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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 Organic Chem Lab Survival Manual 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 Organic Chem Lab Survival Manual is mostly macroscale in its orientation.
CHAPTER 1 SAFETY FIRST, LAST, AND ALWAYS
Accidents Will Not Happen
Disposing of Waste
Material Safety Data Sheet (MSDS)
Green Chemistry and Planning an Organic Synthesis
An iBag for Your iThing
Exercises
CHAPTER 2 KEEPING A NOTEBOOK
A Technique Experiment
A Synthesis Experiment
The Six Maybe Seven Elements in Your Experimental Write-Up
The Acid Test
Notebook Mortal Sin
Calculation of Percent Yield (Not Yeild!)
Estimation Is Your Friend
Exercises
CHAPTER 3 INTERPRETING A HANDBOOK
Google and the WIKI
The Terphenyl Anomaly
Exercises
CHAPTER 4 JOINTWARE
Stoppers with Only One Number
Another Episode of Love of Laboratory
Hall of Blunders and Things Not Quite Right
The O-Ring and Cap Branch Out
Greasing the Joints
Storing Stuff and Sticking Stoppers
Corking a Vessel
CHAPTER 5 MICROSCALE JOINTWARE
Microscale: A Few Words
Uh-Oh Rings
The O-Ring Cap Seal
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
Gas Collection Apparatus
CHAPTER 6 OTHER INTERESTING EQUIPMENT
Funnels, and Beakers, and Flasks—Oh My!
The Flexible Double-Ended Stainless Steel Spatula
CHAPTER 7 PIPET TIPS
Pre-Preparing Pasteur Pipets
Pipet Cutting
Pipet Filtering—Liquids
Pipet Filtering—Solids
CHAPTER 8 SYRINGES, NEEDLES, AND SEPTA
The Rubber Septum
CHAPTER 9 CLEAN AND DRY
Drying Your Glassware When You Don’t Need To
Drying Your Glassware When You Do Need To
CHAPTER 10 DRYING AGENTS
Typical Drying Agents
Using a Drying Agent
Following Directions and Losing Product Anyway
Drying Agents: Microscale
Drying in Stages: The Capacity and Efficiency of Drying Agents
Exercises
CHAPTER 11 ON PRODUCTS
Solid Product Problems
Liquid Product Problems
The Sample Vial
Hold It! Don’t Touch That Vial
CHAPTER 12 THE MELTING-POINT EXPERIMENT
Sample Preparation
Melting-Point Hints
The Mel-Temp Apparatus
The Fisher-Johns Apparatus
The Thomas-Hoover Apparatus
Operation of the Thomas-Hoover Apparatus
Using the Thiele Tube
Exercises
CHAPTER 13 RECRYSTALLIZATION
Finding a Good Solvent
General Guidelines for a Recrystallization
Gravity Filtration
The Buchner Funnel and Filter Flask
The Hirsch Funnel and Friends
Activated Charcoal
The Water Aspirator: A Vacuum Source
The Water Trap
Working with a Mixed-Solvent System—The Good Part
A Mixed-Solvent System—The Bad Part
Salting Out
World-Famous Fan-Folded Fluted Paper
Exercises
CHAPTER 14 RECRYSTALLIZATION: MICROSCALE
Isolating the Crystals
Craig Tube Filtration
Centrifuging the Craig Tube
Getting the Crystals Out
CHAPTER 15 EXTRACTION AND WASHING
Never-Ever Land
Starting an Extraction
Dutch Uncle Advice
The Separatory Funnel
The Stopper
The Teflon Stopcock
How to Extract and Wash What
The Road to Recovery—Back-Extraction
A Sample Extraction
Performing an Extraction or Washing
Extraction Hints
Exercises
CHAPTER 16 EXTRACTION AND WASHING: MICROSCALE
Mixing
Separation: Removing the Bottom Layer
Separation: Removing the Top Layer
Separation: Removing Both Layers
CHAPTER 17 SOURCES OF HEAT
Boiling Stones
The Steam Bath
The Bunsen Burner
The Heating Mantle
Proportional Heaters and Stepless Controllers
Exercise
CHAPTER 18 CLAMPS AND CLAMPING
Clamping a Distillation Setup
Clipping a Distillation Setup
CHAPTER 19 DISTILLATION
Distillation Notes
Class 1: Simple Distillation
The Distillation Example
The Distillation Mistake
Class 2: Vacuum Distillation
Class 3: Fractional Distillation
Azeotropes
Class 4: Steam Distillation
Steam Distillation Notes
Simulated Bulb-to-Bulb Distillation: Fakelrohr
Exercises
CHAPTER 20 MICROSCALE DISTILLATION
Like the Big Guy
Microscale Distillation II: The Hickman Still
The Hickman Still Setup
Hickman Still Heating
Recovering Your Product
A Port in a Storm
CHAPTER 21 THE ROTARY EVAPORATOR
Exercises
CHAPTER 22 REFLUX AND ADDITION
Standard Reflux
A Dry Reflux
Addition and Reflux
Exercise
CHAPTER 23 REFLUX: MICROSCALE
Addition and Reflux: Microscale
CHAPTER 24 SUBLIMATION
CHAPTER 25 MICROSCALE BOILING POINT
Microscale Boiling Point
Ultramicroscale Boiling Point
CHAPTER 26 CHROMATOGRAPHY: SOME GENERALITIES
Adsorbents
Separation or Development
The Eluatropic Series
CHAPTER 27 THIN-LAYER CHROMATOGRAPHY: TLC
We Don’t Make Our Own TLC Plates Any More, But...
The Plate Spotter
Spotting the Plates
Developing a Plate
Visualization
Interpretation
Multiple Spotting
Cospotting
Other TLC Problems
Preparative TLC
Exercises
CHAPTER 28 WET-COLUMN CHROMATOGRAPHY
Preparing the Column
Compounds on the Column
Visualization and Collection
Wet-Column Chromatography: Microscale
Flash Chromatography
Microscale Flash Chromatography
Exercises
CHAPTER 29 REFRACTOMETRY
The Abbé Refractometer
Before Using the Abbé Refractometer: A Little Practice
Using the Abbé Refractometer
Refractometry Hints
CHAPTER 30 GAS CHROMATOGRAPHY
The Mobile Phase: Gas
GC Sample Preparation
GC Sample Introduction
Sample in the Column
Sample at the Detector
Electronic Interlude
Sample on the Computer
Parameters, Parameters
Exercises
CHAPTER 31 HP LIQUID CHROMATOGRAPHY
The Mobile Phase: Liquid
HPLC Sample Preparation
HPLC Sample Introduction
Sample in the Column
Sample at the Detector
Sample on the Computer
Parameters, Parameters
Exercises
CHAPTER 32 INFRARED SPECTROSCOPY (AND A BIT OF UV-VIS, TOO)
Molecules as Balls on Springs
Ah, Quantum Mechanics
The Dissonant Oscillator
But Wait! There’s More
More Complicated Molecules
Correlation Tables to the Rescue
Troughs and Reciprocal Centimeters
Some Functional Group Analysis
A Systematic Interpretation
Infrared Sample Preparation
Running the Spectrum
The Fourier Transform Infrared (FTIR)
A Reflectance Attachment: Something to Think About
And UV-VIS Too!
Electrons Get to Jump
Instrument Configuration
Exercises
CHAPTER 33 NUCLEAR MAGNETIC RESONANCE
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
Be It Better Resolved . . .
Incredibly Basic FT-NMR
NMR Sample Preparation
Some NMR Terms and Interpretations
CHAPTER 34 THEORY OF DISTILLATION
Class 1: Simple Distillation
Class 3: Fractional Distillation
Class 4: Steam Distillation
INDEX
