The organic chem lab survival manual : a student's guide to techniques

James W. Zubrick

This book presents the basic techniques of the organic chemistry laboratory with an emphasis on doing the work correctly the first time. New to this edition are discussions on safety in the laboratory with new consideration of the addition of such technology as the iPad, Nook, Kindle, and even text messaging. Updated discussion is added on Microscale; a number of NMR spectra have been added, with basic interpretation and suggestions on presentation of the data; and lastly, presentation of a more modern outline of the instrumentation of HPLC is included.

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[目次]

  • 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 Abbe Refractometer 243 Before Using the Abbe Refractometer: A Little Practice 245 Using the Abbe 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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この本の情報

書名 The organic chem lab survival manual : a student's guide to techniques
著作者等 Zubrick, James W
出版元 Wiley
刊行年月 c2014
版表示 9th ed
ページ数 xiv, 354 p.
大きさ 23 cm
ISBN 9781118083390
NCID BB11622885
※クリックでCiNii Booksを表示
言語 英語
出版国 アメリカ合衆国
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