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Table Of Contents

CHAPTER 1 SAFETY FIRST, LAST, AND ALWAYS 1
CHAPTER 6 OTHER INTERESTING EQUIPMENT 62
CHAPTER 32 INFRARED SPECTROSCOPY (AND A BIT OF UV-VIS,TOO) 271
ACCIDENTS WILL NOT HAPPEN
DISPOSING OF WASTE
DISPOSING OF WASTE 5
Mixed Waste
MATERIAL SAFETY DATA SHEET (MSDS)
GREEN CHEMISTRY AND PLANNING AN ORGANIC SYNTHESIS
GREEN CHEMISTRY AND PLANNING AN ORGANIC SYNTHESIS 9
A TECHNIQUE EXPERIMENT
A SYNTHESIS EXPERIMENT
A SYNTHESIS EXPERIMENT 13
NOTEBOOK MORTAL SIN 25
MERCK INDEX
There’s a CD
THE ALDRICH CATALOG
THE ALDRICH CATALOG 35
NOT CLEAR–CLEAR?
INFO ON THE INTERNET
STOPPERS WITH ONLY ONE NUMBER
ANOTHER EPISODE OF LOVE OF LABORATORY
HALL OF BLUNDERS AND THINGS NOT QUITE RIGHT
Round-Bottom Flasks
Columns and Condensers
The Adapter with Lots of Names
Inserting Adapter Upside Down
Inserting Adapter Upside Down sans Glass
THE O-RING AND CAP BRANCH OUT
GREASING THE JOINTS
To Grease or Not to Grease
Preparation of the Joints
STORING STUFF AND STICKING STOPPERS
CORKING A VESSEL
THE CORK PRESS
MICROSCALE: A FEW WORDS
UH-OH RINGS
THE O-RING CAP SEAL
Skinny Apparatus
Not-So-Skinny Apparatus
Sizing Up the Situation
Why I Don’t Really Know How Vacuum-Tight These Seals Are
THE COMICAL VIAL (THAT’S CONICAL! )
The Conical Vial as Vial
Packaging Oops
Tare to the Analytical Balance
The Electronic Analytical Balance
Heating These Vials
THE MICROSCALE DRYING TUBE
THE MICROSCALE DRYING TUBE 57
GAS COLLECTION APPARATUS
Generating the Gas
Isolating the Product
THE FLEXIBLE DOUBLE-ENDED STAINLESS STEEL SPATULA
PRE-PREPARING PASTEUR PIPETS
Calibration
PIPET FILTERING—SOLIDS 71
DRYING YOUR GLASSWARE WHEN YOU DON’T NEED TO
DRYING YOUR GLASSWARE WHEN YOU DO NEED TO
DRYING YOUR GLASSWARE WHEN YOU DO NEED TO 79
TYPICAL DRYING AGENTS
FOLLOWING DIRECTIONS AND LOSING PRODUCT ANYWAY
DRYING AGENTS: MICROSCALE
DRYING IN STAGES: THE CAPACITY AND EFFICIENCY OF DRYING AGENTS
SOLID PRODUCT PROBLEMS
LIQUID PRODUCT PROBLEMS
THE SAMPLE VIAL
HOLD IT! DON’T TOUCH THAT VIAL
SAMPLE PREPARATION
Loading the Melting-Point Tube
Closing Off Melting-Point Tubes
MELTING-POINT HINTS
THE MEL-TEMP APPARATUS
THE MEL-TEMP APPARATUS 91
OPERATION OF THE MEL-TEMP APPARATUS
THE FISHER-JOHNS APPARATUS
THE FISHER-JOHNS APPARATUS 93
OPERATION OF THE FISHER-JOHNS APPARATUS
THE THOMAS-HOOVER APPARATUS
THE THOMAS-HOOVER APPARATUS 95
OPERATION OF THE THOMAS-HOOVER APPARATUS
OPERATION OF THE THOMAS-HOOVER APPARATUS 97
USING THE THIELE TUBE
USING THE THIELE TUBE 99
Cleaning the Tube
Getting the Sample Ready
Dunking the Melting-Point Tube
Heating the Sample
FINDING A GOOD SOLVENT
GENERAL GUIDELINES FOR A RECRYSTALLIZATION
GRAVITY FILTRATION
GRAVITY FILTRATION 107
THE BUCHNER FUNNEL AND FILTER FLASK
THE HIRSCH FUNNEL AND FRIENDS
THE HIRSCH FUNNEL AND FRIENDS 113
ACTIVATED CHARCOAL
THE WATER ASPIRATOR: A VACUUM SOURCE
WORKING WITH A MIXED-SOLVENT SYSTEMTHE GOOD PART
WORKING WITH A MIXED-SOLVENT SYSTEM—THE GOOD PART 115
SALTING OUT 117
WORLD-FAMOUS FAN-FOLDED FLUTED PAPER
ISOLATING THE CRYSTALS
CRAIG TUBE FILTRATION
CENTRIFUGING THE CRAIG TUBE
Getting the Crystals Out
STARTING AN EXTRACTION
STARTING AN EXTRACTION 129
DUTCH UNCLE ADVICE
THE SEPARATORY FUNNEL
The Glass Stopcock
THE SEPARATORY FUNNEL 131
The Teflon Stopcock
HOW TO EXTRACT AND WASH WHAT
The Road to Recovery—Back-Extraction
A Sample Extraction
Performing an Extraction or Washing
SEPARATION: REMOVING THE TOP LAYER 143
SEPARATION: REMOVING BOTH LAYERS
PROPORTIONAL HEATERS AND STEPLESS CONTROLLERS
CLAMPING A DISTILLATION SETUP
CLAMPING A DISTILLATION SETUP 157
CLIPPING A DISTILLATION SETUP
CLIPPING A DISTILLATION SETUP 161
DISTILLATION NOTES
Sources of Heat
The Three-Way Adapter
The Distilling Flask
The Thermometer Adapter
The Ubiquitous Clamp
The Thermometer
The Condenser
The Vacuum Adapter
The Receiving Flask
THE DISTILLATION EXAMPLE
THE DISTILLATION EXAMPLE 169
THE DISTILLATION MISTAKE
CLASS 2: VACUUM DISTILLATION
Pressure Measurement
Pressure and Temperature Corrections
Vacuum Distillation Notes
CLASS 3: FRACTIONAL DISTILLATION
How This Works
Fractional Distillation Notes
CLASS 4: STEAM DISTILLATION
CLASS 4: STEAM DISTILLATION 183
External Steam Distillation
Internal Steam Distillation
STEAM DISTILLATION NOTES
STEAM DISTILLATION NOTES 185
SIMULATED BULB-TO-BULB DISTILLATION: FAKELROHR
SIMULATED BULB-TO-BULB DISTILLATION: FAKELROHR 187
Class 1: Simple Distillation
Class 2: Vacuum Distillation
Class 3: Fractional Distillation
Class 4: Steam Distillation
MICROSCALE DISTILLATION II: THE HICKMAN STILL
The Hickman Still Setup
Hickman Still Heating
Recovering Your Product
ULTRAMICROSCALE BOILING POINT
SEPARATION OR DEVELOPMENT
THE ELUATROPIC SERIES
PREPARATION OF TLC PLATES
THE PLATE SPOTTER
SPOTTING THE PLATES
SPOTTING THE PLATES 225
DEVELOPING A PLATE
MULTIPLE SPOTTING
OTHER TLC PROBLEMS
PREPARATIVE TLC 233
PREPARING THE COLUMN
COMPOUNDS ON THE COLUMN
COMPOUNDS ON THE COLUMN 239
VISUALIZATION AND COLLECTION
WET-COLUMN CHROMATOGRAPHY: MICROSCALE
WET-COLUMN CHROMATOGRAPHY: MICROSCALE 241
FLASH CHROMATOGRAPHY
MICROSCALE FLASH CHROMATOGRAPHY
BEFORE USING THE ABBÉ REFRACTOMETER: A LITTLE PRACTICE
USING THE ABBÉ REFRACTOMETER
USING THE ABBÉ REFRACTOMETER 247
REFRACTOMETRY HINTS
REFRACTOMETRY HINTS 249
THE MOBILE PHASE: GAS
GC SAMPLE PREPARATION
GC SAMPLE INTRODUCTION
SAMPLE IN THE COLUMN
SAMPLE AT THE DETECTOR
ELECTRONIC INTERLUDE
SAMPLE ON THE COMPUTER
SAMPLE ON THE COMPUTER 257
PARAMETERS, PARAMETERS
Gas Flow Rate
Temperature
THE MOBILE PHASE: LIQUID
A Bubble Trap
The Pulse Dampener
HPLC SAMPLE PREPARATION
HPLC SAMPLE PREPARATION 265
HPLC SAMPLE INTRODUCTION
SAMPLE IN THE COLUMN 267
Eluent Flow Rate
Eluent Composition
MOLECULES AS BALLS ON SPRINGS
AH, QUANTUM MECHANICS
AH, QUANTUM MECHANICS 273
THE DISSONANT OSCILLATOR
BUT WAIT! THERE’S MORE
MORE COMPLICATED MOLECULES
CORRELATION TABLES TO THE RESCUE
TROUGHS AND RECIPROCAL CENTIMETERS
TROUGHS AND RECIPROCAL CENTIMETERS 275
SOME FUNCTIONAL GROUP ANALYSIS
A SYSTEMATIC INTERPRETATION
A SYSTEMATIC INTERPRETATION 281
Solid Samples
RUNNING THE SPECTRUM
USING THE PERKIN-ELMER 710B
The 100% Control: An Important Aside
USING THE PERKIN-ELMER 710B 293
CALIBRATION OF THE SPECTRUM
CALIBRATION OF THE SPECTRUM 295
INTERPRETING IR SPECTRA FINISHING TOUCHES
The Optical System
AND UV-VIS TOO!
ELECTRONS GET TO JUMP
INSTRUMENT CONFIGURATION
Sample (and Reference) Cells
NUCLEI HAVE SPIN, TOO
THE MAGNETIC CATCH
EVERYBODY LINE UP, FLIP, AND RELAX
A MORE SENSITIVE CENSUS
THE CHEMICAL SHIFT
T FOR ONE AND TWO
T FOR ONE AND TWO 309
BE IT BETTER RESOLVED . .
INCREDIBLY BASIC FT-NMR
LIQUID SAMPLE PREPARATION
LIQUID SAMPLE PREPARATION 311
SOLID SAMPLES
Protonless Solvents
Deuterated Solvents
FT- NMR SAMPLE PREPARATION
SOME NMR INTERPRETATION
The Zero Point
The Chemical Shift
Some Anisotropy
Spin–Spin Splitting
Integration
A Final Note
CLASS 1: SIMPLE DISTILLATION
Clausius and Clapeyron
A Hint from Dalton
CLASS 3: FRACTIONAL DISTILLATION 325
Dalton and Raoult
A Little Algebra
Clausius and Clapeyron Meet Dalton and Raoult
Dalton Again
What Does It All Mean?
Reality Intrudes I: Changing Composition
Reality Intrudes II: Nonequilibrium Conditions
Reality Intrudes III: Azeotropes
Other Deviations
INDEX
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The Organic Chemistry Lab survival manual

The Organic Chemistry Lab survival manual

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Published by: AsarTehutiImhotep on Jun 30, 2011
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