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Copyright, iv
Preface, vii
Chapter 1. SAFETY FIRST, LAST, AND ALWAYS, 1
Accidents Will Not Happen, 5
Disposing of Waste, 5
Mixed Waste, 7
Chapter 2. KEEPING A NOTEBOOK, 9
A Technique Experiment, 10
Notebook Notes, 11
A Synthesis Experiment, 11
Notebook Notes, 11
Calculation of Percent Yield (Not Yeild!), 21
Estimation Is Your Friend, 23
The Acid Test, 23
Notebook Mortal Sin, 24
Chapter 3. INTERPRETING A HANDBOOK, 25
CRC Handbook, 26
Entry: 1-Bromobutane, 26
Entry: Benzoic Acid, 28
Lange’s, 28
Entry: 1-Bromobutane, 29
Entry: Benzoic Acid, 29
Merck Index, 30
Entry: 1-Bromobutane, 30
Entry: Benzoic Acid, 32
The Aldrich Catalog, 32
Entry: 1-Bromobutane, 33
Entry: Benzoic Acid, 34
MSDS: Material Safety Data Sheet, 34
Not Clear–Clear?, 35
Info on the Internet, 35
Chapter 4. JOINTWARE, 37
Stoppers With Only One Number, 38
Another Episode of Love of Laboratory, 39
Hall of Blunders and Things Not Quite Right, 41
Round-Bottom Flasks, 41
Columns and Condensers, 42
The Adapter with Lots of Names, 42
Forgetting the Glass, 44
Inserting Adapter Upside Down, 45
Inserting Adapter Upside Down sans Glass, 45
Greasing the Joints, 45
To Grease or Not to Grease, 45
Preparation of the Joints, 46
Into the Grease Pit, 46
Storing Stuff and Sticking Stoppers, 47
Corking a Vessel, 47
The Cork Press, 49
The O-Ring and Cap Branch Out, 49
Chapter 5. MICROSCALE JOINTWARE, 50
Microscale: A Few Words, 51
Uh-Oh Rings, 51
The O-Ring Cap Seal, 51
Sizing Up the Situation, 52
Why I Don’t Really Know How Vacuum Tight These Seals Are, 54
The Comical Vial (That’s Conical!), 54
The Conical Vial as Vial, 55
Packaging Oops, 55
Tare to the Analytical Balance, 55
The Electronic Analytical Balance, 56
Heating These Vials, 56
The Microscale Drying Tube, 57
Gas Collection Apparatus, 58
Generating the Gas, 59
Isolating the Product, 61
Chapter 6. OTHER INTERESTING EQUIPMENT, 62
Funnels, and Beakers, and Flasks—Oh My!, 64
The Flexible Double-Ended Stainless Steel Spatula, 64
Chapter 7. PIPET TIPS, 66
Pre-preparing Pasteur Pipets, 67
Calibration, 68
Operation, 68
Amelioration, 68
Pipet Cutting, 70
Pipet Filtering—Liquids, 70
Pipet Filtering—Solids, 71
Chapter 8. SYRINGES, NEEDLES, AND SEPTA, 73
The Rubber Septum, 76
Chapter 9. CLEAN AND DRY, 77
Drying Your Glassware When You Don’t Need To, 78
Drying Your Glassware When You Do Need To, 79
Chapter 10. DRYING AGENTS, 80
Typical Drying Agents, 81
Using a Drying Agent, 82
Following Directions and Losing Product Anyway, 82
Drying Agents: Microscale, 82
Drying in Stages: The Capacity and Efficiency of Drying Agents, 83
Chapter 11. ON PRODUCTS, 84
Solid Product Problems, 85
Liquid Product Problems, 85
The Sample Vial, 85
Hold It! Don’t Touch That Vial, 86
Chapter 12. THE MELTING-POINT EXPERIMENT, 87
Sample Preparation, 88
Loading the Melting-Point Tube, 89
Closing Off Melting-Point Tubes, 90
Melting-Point Hints, 90
The Mel-Temp Apparatus, 91
Operation of the Mel-Temp Apparatus, 92
The Fisher-Johns Apparatus, 93
Operation of the Fisher-Johns Apparatus, 94
The Thomas-Hoover Apparatus, 95
Operation of the Thomas-Hoover Apparatus, 97
Using the Thiele Tube, 99
Cleaning the Tube, 100
Getting the Sample Ready, 101
Dunking the Melting-Point Tube, 102
Heating the Sample, 103
Chapter 13. RECRYSTALLIZATION, 104
Finding a Good Solvent, 105
General Guidelines for a Recrystallization, 106
Gravity Filtration, 107
The Buchner Funnel and Filter Flask, 110
Just a Note, 113
The Hirsch Funnel and Friends, 113
Activated Charcoal, 114
The Water Aspirator: A Vacuum Source, 114
The Water Trap, 115
Working with a Mixed-Solvent System—The Good Part, 115
The Ethanol–Water System, 116
A Mixed-Solvent System—The Bad Part, 116
Salting Out, 117
World Famous Fan-Folded Fluted Paper, 118
Chapter 14. RECRYSTALLIZATION: MICROSCALE, 120
Isolating the Crystals, 121
Craig Tube Filtration, 122
Centrifuging the Craig Tube, 124
Getting the Crystals Out, 125
Chapter 15. EXTRACTION AND WASHING, 127
Never-Ever Land, 128
Starting an Extraction, 129
Dutch Uncle Advice, 130
The Separatory Funnel, 131
The Stopper, 131
The Glass Stopcock, 131
The Teflon Stopcock, 132
How to Extract and Wash What, 134
The Road to Recovery—Back-Extraction, 135
A Sample Extraction, 136
Performing an Extraction or Washing, 137
Extraction Hints, 139
Chapter 16. EXTRACTION AND WASHING: MICROSCALE, 141
Mixing, 142
Separation: Removing the Bottom Layer, 142
Separation: Removing the Top Layer, 143
Separation: Removing Both Layers, 144
Chapter 17. AND NOW—BOILING STONES, 145
Chapter 18. SOURCES OF HEAT, 147
The Steam Bath, 148
The Bunsen Burner, 149
Burner Hints, 150
The Heating Mantle, 150
Proportional Heaters and Stepless Controllers, 153
Chapter 19. CLAMPS AND CLAMPING, 156
Clamping a Distillation Setup, 159
Clipping a Distillation Setup, 163
Chapter 20. DISTILLATION, 166
Distillation Notes, 167
Class 1: Simple Distillation, 168
Sources of Heat, 168
The Three-Way Adapter, 169
The Distilling Flask, 169
The Thermometer Adapter, 170
The Ubiquitous Clamp, 170
The Thermometer, 170
The Condenser, 170
The Vacuum Adapter, 170
The Receiving Flask, 171
The Ice Bath, 171
The Distillation Example, 171
The Distillation Mistake, 172
Class 2: Vacuum Distillation, 172
Pressure Measurement, 173
Manometer Hints, 175
Leaks, 175
Pressure and Temperature Corrections, 175
Vacuum Distillation Notes, 179
Class 3: Fractional Distillation, 180
How This Works, 180
Fractional Distillation Notes, 182
Azeotropes, 185
Class 4: Steam Distillation, 186
External Steam Distillation, 186
Internal Steam Distillation, 187
Steam Distillation Notes, 188
Simulated Bulb-to-Bulb Distillation: Fakelrohr, 191
Chapter 21. MICROSCALE DISTILLATION, 192
Like the Big Guy, 193
Class 1: Simple Distillation, 193
Class 2: Vacuum Distillation, 193
Class 3: Fractional Distillation, 193
Class 4: Steam Distillation, 193
Microscale Distillation II: The Hickman Still, 194
The Hickman Still Setup, 194
Hickman Still Heating, 195
Recovering Your Product, 195
Chapter 22. THE ROTARY EVAPORATOR, 197
Chapter 23. REFLUX AND ADDITION, 202
Standard Reflux, 203
A Dry Reflux, 204
Addition and Reflux, 206
Funnel Fun, 206
How to Set Up, 207
Chapter 24. REFLUX: MICROSCALE, 210
Addition and Reflux: Microscale, 211
Chapter 25. SUBLIMINATION, 213
Chapter 26. MICROSCALE BOILING POINT, 216
Microscale Boiling Point, 217
Ultramicroscale Boiling Point, 218
Chapter 27. CHROMATOGRAPHY: SOME GENERALITIES, 220
Adsorbents, 221
Separation or Development, 221
The Eluatropic Series, 221
Chapter 28. THIN-LAYER CHROMATOGRAPHY: TLC, 224
Preparation of TLC Plates, 225
Pre-prepared TLC Plates, 226
The Plate Spotter, 226
Spotting the Plates, 227
Developing a Plate, 228
Visualization, 230
Interpretation, 231
Multiple Spotting, 233
Cospotting, 233
Other TLC Problems, 235
Preparative TLC, 235
Chapter 29. WET-COLUMN CHROMATOGRAPHY, 238
Preparing the Column, 239
Compounds on the Column, 241
Visualization and Collection, 242
Wet-Column Chromatography: Microscale, 243
Flash Chromatography, 245
Microscale Flash Chromatography, 245
Chapter 30. REFRACTOMETRY, 246
The Abbé Refractometer, 247
Before Using the Abbé Refractometer: A Little Practice, 249
Using the Abbé Refractometer, 249
Refractometry Hints, 251
Chapter 31. INSTRUMENTATION IN THE LAB, 252
Chapter 32. GAS CHROMATOGRAPHY, 254
The Mobile Phase: Gas, 255
GC Sample Preparation, 256
GC Sample Introduction, 256
Sample in the Column, 258
Sample at the Detector, 258
Electronic Interlude, 260
Sample on the Chart Recorder, 261
Sample on the Computer Recorder, 262
Parameters, Parameters, 262
Gas Flow Rate, 262
Temperature, 262
Chapter 33. HP LIQUID CHROMATOGRAPHY, 264
The Mobile Phase: Liquid, 265
A Bubble Trap, 265
The Pump, 267
The Pulse Dampener, 268
HPLC Sample Preparation, 269
HPLC Sample Introduction, 270
Sample in the Column, 271
Sample at the Detector, 271
Sample on the Chart Recorder, 272
Sample on the Computer Recorder, 273
Parameters, Parameters, 273
Eluent Flow Rate, 273
Temperature, 273
Eluent Composition, 273
Chapter 34. INFRARED SPECTROSCOPY, 275
Molecules As Balls On Springs, 276
Ah, Quantum Mechanics, 277
The Dissonant Oscillator, 277
But Wait! There’s More, 278
More Complicated Molecules, 279
Correlation Tables to the Rescue, 279
Troughs and Reciprocal Centimeters, 279
Some Functional Group Analysis, 285
A Systematic Interpretation, 285
Infrared Sample Preparation, 288
Liquid Samples, 288
Solid Samples, 289
The Thin-Film Solid, 289
The Nujol Mull, 290
Solid KBr Methods, 290
Preparing the Solid Solution, 290
Pressing a KBr Disk—The Minipress, 292
Pressing a KBr Disk—The Hydraulic Press, 292
Running the Spectrum, 294
The Perkin-Elmer 710B IR, 296
Using the Perkin-Elmer 710B, 297
The 100% Control: An Important Aside, 298
Calibration of the Spectrum, 299
IR Spectra: The Finishing Touches, 300
Interpreting IR Spectra, 302
The Fourier Transform Infrared (FTIR), 302
The Optical System, 303
Chapter 35. NUCLEAR MAGNETIC RESONANCE, 307
Liquid Sample Preparation, 308
Solid Samples, 310
Protonless Solvents, 310
Deuterated Solvents, 310
FT-NMR Sample Preparation, 311
Some NMR Interpretation, 311
The Zero Point, 313
The Chemical Shift, 313
Some Anisotropy, 315
Spin–Spin Splitting, 315
Integration, 317
A Final Note, 317
Chapter 36. THEORY OF DISTILLATION, 318
Class 1: Simple Distillation, 319
Clausius and Clapeyron, 321
Class 3: Fractional Distillation, 322
A Hint from Dalton, 322
Dalton and Raoult, 323
A Little Algebra, 323
Clausius and Clapeyron Meet Dalton and Raoult, 324
Dalton Again, 325
What Does It All Mean?, 326
Reality Intrudes I: Changing Composition, 329
Reality Intrudes II: Nonequilibrium Conditions, 330
Reality Intrudes III: Azeotropes, 330
Minimum-Boiling Azeotropes, 331
Maximum-Boiling Azeotropes, 332
Azeotropes on Purpose, 332
Other Deviations, 332
Class 4: Steam Distillation, 333
Chapter 37. THEORY OF EXTRACTION, 336
INDEX, 339

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