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Zubrick James W. The Organic Chem Lab Survival Manual - A Student's Guide to Techniques 10 ed. 2016 [pdf 317sc 300c. 5.64mb]Written for the laboratory that accompanies the sophomore/junior level courses in Organic Chemistry, Zubrick provides students with a valuable guide to the basic techniques of the Organic Chemistry lab. The book will help students understand and practice good lab safety. It will also help students become familiar with basic instrumentation, techniques and apparatus and help them master the latest techniques such as interpretation of infrared spectroscopy. The guide is mostly macroscale in its orientation. Cover......Page 1 Title Page......Page 3 Copyright......Page 4 Preface to the Tenth Edition......Page 5 Contents......Page 7 Chapter 1 Safety First, Last, and Always......Page 17 Disposing of Waste......Page 21 Mixed Waste......Page 23 Green Chemistry and Planning an Organic Synthesis......Page 24 Exercises......Page 26 Chapter 2 Keeping a notebook......Page 27 Notebook Notes......Page 28 A Synthesis Experiment......Page 32 Notebook Notes......Page 33 The Six Maybe Seven Elements in Your Experimental Write-Up......Page 36 Notebook Mortal Sin......Page 37 Calculation of Percent Yield (Not Yeild!)......Page 38 Exercises......Page 40 Chapter 3 Mining your own data......Page 41 Google and the Wiki......Page 42 Exercises......Page 45 Chapter 4 Jointware......Page 46 Stoppers With Only One Number......Page 47 Another Episode of Love of Laboratory......Page 49 Columns and Condensers......Page 50 The Adapter with Lots of Names......Page 51 Inserting Adapter Upside Down......Page 52 Inserting Adapter Upside Down sans Glass......Page 53 To Grease or Not to Grease......Page 54 Into the Grease Pit......Page 55 Corking a Vessel......Page 56 Microscale: A Few Words......Page 57 Skinny Apparatus......Page 58 Sizing Up the Situation......Page 59 Why I Don’t Really Know How Vacuum-Tight These Seals Are......Page 60 The Conical Vial as Vial......Page 61 The Electronic Analytical Balance......Page 62 Heating These Vials......Page 63 Gas Collection Apparatus......Page 64 Generating the Gas......Page 65 Isolating the Product......Page 67 Chapter 6 Other Interesting Equipment......Page 68 Funnels, and Beakers, and Flasks—Oh My!......Page 69 The Flexible Double-Ended Stainless Steel Spatula......Page 70 Transferring a Powdered Solid with the Spatula......Page 71 Calibration......Page 72 Operation......Page 73 Pipet Cutting......Page 74 Pipet Filtering—Liquids......Page 76 Pipet Filtering—Solids......Page 77 Chapter 8 Syringes, Needles, and Septa......Page 79 The Rubber Septum......Page 81 Chapter 9 Clean and Dry......Page 82 Drying Your Glassware When You Do Need To......Page 83 Typical Drying Agents......Page 84 Using a Drying Agent......Page 85 Drying in Stages: The Capacity and Efficiency of Drying Agents......Page 86 Exercises......Page 87 Liquid Product Problems......Page 88 Hold It! Don’t Touch That Vial......Page 89 Chapter 12 The Melting-Point Experiment......Page 90 Loading the Melting-Point Tube......Page 91 Closing Off Melting-Point Tubes......Page 92 The Mel-Temp Apparatus......Page 93 Operation of the Mel-Temp Apparatus......Page 95 The SRS DigiMelt......Page 96 The Fisher-Johns Apparatus......Page 98 Operation of the Fisher-Johns Apparatus......Page 99 The Thomas-Hoover Apparatus......Page 100 Operation of the Thomas-Hoover Apparatus......Page 101 Using the Thiele Tube......Page 104 Getting the Sample Ready......Page 105 Dunking the Melting-Point Tube......Page 106 Exercises......Page 107 Chapter 13 Recrystallization......Page 108 Finding a Good Solvent......Page 109 General Guidelines for a Recrystallization......Page 110 Gravity Filtration......Page 111 The Buchner Funnel and Filter Flask......Page 113 Just a Note......Page 116 Activated Charcoal......Page 117 The Water Trap......Page 118 The Ethanol—Water System......Page 119 A Mixed-Solvent System—The Bad Part......Page 120 World-Famous Fan-Folded Fluted Paper......Page 121 Exercises......Page 123 Chapter 14 Recrystallization: Microscale......Page 124 Craig Tube Filtration......Page 125 Getting the Crystals Out......Page 129 Chapter 15 Extraction and Washing......Page 130 Starting an Extraction......Page 131 Dutch Uncle Advice......Page 132 The Stopper......Page 133 The Teflon Stopcock......Page 134 How to Extract and Wash What......Page 135 The Road to Recovery—Back-Extraction......Page 136 A Sample Extraction......Page 137 Performing an Extraction or Washing......Page 139 Extraction Hints......Page 140 Theory of Extraction......Page 141 Exercises......Page 143 Separation: Removing the Bottom Layer......Page 144 Separation: Removing the Top Layer......Page 145 Separation: Removing Both Layers......Page 146 Boiling Stones......Page 147 The Steam Bath......Page 148 The Bunsen Burner......Page 149 Burner Hints......Page 150 The Heating Mantle......Page 151 Proportional Heaters and Stepless Controllers......Page 153 Exercise......Page 155 Chapter 18 Clamps and Clamping......Page 156 Clamping a Distillation Setup......Page 158 Clipping a Distillation Setup......Page 163 Chapter 19 Distillation......Page 166 Sources of Heat......Page 167 The Distilling Flask......Page 168 The Ubiquitous Clamp......Page 169 The Ice Bath......Page 170 The Distillation Mistake......Page 171 Class 2: Vacuum Distillation......Page 172 Pressure Measurement......Page 173 Leaks......Page 174 Pressure and Temperature Corrections......Page 175 Vacuum Distillation Notes......Page 178 How This Works......Page 180 Fractional Distillation Notes......Page 183 External Steam Distillation......Page 184 Internal Steam Distillation......Page 186 Steam Distillation Notes......Page 187 Simulated Bulb-to-Bulb Distillation: Fakelrohr......Page 188 Exercises......Page 189 Class 2: Vacuum Distillation......Page 191 The Hickman Still Setup......Page 192 Hickman Still Heating......Page 193 A Port in a Storm......Page 194 Chapter 21 The Rotary Evaporator......Page 195 Exercises......Page 198 Standard Reflux......Page 199 A Dry Reflux......Page 201 Funnel Fun......Page 202 How to Set Up......Page 204 Exercise......Page 205 Addition and Reflux: Microscale......Page 206 Chapter 24 Sublimation......Page 208 Microscale Boiling Point......Page 211 Ultramicroscale Boiling Point......Page 213 Adsorbents......Page 215 The Eluatropic Series......Page 216 We Don’t Make Our Own TLC Plates Any More, But.........Page 218 The Plate Spotter......Page 219 Spotting the Plates......Page 220 Developing a Plate......Page 221 Visualization......Page 222 Interpretation......Page 223 Multiple Spotting......Page 225 Other TLC Problems......Page 226 Exercises......Page 228 Preparing the Column......Page 230 Compounds on the Column......Page 232 Visualization and Collection......Page 233 Wet-Column Chromatography: Microscale......Page 234 Flash Chromatography......Page 235 Microscale Flash Chromatography......Page 236 Exercises......Page 237 Chapter 29 Refractometry......Page 238 The Abbé Refractometer......Page 239 Before Using the Abbé Refractometer: A Little Practice......Page 240 Using the Abbé Refractometer......Page 241 Refractometry Hints......Page 242 The Mobile Phase: Gas......Page 243 GC Sample Introduction......Page 244 Sample in the Column......Page 246 Sample at the Detector......Page 247 Electronic Interlude......Page 248 Sample on the Computer......Page 249 Temperature......Page 250 Exercises......Page 251 Chapter 31 HP Liquid Chromatography......Page 252 The Mobile Phase: Liquid......Page 253 A Bubble Trap......Page 254 HPLC Sample Preparation......Page 255 HPLC Sample Introduction......Page 257 Sample at the Detector......Page 258 Parameters, Parameters......Page 259 Exercises......Page 260 Molecules As Balls On Springs......Page 261 The Dissonant Oscillator......Page 263 More Complicated Molecules......Page 264 Correlation Tables to the Rescue......Page 266 Some Functional Group Analysis......Page 270 A Systematic Interpretation......Page 272 Liquid Samples......Page 274 Solid Samples......Page 275 Running the Spectrum......Page 278 Interpreting IR Spectra—Finishing Touches......Page 279 The Optical System......Page 280 Electrons Get to Jump......Page 284 Instrument Configuration......Page 285 Solvents......Page 286 Exercises......Page 287 Nuclei Have Spin, Too......Page 288 Everybody Line Up, Flip, and Relax......Page 289 The Chemical Shift......Page 290 Be It Better Resolved.........Page 291 NMR Sample Preparation......Page 292 The Chemical Shift and TMS Zero......Page 296 Integration and Labeling......Page 298 Threaded Interpretations: Spectrum #2 (Toluene) and Spectrum #3 (p-Dichlorobenzene)......Page 299 Threaded Interpretations: Spectrum #4 (Ethylbenzene) and Spectrum #5 (A Double Resonance Experiment)......Page 301 Use a Correlation Chart......Page 304 Exercises......Page 306 Index......Page 307 EULA......Page 317 "Written for the laboratory that accompanies the sophomore/junior level courses in Organic Chemistry, Zubrick provides students with a valuable guide to the basic techniques of the Organic Chemistry lab. The book will help students understand and practice good lab safety. It will also help students become familiar with basic instrumentation, techniques and apparatus and help them master the latest techniques such as interpretation of infrared spectroscopy. The guide is mostly macroscale in its orientation."-- Provided by publisher