Ray Fluorescence (WDXRF), 337
20.4.1 Introduction, 337
20.4.2 WDXRF Instrumentation, 338
20.4.2.1 Simultaneous WDXRF Instrumentation, 338
20.4.2.2 Sequential WDXRF Instrumentation, 340
20.5 Applications of XRF, 341
20.6 X-ray Diffraction (XRD), 342
20.6.1 Introduction, 342
20.6.2 X-Ray Crystallography, 344
20.6.3 Bragg’s Law, 345
20.6.4 Diffraction Patterns, 345
20.6.5 The Goniometer, 346
20.6.6 XRD Spectra, 346
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 V, 355
21.5 Resolution/^, 356
21.6 Rate Theory versus Plate Theory, 357
21.6.1 Multiple Flow Paths or Eddy Diffusion (A Coefficient), 358
21.6.2 Longitudinal (Molecular) Diffusion (B Coefficient), 359
21.6.3 Mass Transfer Resistance between Phases (Cs and Cm Coefficients), 361
21.7 Retention Factor ¡d, 361
References, 362
22 High Performance Liquid Chromatography (HPLC) 363
22.1 HPLC Background, 363
22.2 Design and Components of HPLC, 363
22.2.1 HPLC Pump, 366
22.2.2 HPLC Columns, 368
22.2.2.1 HPLC Column Stationary Phases, 368
22.2.3 HPLC Detectors, 372
22.2.4 HPLC Fraction Collector, 374
22.2.5 Current Commercially Available HPLC Systems, 375
22.2.6 Example of HPLC Analyses, 375
22.2.6.1 HPLC Analysis of Acidic Pesticides, 375
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
24.3.1 Example I, 398
24.3.2 Example II, 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
25.5.1 Injection Port Septa, 407
25.5.1.1 Merlin Microseal, 407
xviii
CONTENTS
25.5.2 Injection Port Sleeve (Liner), 408
25.5.2.1 Attributes of a Proper Liner, 409
25.5.3 Injection Port Flows, 412
25.5.4 Packed Column Injection Port, 412
25.5.5 Capillary Column Split Injection Port, 414
25.5.6 Capillary Column Splitless Injection Port, 414
25.6 The GC Oven, 415
25.7 GC Programming and Control, 417
25.8 GC Detectors, 418
25.8.1 Flame Ionization Detector (FID), 418
25.8.2 Electron Capture Detector (ECD), 418
25.8.3 Flame Photometric Detector (FPD), 419
25.8.4 Nitrogen Phosphorus Detector (NPD), 419
25.8.5 Thermal Conductivity Detector (TCD), 420
26 Gas Chromatography-Mass Spectrometry (GC-MS) 421
26.1 Introduction, 421
26.2 Electron Ionization (El), 421
26.3 Electron Ionization (EI)/OE Processes, 422
26.4 Oleamide Fragmentation Pathways: OE 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
27.1.1 Overview and Comparison of HPLC and CZE, 435
27.2 Strong Ion Exchange HPLC, 435
27.3 CZE, 435
27.3.1 Electroosmotic Flow (EOF), 436
27.3.2 Applications of CZE, 436
27.4 Binding Constants by Cation Exchange and CZE, 436
27.4.1 Ranking of Binding Constants, 436
27.4.2 Experimental Setup, 436
27.4.3 UV/Vis Study of the Compounds and Complexes, 437
27.4.4 Fluorescence Study of the Dye/A007 Complexes, 438
27.4.5 Computer Modeling of the Complex, 438
27.4.6 Cation Exchange Liquid Chromatography Results, 440
27.4.6.1 Description of HPLC Pseudophase, 441
27.4.7 Capillary Electrophoresis (CE), 441
27.4.7.1 Introduction, 441
27.4.7.2 CE Instrumentation, 441
27.4.7.3 Theory of CE Separation, 441
27.4.7.4 Results of CE Binding Analysis
of Dyes and A007, 441
27.4.7.5 Electropherograms of Dye/A007 Complexes, 446
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
28.3.1 Proteomics, 451
28.3.2 Metabolomics, 452
28.3.3 Lipidomics, 454
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 (Cl), 467
29.2.1 Positive Cl, 468
29.2.2 Negative Cl, 470
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
29.6.1 APPI Mechanism, 478
29.6.2 APPI VUV Lamps, 478
29.6.3 APPI Sources, 478
29.6.4 Comparison of ESI and APPI, 479
29.7 Matrix Assisted Laser Desorption Ionization (MALDI), 483
29.8 FAB, 485
29.8.1 Application of FAB versus El, 487
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-FIight/Time-of-FIight 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
30.10.1 Introduction, 508
30.10.2 FTICR Mass Analyzer, 509
30.10.3 FTICR Trapped Ion Behavior, 509
30.10.4 Cyclotron and Magnetron Ion Motion, 515
30.10.5 Basic Experimental Sequence, 515
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
XX
CONTENTS
31.3
31.4
31.5
Fatty Acids, 530
31.3.1 Negative Ion Mode Electrospray Behavior of Fatty Acids, 532
Wax Esters, 537
31.4.1 Oxidized Wax Esters, 538
31.4.2 Oxidation of Monounsaturated Wax Esters by Fenton Reaction, 538
Sterols, 542
31.5.1 Synthesis of Cholesteryl Phosphate, 542
31.5.2 Single-Stage and High-Resolution Mass Spectrometry, 543
31.5.3 Proton Nuclear Magnetic Resonance (*H-NMR), 543
31.5.4 Theoretical NMR Spectroscopy, 544
31.5.5 Structure Elucidation, 544
31.6 Acylglycerols, 548
31.6.1 Analysis of Monopentadecanoin, 548
31.6.2 Analysis of 1,3-Dipentadecanoin, 548
31.6.3 Analysis of Triheptadecanoin, 550
31.7 ESI-Mass Spectrometry of Phosphorylated Lipids, 551
31.7.1 Electrospray Ionization Behavior of Phosphorylated Lipids, 551
31.7.2 Positive Ion Mode ESI of Phosphorylated Lipids, 553
31.7.3 Negative Ion Mode ESI of Phosphorylated Lipids, 556
31.8 Chapter Problems, 556
References, 557
32 Macromolecule Analysis 559
32.1 Introduction, 559
32.2 Carbohydrates, 559
32.2.1 Ionization of Oligosaccharides, 561
32.2.2 Carbohydrate Fragmentation, 561
32.2.3 Complex Oligosaccharide Structural Elucidation, 564
32.3 Nucleic Acids, 565
32.3.1 Negative Ion Mode ESI of a Yeast 76-mer tRNAPhe, 569
32.3.2 Positive Ion Mode MALDI Analysis, 573
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
33.3.1 History and Strategy, 580
33.3.2 Protein Identification through Product Ion Spectra, 584
33.3.3 High-Energy Product Ions, 587
33.3.4 De Novo Sequencing, 587
33.3.5 Electron Capture Dissociation, 589
33.4 Top-Down Proteomics: Mass Spectrometry of Intact Proteins, 590
33.4.1 Background, 590
33.4.2 GP Basicity and Protein Charging, 591
33.4.3 Calculation of Charge State and Molecular Weight, 592
33.4.4 Top-Down Protein Sequencing, 593
33.5 PTM of Proteins, 594
33.5.1 Three Main Types of PTM, 594
33.5.2 Glycosylation of Proteins, 594
33.5.3 Phosphorylation of Proteins, 596
33.5.3.1 Phosphohistidine as PTM, 602
33.5.4 Sulfation of Proteins, 608
33.5.4.1 Glycosaminoglycan Sulfation, 608
33.5.4.2 Tyrosine Sulfation, 609
CONTENTS
xxi
33.6 Systems Biology and Bioinformatics, 614
33.6.1 Biomarkers in Cancer, 616
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
A comprehensive study of analytical chemistry providing the basics of analytical
chemistry and introductions to the laboratory
Analytical Chemistry: A Chemist and Laboratory Technician s Toolkit provides an introduction to the laboratory
including safety and lab basics, and then moves through the fundamentals of analytical techniques such as
spectroscopy and chromatography, most common lab instrumentation, and examples of laboratory programs
such as laboratory information management systems (UMS).
Also included is a teaching companion, reference, and toolkit program called ChemTech.The ChemTech program
contains lesson exercises that stress and review topics covered in the book. Also included are useful calculators,
an interactive periodic table, and a copy of all of the chapters of the book that can be opened and read on a
computer or other electronic devices.
Analytical Chemistry features:
The basics of a chemistry lab including lab safety, glassware, and common instrumentation
Fundamentals of analytical techniques such as wet chemistry, instrumental analyses, spectroscopy,
chromatography, FTIR, NMR, XRF, XRD, HPLC, GC-MS, Capillary Electrophoresis, and proteomics
ChemTech an interactive program that contains lesson exercises, useful calculators and an interactive periodic
table
A very useful computer program UMS is used to input data, track sample progress, record sample data such
as company, type, and tests needed and so forth. A chapter on UMS provides examples for logging in samples,
inputting data, searching samples, approving samples, and printing reports and Certificates of Analysis (C of A).
The ChemTech program is a teaching tool designed to equip the chemist, the laboratory analyst, and the technician
for a career in the analytical laboratory whether it is a clinical lab, an industrial, petrochemical, petroleum,
environmental, college or university, or contract lab.
The book is a core reference for chemists, lab technicians, undergraduate students studying the sciences, an
undergraduate analytical chemistry class, or a graduate analytical chemistry class. Also a vital tool for the
method developer and researcher who are interested in areas of analytical chemistry not familiar with including
academic groups, pharmaceutical companies, contract labs, environmental labs, petrochemical and polymer
industry, and the health care industry.
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 SpectrometryTechniques (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.
www.wiley.com
Wiley
Also available
as an e-book
Cover Image: Courtesy of
Bryan M. Ham Aihui MaHam
|
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| dewey-search | 543 |
| dewey-sort | 3543 |
| dewey-tens | 540 - Chemistry and allied sciences |
| discipline | Chemie / Pharmazie |
| format | Book |
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| title | Analytical chemistry a chemist and laboratory technician's toolkit |
| title_auth | Analytical chemistry a chemist and laboratory technician's toolkit |
| title_exact_search | Analytical chemistry a chemist and laboratory technician's toolkit |
| title_full | Analytical chemistry a chemist and laboratory technician's toolkit Bryan M. Ham, Aihui MaHam |
| title_fullStr | Analytical chemistry a chemist and laboratory technician's toolkit Bryan M. Ham, Aihui MaHam |
| title_full_unstemmed | Analytical chemistry a chemist and laboratory technician's toolkit Bryan M. Ham, Aihui MaHam |
| title_short | Analytical chemistry |
| title_sort | analytical chemistry a chemist and laboratory technician s toolkit |
| title_sub | a chemist and laboratory technician's toolkit |
| topic | Chemistry, Analytic Handbooks, manuals, etc Analytische Chemie (DE-588)4129906-1 gnd |
| topic_facet | Chemistry, Analytic Handbooks, manuals, etc Analytische Chemie Anleitung |
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