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CHAPTER 1 SAFETY FIRST, LAST, AND ALWAYS 1
Accidents Will Not Happen 5
Disposing of Waste 5
Mixed Waste 7
Material Safety Data Sheet (MSDS) 8
Green Chemistry and Planning an Organic Synthesis 9
An iBag for Your iThing 10
Exercises 10
CHAPTER 2 KEEPING A NOTEBOOK 11
A Technique Experiment 12
Notebook Notes 13
A Synthesis Experiment 13
Notebook Notes 13
Calculation of Percent Yield (Not Yeild!) 23
Estimation Is Your Friend 25
The Acid Test 25
Notebook Mortal Sin 25
Exercises 26
CHAPTER 3 INTERPRETING A HANDBOOK 27
CRC Handbook 28
Entry: 1-Bromobutane 28
Entry: Benzoic Acid 29
Lange’s 31
Entry: 1-Bromobutane 31
Entry: Benzoic Acid 31
Merck Index 31
Entry: 1-Bromobutane 33
Entry: Benzoic Acid 34
There’s a CD 34
The Aldrich Catalog 35
Entry: 1-Bromobutane 35
Entry: Benzoic Acid 36
Not Clear–Clear? 36
Info on the Internet 37
Exercises 37
CHAPTER 4 JOINTWARE 38
Stoppers with Only One Number 39
Another Episode of Love of Laboratory 40
Hall of Blunders and Things Not Quite Right 42
Round-Bottom Flasks 42
Columns and Condensers 43
The Adapter with Lots of Names 43
Forgetting the Glass 45
Inserting Adapter Upside Down 45
Inserting Adapter Upside Down sans Glass 46
The O-Ring and Cap Branch Out 46
Greasing the Joints 46
To Grease or Not to Grease 47
Preparation of the Joints 47
Into the Grease Pit 47
Storing Stuff and Sticking Stoppers 48
Corking a Vessel 48
CHAPTER 5 MICROSCALE JOINTWARE 50
Microscale: A Few Words 51
Uh-Oh Rings 51
The O-Ring Cap Seal 51
Skinny Apparatus 51
Not-So-Skinny Apparatus 52
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! 63
The Flexible Double-Ended Stainless Steel Spatula 63
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 75
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 83
Drying in Stages: The Capacity and Efficiency of Drying Agents 83
Exercises 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
Exercises 103
CHAPTER 13 RECRYSTALLIZATION 104
Finding a Good Solvent 105
General Guidelines for a Recrystallization 106
My Product Disappeared 107
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
Exercises 119
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
Exercises 140
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 SOURCES OF HEAT 145
Boiling Stones 146
The Steam Bath 146
The Bunsen Burner 147
Burner Hints 149
The Heating Mantle 150
Proportional Heaters and Stepless Controllers 152
Exercise 153
CHAPTER 18 CLAMPS AND CLAMPING 154
Clamping a Distillation Setup 157
Clipping a Distillation Setup 161
CHAPTER 19 DISTILLATION 164
Distillation Notes 165
Class 1: Simple Distillation 166
Sources of Heat 166
The Three-Way Adapter 167
The Distilling Flask 167
The Thermometer Adapter 168
The Ubiquitous Clamp 168
The Thermometer 168
The Condenser 168
The Vacuum Adapter 168
The Receiving Flask 169
The Ice Bath 169
The Distillation Example 169
The Distillation Mistake 170
Class 2: Vacuum Distillation 170
Pressure Measurement 171
Manometer Hints 173
Leaks 173
Pressure and Temperature Corrections 173
Vacuum Distillation Notes 177
Class 3: Fractional Distillation 178
How This Works 178
Fractional Distillation Notes 180
Azeotropes 183
Class 4: Steam Distillation 183
External Steam Distillation 184
Internal Steam Distillation 185
Steam Distillation Notes 185
Simulated Bulb-to-Bulb Distillation: Fakelrohr 187
Exercises 189
CHAPTER 20 MICROSCALE DISTILLATION 190
Like the Big Guy 191
Class 1: Simple Distillation 191
Class 2: Vacuum Distillation 191
Class 3: Fractional Distillation 191
Class 4: Steam Distillation 191
Microscale Distillation II: The Hickman Still 192
The Hickman Still Setup 192
Hickman Still Heating 193
Recovering Your Product 193
A Port in a Storm 194
CHAPTER 21 THE ROTARY EVAPORATOR 195
Exercises 199
CHAPTER 22 REFLUX AND ADDITION 200
Standard Reflux 201
A Dry Reflux 202
Addition and Reflux 204
Funnel Fun 204
How to Set Up 205
Exercise 207
CHAPTER 23 REFLUX: MICROSCALE 208
Addition and Reflux: Microscale 209
CHAPTER 24 SUBLIMATION 211
CHAPTER 25 MICROSCALE BOILING POINT 214
Microscale Boiling Point 215
Ultramicroscale Boiling Point 216
CHAPTER 26 CHROMATOGRAPHY: SOME GENERALITIES 218
Adsorbents 219
Separation or Development 219
The Eluatropic Series 219
CHAPTER 27 THIN-LAYER CHROMATOGRAPHY: TLC 222
We Don’t Make Our Own TLC Plates Any More, But… 223
Pre-prepared TLC Plates 223
The Plate Spotter 223
Spotting the Plates 224
Developing a Plate 225
Visualization 227
Interpretation 228
Multiple Spotting 230
Cospotting 230
Other TLC Problems 231
Preparative TLC 232
Exercises 233
CHAPTER 28 WET-COLUMN CHROMATOGRAPHY 234
Preparing the Column 235
Compounds on the Column 237
Visualization and Collection 238
Wet-Column Chromatography: Microscale 239
Flash Chromatography 241
Microscale Flash Chromatography 241
Exercises 241
CHAPTER 29 REFRACTOMETRY 242
The Abbé Refractometer 243
Before Using the Abbé Refractometer: A Little Practice 245
Using the Abbé Refractometer 245
Refractometry Hints 247
CHAPTER 30 GAS CHROMATOGRAPHY 248
The Mobile Phase: Gas 249
GC Sample Preparation 250
GC Sample Introduction 250
Sample in the Column 252
Sample at the Detector 252
Electronic Interlude 254
Sample on the Computer 255
Parameters, Parameters 256
Gas Flow Rate 256
Temperature 256
Exercises 257
CHAPTER 31 HP LIQUID CHROMATOGRAPHY 258
The Mobile Phase: Liquid 259
A Bubble Trap 259
The Pump and Pulse Dampener Module 261
HPLC Sample Preparation 262
HPLC Sample Introduction 263
Sample in the Column 264
Sample at the Detector 265
Sample on the Computer 266
Parameters, Parameters 266
Eluent Flow Rate 266
Temperature 266
Eluent Composition 267
Exercises 267
CHAPTER 32 INFRARED SPECTROSCOPY (AND A BIT OF UV-VIS, TOO) 268
Molecules as Balls on Springs 269
Ah, Quantum Mechanics 270
The Dissonant Oscillator 271
But Wait! There’s More 271
More Complicated Molecules 272
Correlation Tables to the Rescue 272
Troughs and Reciprocal Centimeters 272
Some Functional Group Analysis 278
A Systematic Interpretation 278
Infrared Sample Preparation 281
Liquid Samples 281
Solid Samples 282
Running the Spectrum 287
The Perkin-Elmer 710B IR 289
Using the Perkin-Elmer 710B 290
The 100% Control: An Important Aside 291
Calibration of the Spectrum 293
IR Spectra: The Finishing Touches 294
Interpreting IR Spectra—Finishing Touches 295
The Fourier Transform Infrared (FTIR) 296
The Optical System 296
A Reflectance Attachment: Something to Think About 300
And UV-VIS Too! 300
Electrons Get to Jump 300
Instrument Configuration 301
Source 301
Sample (and Reference) Cells 302
Solvents 303
Exercises 303
CHAPTER 33 NUCLEAR MAGNETIC RESONANCE 304
Nuclei Have Spin, Too 305
The Magnetic Catch 305
Everybody Line Up, Flip, and Relax 306
A More Sensitive Census 306
The Chemical Shift 307
T for One and Two 307
Be It Better Resolved . . . 308
Incredibly Basic FT-NMR 308
NMR Sample Preparation 309
Some NMR Terms and Interpretations 312
The Chemical Shift and TMS Zero 312
Integration and Labeling 314
Threaded Interpretations: Spectrum #1 (t-butyl alcohol) 315
Threaded Interpretations: Spectrum #2 (Toluene) and Spectrum #3 (p-Dichlorobenzene) 315
Threaded Interpretations: Spectrum #4 (Ethylbenzene) and Spectrum #5 (A Double Resonance Experiment) 319
Use a Correlation Chart 320
Exercises 323
CHAPTER 34 THEORY OF DISTILLATION 324
Class 1: Simple Distillation 325
Clausius and Clapeyron 327
Class 3: Fractional Distillation 328
A Hint from Dalton 328
Dalton and Raoult 329
A Little Algebra 329
Clausius and Clapeyron Meet Dalton and Raoult 330
Dalton Again 331
What Does It All Mean? 332
Reality Intrudes I: Changing Composition 335
Reality Intrudes II: Nonequilibrium Conditions 336
Reality Intrudes III: Azeotropes 336
Other Deviations 338
Class 4: Steam Distillation 339
CHAPTER 35 THEORY OF EXTRACTION 342
INDEX 345
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