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Safety First, Last, and Always | |
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Accidents Will Not Happen | |
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Disposing of Waste | |
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Mixed Waste | |
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Keeping a Notebook | |
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A Technique Experiment | |
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Notebook Notes | |
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A Synthesis Experiment | |
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Notebook Notes | |
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The Acid Test | |
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Interpreting a Handbook | |
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CRC Handbook | |
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Entry: 1-Bromobutane | |
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Entry: Benzoic Acid | |
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Lange's | |
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Entry: 1-Bromobutane | |
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Entry: Benzoic Acid | |
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Merck Index | |
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Entry: 1-Bromobutane | |
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Entry: Benzoic Acid | |
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The Aldrich Catalog | |
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Entry: 1-Bromobutane | |
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Entry: Benzoic Acid | |
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Not Clear-Clear? | |
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Info on the Internet | |
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Jointware | |
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Stoppers with Only One Number | |
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Another Episode of Love of Laboratory | |
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Hall of Blunders and Things Not Quite Right | |
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Round-Bottom Flasks | |
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Columns and Condensers | |
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The Adapter with Lots of Names | |
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Forgetting the Glass | |
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Inserting Adapter Upside Down | |
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Inserting Adapter Upside Down sans Glass | |
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Greasing the Joints | |
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To Grease or Not to Grease | |
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Preparation of the Joints | |
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Into the Grease Pit | |
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Storing Stuff and Sticking Stoppers | |
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Corking a Vessel | |
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The Cork Press | |
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The O-Ring and Cap Branch Out | |
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Microscale Jointware | |
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Microscale: A Few Words | |
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Uh-Oh Rings | |
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The O-Ring Cap Seal | |
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Sizing Up the Situation | |
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Why I Don't Really Know How Vacuum Tight These Seals Are | |
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The Comical Vial (That's Conical!) | |
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The Conical Vial as Vial | |
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Packaging Oops | |
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Tare to the Analytical Balance | |
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The Electronic Analytical Balance | |
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Heating These Vials | |
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The Microscale Drying Tube | |
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Gas Collection Apparatus | |
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Generating the Gas | |
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Isolating the Product | |
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Other Interesting Equipment | |
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Pipet Tips | |
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Pre-preparing Pasteur Pipets | |
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Calibration | |
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Operation | |
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Amelioration | |
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Pipet Cutting | |
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Pipet Filtering-Liquids | |
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Pipet Filtering-Solids | |
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Syringes, Needles, and Septa | |
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The Rubber Septum | |
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Clean and Dry | |
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Drying Your Glassware When You Don't Need To | |
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Drying Your Glassware When You Need To | |
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Drying Agents | |
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Typical Drying Agents | |
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Using a Drying Agent | |
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Following Directions and Losing Product Anyway | |
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Drying Agents: Microscale | |
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On Products | |
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Solid Product Problems | |
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Liquid Product Problems | |
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The Sample Vial | |
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Hold It! Don't Touch That Vial | |
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The Melting Point Experiment | |
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Sample Preparation | |
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Loading the Melting Point Tube | |
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Closing Off Melting Point Tubes | |
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Melting Point Hints | |
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The Mel-Temp Apparatus | |
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Operation of the Mel-Temp Apparatus | |
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The Fisher-Johns Apparatus | |
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Operation of the Fisher-Johns Apparatus | |
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The Thomas-Hoover Apparatus | |
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Operation of the Thomas-Hoover Apparatus | |
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Using the Thiele Tube | |
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Cleaning the Tube | |
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Getting the Sample Ready | |
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Dunking the Melting Point Tube | |
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Heating the Sample | |
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Recrystallization | |
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Finding a Good Solvent | |
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General Guidelines for a Recrystallization | |
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Gravity Filtration | |
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The Buchner Funnel and Filter Flask | |
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Just a Note | |
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The Hirsch Funnel and Friends | |
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Activated Charcoal | |
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The Water Aspirator: A Vacuum Source | |
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The Water Trap | |
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Working with a Mixed-Solvent System--The Good Part | |
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The Ethanol-Water System | |
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A Mixed-Solvent System--The Bad Part | |
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Salting Out | |
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World Famous Fan-Folded Fluted Paper | |
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Recrystallization: Microscale | |
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Isolating the Crystals | |
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Craig Tube Filtration | |
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Centrifuging the Craig Tube | |
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Getting the Crystals Out | |
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Extraction and Washing | |
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Never-Ever Land | |
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Starting an Extraction | |
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Dutch Uncle Advice | |
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The Separatory Funnel | |
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The Stopper | |
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The Glass Stopcock | |
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The Teflon Stopcock | |
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The Stem | |
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Washing and Extracting Various Things | |
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How to Extract and Wash What | |
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The Road to Recovery--Back-Extraction | |
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A Sample Extraction | |
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Performing an Extraction or Washing | |
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Extraction Hints | |
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Extraction and Washing: Microscale | |
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Mixing | |
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Separation: Removing the Bottom Layer | |
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Separation: Removing the Top Layer | |
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And Now--Boiling Stones | |
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Sources of Heat | |
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The Steam Bath | |
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The Bunsen Burner | |
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Burner Hints | |
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The Heating Mantle | |
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Proportional Heaters and Stepless Controllers | |
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Clamps and Clamping | |
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Clamping a Distillation Setup | |
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Clipping a Distillation Setup | |
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Distillation | |
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Distillation Notes | |
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Simple Distillation | |
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Sources of Heat | |
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The Three-Way Adapter | |
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The Distilling Flask | |
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The Thermometer Adapter | |
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The Ubiquitous Clamp | |
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The Thermometer | |
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The Condenser | |
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The Vacuum Adapter | |
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The Receiving Flask | |
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The Ice Bath | |
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The Distillation Example | |
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The Distillation Mistake | |
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Vacuum Distillation | |
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Pressure Measurement | |
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Manometer Hints | |
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Leaks | |
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Pressure and Temperature Corrections | |
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Vacuum Distillation Notes | |
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Fractional Distillation | |
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How This Works | |
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Fractional Distillation Notes | |
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Azeotropes | |
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Steam Distillation | |
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External Steam Distillation | |
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Internal Steam Distillation | |
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Steam Distillation Notes | |
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Microscale Distillation | |
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Like the Big Guy | |
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Simple Distillation | |
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Vacuum Distillation | |
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Fractional Distillation | |
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Steam Distillation | |
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Microscale Distillation II: The Hickman Still | |
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The Hickman Still Setup | |
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Hickman Still Heating | |
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Recovering Your Product | |
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Reflux and Addition | |
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Standard Reflux | |
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A Dry Reflux | |
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Addition and Reflux | |
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Funnel Fun | |
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How to Set Up | |
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Reflux: Microscale | |
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Addition and Reflux: Microscale | |
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Sublimation | |
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Microscale Boiling Point | |
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Microscale BP | |
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Ultramicroscale BP | |
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Chromatography: Some Generalities | |
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Adsorbents | |
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Separation or Development | |
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The Eluatropic Series | |
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Thin-Layer Chromatography: TLC | |
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Preparation of TLC Plates | |
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Pre-prepared TLC Plates | |
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The Plate Spotter | |
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Spotting the Plates | |
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Developing a Plate | |
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Visualization | |
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Interpretation | |
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Multiple Spotting | |
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Cospotting | |
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Other TLC Problems | |
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Preparative TLC | |
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Wet-Column Chromatography | |
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Preparing the Column | |
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Compounds on the Column | |
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Visualization and Collection | |
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Wet-Column Chromatography: Microscale | |
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Flash Chromatography | |
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Microscale Flash Chromatography | |
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Refractometry | |
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The Abbe Refractometer | |
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Using the Abbe Refractometer | |
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Refractometry Hints | |
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Instrumentation in the Lab | |
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Gas Chromatography | |
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The Mobile Phase: Gas | |
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GC Sample Preparation | |
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GC Sample Introduction | |
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Sample in the Column | |
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Sample at the Detector | |
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Electronic Interlude | |
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Sample on the Chart Recorder | |
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Sample on the Computer Recorder | |
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Parameters, Parameters | |
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Gas Flow Rate | |
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Temperature | |
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Hp Liquid Chromatography | |
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The Mobile Phase: Liquid | |
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A Bubble Trap | |
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The Pump | |
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The Pulse Dampener | |
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HPLC Sample Preparation | |
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HPLC Sample Introduction | |
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Sample in the Column | |
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Sample at the Detector | |
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Sample on the Chart Recorder | |
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Sample on the Computer Recorder | |
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Parameters, Parameters | |
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Eluent Flow Rate | |
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Temperature | |
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Eluent Composition | |
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Infrared Spectroscopy | |
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Infrared Sample Preparation | |
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Liquid Samples | |
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Solid Samples | |
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The Nujol Mull | |
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Solid KBr Methods | |
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Preparing the Solid Solution | |
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Pressing a KBr Disk--The Minipress | |
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Pressing a KBr Disk--The Hydraulic Press | |
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Running the Spectrum | |
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The Perkin-Elmer 710B IR | |
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Using the Perkin-Elmer 710B | |
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The 100% Control: An Important Aside | |
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Calibration of the Spectrum | |
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IR Spectra: The Finishing Touches | |
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Interpreting IRs | |
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The Fourier Transform Infrared (FTIR) | |
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The Optical System | |
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Nuclear Magnetic Resonance | |
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Liquid Sample Preparation | |
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Solid Samples | |
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Protonless Solvents | |
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Deuterated Solvents | |
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FT-NMR Sample Preparation | |
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Some NMR Interpretation | |
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The Zero Point | |
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The Chemical Shift | |
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Some Anisotropy | |
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Spin-Spin Splitting | |
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Integration | |
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A Final Note | |
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Theory of Distillation | |
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Simple Distillation | |
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Clausius and Clapeyron | |
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Fractional Distillation | |
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A Hint from Dalton | |
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Dalton and Raoult | |
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A Little Algebra | |
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Clausius and Clapeyron Meet Dalton and Raoult | |
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Dalton Again | |
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What Does It All Mean? | |
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Changing Composition | |
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Nonequilibrium Conditions | |
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Azeotropes | |
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Minimum-Boiling Azeotropes | |
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Maximum-Boiling Azeotropes | |
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Azeotropes on Purpose | |
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Other Deviations | |
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Steam Distillation | |
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Theory of Extraction | |
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Index | |