Organic Laboratory Techniques

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9780534379810: Organic Laboratory Techniques
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This highly effective and practical manual is designed to be used as a supplementary text for the organic chemistry laboratory course - and with virtually any main text - in which experiments are supplied by the instructor or in which the students work independently. Each technique contains a brief theoretical discussion. Steps used in each technique, along with common problems that might arise. These respected and renowned authors include supplemental or related procedures, suggested experiments, and suggested readings for many of the techniques. Additionally, each chapter ends with a set of study problems that primarily stress the practical aspects of each technique, and microscale techniques are included throughout the text, as appropriate. Additional exercises, reference material, and quizzes are available online.

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INTRODUCTION TO THE ORGANIC LABORATORY Safety in the Laboratory / The Laboratory Notebook / Laboratory Equipment 1. CRYSTALLIZATION Solvents for Crystallization / Steps in Crystallization / Supplemental Procedures 2. MELTING POINTS Characteristics of Melting Points / Melting-Point Apparatus / Steps in Determining a Melting Point / Supplemental Procedures 3. EXTRACTION Immiscible Liquids / Distribution Coefficients / Extraction Solvents / Chemically Active Extraction / Steps in Extractions / Additional Techniques Used in Extractions / Other Extraction Techniques 4. DRYING ORGANIC SOLUTIONS Extraction with Aqueous Sodium Chloride / Solid Inorganic Drying Agents / Procedure for Using Solid Inorganic Drying Agents / Azeotropic Drying 5. SIMPLE DISTILLATION Characteristics of Distillation / Steps in a Simple Distillation / Microscale and Semi-Microscale Distillation 6. FRACTIONAL DISTILLATION Efficiency of the Fractionation Column / Steps in Fractional Distillation / Microscale Fractional Distillation 7. VACUUM DISTILLATION Boiling Point and Pressure / Apparatus for Simple Vacuum Distillation / Steps in Vacuum Distillation 8. STEAM DISTILLATION Characteristics of Steam Distillation / Calculation of the Amount of Water Needed in a Steam Distillation / Apparatus for Steam Distillation 9. SUBLIMATION Atmospheric Sublimation / Vacuum Sublimation 10. REFRACTIVE INDEX Correcting for Temperature Differences / Steps in Using a Refractometer 11. COLUMN CHROMATOGRAPHY Gravity Column Chromatography. Flash Chromatography (Macroscale) / Flash Chromatography (Microscale) / High-Performance Liquid Chromatography (HPLC) 12. THIN LAYER CHROMATOGRAPHY The RF Value / Equipment for TLC / Steps in a TLC Analysis / A Related Technique: Paper Chromatography 13. GAS CHROMATOGRAPHY Gas Chromatography / The Gas Chromatograph / Steps in a GC Analysis / Problems Encountered in GC / Uses of Gas Chromatograms 14. CARRYING OUT TYPICAL REACTIONS Stirring / Heating Reaction Mixtures / Controlling Exothermic Reactions / Adding Reagents to a Reaction Mixture. Excluding Moisture from a Reaction Mixture / Setting Up a Three-Neck Reaction Flask / Hydrogen Halide Gas Traps 15. INFRARED SPECTROSCOPY The Infrared Spectrum / Absorption of Infrared Radiation / Interpreting Infrared Spectra / Identifying Types of Compounds / Preparing a Sample for an Infrared Spectrum / Instrumentation 16. PROTON NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY The NMR Spectrum / Interpreting NMR Spectra / Use of Deuterium in Proton NMR Spectroscopy / NMR Spectra of Unknowns / The NMR Spectrometer / Preparing Samples for NMR Spectra 17. THE CHEMICAL LITERATURE Introduction to the Chemical Literature / Secondary Literature / Primary Literature / APPENDIX I. COMMONLY USED CALCULATIONS / Molarity / Normality / Dilutions / Percent Concentrations / Percent Yields and Theoretical Yields / APPENDIX II / ELEMENTAL ANALYSES / Determining the Empirical Formula / Determining the Molecular Formula / Interpreting the Results of Elemental Analysis / Degree of Unsaturation / APPENDIX III. HEALTH HAZARDS OF COMPOUNDS USED IN ORGANIC CHEMISTRY / Where to Find Chemical Hazard Information / Understanding Health Hazard Warnings

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