9780716766384

Techniques in Organic Chemistry : Miniscale, Standard-Taper Microscale, Williamson Microscale

by ; ;
  • ISBN13:

    9780716766384

  • ISBN10:

    0716766388

  • Edition: 1st
  • Format: Paperback
  • Copyright: 2002-07-19
  • Publisher: W. H. Freeman

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Table of Contents

Preface ix
PART 1 BASIC TECHNIQUES 1(150)
Safety
2(14)
Causes of Laboratory Accidents
2(3)
Safety Features in Your Laboratory
5(1)
Preventing Accidents
6(2)
What to Do If an Accident Occurs
8(1)
Chemical Toxicology
9(2)
Where to Find Chemical Safety Information
11(3)
Protecting the Environment
14(2)
Laboratory Glassware
16(7)
Desk Equipment
17(1)
Standard Taper Miniscale Glassware
18(2)
Microscale Glassware
20(2)
Cleaning Laboratory Glassware
22(1)
The Laboratory Notebook
23(4)
Organization of the Laboratory Notebook
23(3)
Calculation of the Percent Yield
26(1)
Using Handbooks and Online Databases
27(5)
Handbooks
27(2)
Online Resources
29(3)
Measuring Mass and Volume
32(8)
Weighing
32(2)
Measuring Volume
34(6)
Heating and Cooling Methods
40(8)
Boiling Stones
41(1)
Heating Devices
41(6)
Cooling Methods
47(1)
Assembly of Reaction Apparatus
48(8)
Refluxing a Reaction Mixture
48(2)
Anhydrous Reaction Conditions
50(1)
Addition of Reagents During a Reaction
51(1)
Removal of Noxious Vapors
52(4)
Extraction and Drying Agents
56(22)
Extraction: The Theory
58(1)
Miniscale Extractions
59(2)
Additional Information About Extractions
61(3)
Summary of the Miniscale Extraction Procedure
64(1)
Using Pasteur Pipets to Transfer Liquids in Microscale Operations
65(2)
Microscale Extractions
67(5)
Equipment and Techniques Common to All Microscale Extractions
67(2)
Extractions with an Organic Phase More Dense Than Water
69(1)
Extractions with an Organic Phase Less Dense Than Water
70(2)
Drying Organic Liquids
72(2)
Methods for Separating Drying Agents and Organic Liquids
74(2)
Recovery of the Organic Product from the Dried Extraction Solution
76(2)
Recrystallization
78(15)
Theory of Recrystallization
78(3)
Selecting a Proper Recrystallization Solvent
81(1)
What to Do If No Crystals Appear in the Cooled Solution
82(1)
Pointers for Successful Recrystallizations
83(1)
Miniscale Procedure for Recrystallizing a Solid
83(5)
Removing Impurities from the Recrystallization Solution
86(2)
Summary of the Miniscale Recrystallization Procedure
88(1)
Microscale Recrystallization Methods
88(4)
Recrystallizing 300 Milligrams or Less of a Solid
89(1)
Recrystallizing up to 150 Milligrams of a Solid in a Craig Tube
90(2)
Summary of the Microscale Recrystallization Procedures
92(1)
Melting Points and Melting Ranges
93(11)
Melting Point Theory
93(3)
Apparatus for Determining Melting Ranges
96(2)
Determining Melting Ranges
98(3)
Mixture Melting Point
101(1)
Thermometer Calibration
102(1)
Summary of Melting-Point Determination
103(1)
Boiling Points and Distillation
104(29)
Determination of Boiling Points
104(2)
Boiling Points and Separation of Mixtures
106(3)
Simple Distillation
109(9)
Miniscale Short-Path Distillation
113(1)
Microscale Distillation Using Standard Taper Apparatus
113(3)
Microscale Distillation Using Williamson Apparatus
116(2)
Fractional Distillation
118(4)
Azeotropic Distillation
122(1)
Vacuum Distillation
123(6)
Steam Distillation
129(4)
Sublimation
133(3)
Assembling the Apparatus for a Sublimation
133(2)
Carrying Out a Sublimation
135(1)
Refractometry
136(4)
Theory of Refractometry
13.1(137)
The Refractometer
137(1)
Steps in Determining a Refractive Index
138(1)
Temperature Correction
139(1)
Optical Activity and Polarimetry
140(11)
Mixtures of Optical Isomers: Separation/Resolution
140(3)
Polarimetric Instrumentation
143(2)
Specific Rotation
145(1)
Using the Polarimeter
146(1)
Enantiomeric Excess (Optical Purity)
147(1)
Chiral Shift Reagents and Chiral Chromatography
147(4)
PART 2 CHROMATOGRAPHY 151(44)
Thin-Layer Chromatography
153(10)
Principles of Thin-Layer Chromatography
153(2)
Plates for Thin-Layer Chromatography
155(1)
Sample Application
156(2)
Development of a TLC Plate
158(1)
Choice of Developing Solvent
159(1)
Visualization Techniques
160(2)
Summary of TLC Procedure
162(1)
Gas-Liquid Chromatography
163(15)
Instrumentation
164(2)
Columns and Liquid Stationary Phases
166(3)
Detectors
169(1)
Interpreting Chromatograms
170(2)
Practical GC Operating Procedures
172(2)
Identification of Components Shown on a Chromatogram
174(1)
Quantitative Analysis
175(3)
Liquid Chromatography
178(17)
Adsorbents
179(2)
Elution Solvents
181(1)
Column Dimensions
182(2)
Preparing a Miniscale Column
184(1)
Elution Techniques
185(2)
Microscale Column Chromatography
187(2)
Summary of Column Chromatography Procedure
189(1)
Flash Chromatography
189(2)
High-Performance Liquid Chromatography
191(4)
PART 3 SPECTROSCOPIC METHODS 195(105)
Infrared Spectroscopy
197(27)
Theory of Molecular Vibration
197(1)
IR Spectrum
198(3)
IR Instrumentation
201(1)
Techniques of Sample Preparation
202(4)
Interpreting IR Spectra
206(11)
Sources of Confusion
217(7)
Nuclear Magnetic Resonance Spectroscopy
224(60)
NMR Instrumentation
225(3)
Preparing Samples for NMR Analysis
228(4)
Summary of Steps for Preparing an NMR Sample
232(1)
Interpreting NMR Spectra
232(1)
How Many Types of Hydrogens Are Present?
232(1)
Counting Hydrogens (Integration)
233(1)
Chemical Shift
234(9)
Spin-Spin Splitting (Coupling)
243(9)
Sources of Confusion
252(10)
Interpreting 1H NMR Spectra
262(8)
13C NMR
270(6)
DEPT Experiments
276(8)
Mass Spectrometry
284(16)
Mass Spectrometer
284(2)
The Molecular Ion
286(3)
High-Resolution Mass Spectrometry
289(1)
Fragmentation of the Molecule
290(6)
Case Study
296(2)
Sources of Confusion
298(2)
Integrated Spectroscopy Problems 300
Appendix The Literature of Organic Chemistry 1(1)
Index 1

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