Experimental Organic Chemistry - Daniel R Palleros

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Résumé :

Section 1 The Basics 1

Unit 1 Laboratory Safety 3

1.1 General Safety Guidelines 3

1.2 Chemical Toxicity 6

1.3 Dealing with Chemicals and Waste Disposal 7

1.4 Online Safety Resources 15

Unit 2 Basic Concepts 19

2.1 Polarity and H-Bonds 19

2.2 Physical Data 23

2.3 Solvents 24

2.4 Balancing Chemical Equations 26

2.5 Concentration Units 28

2.6 Moles and Millimoles 29

2.7 Mineral Acids 31

2.8 Calculation of Yields 32

2.9 Scaling Up, Scaling Down 34

2.10 Keeping Lab Books and Writing Lab Reports 34

2.11 Chemical Literature 35

Unit 3 Basic Operations 45

3.1 Handling Liquids 45

3.2 Heating 46

3.3 Filtration 47

3.4 Refluxing 51

3.5 Evaporation 53

3.6 Centrifugation 55

3.7 Caring for Glassware 55

3.8 Measuring Pressure 57

Section 2 The Experiments 59

Unit 4 Recrystallization and Melting Point 61

4.1 Overview 61

4.2 Recrystallization 62

4.3 Decolorizing Charcoal 69

4.4 Recrystallization from Mixed Solvents 70

4.5 Microscale Recrystallization 70

4.6 Melting Point 71

4.7 Sublimation 75

Experiment 4 Recrystallization of Acetanilide and Urea 79

E4.1 Recrystallization of Acetanilide 80

E4.2 Microscale Recrystallization of Urea 82

E4.3 Determination of Melting Points 82

Unit 5 Extraction 86

5.1 Introduction 86

5.2 Solvent-Solvent Partitioning 86

5.3 Macroscale Liquid-Liquid Extraction 92

5.4 Microscale Liquid-Liquid Extraction 93

5.5 Drying the Organic Layer 94

5.6 Solid-Liquid Extraction 95

5.7 Countercurrent Distribution 97

Experiment 5 Isolation of Caffeine from Tea 103

E5.1 Tea, Coffee, and Caffeine 103

E5.2 Caffeine from Tea: Overview of the Experiment 105

E5.3 Isolation of Caffeine 109

E5.4 Purification of Caffeine by Sublimation 110

E5.5 Purification of Caffeine by Recrystallization (Alternative Procedure) 111

Unit 6 Distillation - Separation and Purification of Organic Liquids 113

6.1 Boiling Point 113

6.2 Boiling Point and Molecular Structure 114

6.3 Simple Distillation 115

6.4 Fractional Distillation 120

6.5 Ideal and Nonideal Solutions 123

6.6 Azeotropic Mixtures 124

6.7 Fractionating Columns 125

6.8 Microscale Distillation 126

6.9 Boiling Point Determination 128

6.10 Vacuum Distillation 129

6.11 Steam Distillation 130

Experiment 6A Distillation of Alcohols 136

E6A.1 Distillation of Methanol from a Mixture with Ferric Chloride 136

E6A.2 Separation of Methanol-Water by Simple Distillation 137

E6A.3 Separation of Methanol-Water by Fractional Distillation 138

E6A.4 Analysis of the Distillation Fractions by Density 139

Experiment 6B Isolation of Anise Oil 142

E6B.1 Overview 142

E6B.2 Isolation of Anise Oil 142

Unit 7 Gas Chromatography 144

7.1 Introduction 144

7.2 The Chromatographic Methods 144

7.3 Partition Chromatography 146

7.4 Gas Chromatography 149

7.5 The Gas Chromatograph 151

7.6 Measuring the Retention Time 155

7.7 Integration 156

7.8 Quantitative Analysis 157

7.9 Quantitative Analysis: A Closer Look (Advanced Level) 158

7.10 Qualitative Analysis 161

7.11 Running GC: Step by Step 162

7.12 Gas Chromatography Do's and Don'ts 163

Experiment 7A Gas Chromatography of Alcohols 167

E7A.1 Analysis of Alcohols 167

E7A.2 Separation...

Sommaire:

Daniel R. Palleros is the author of Experimental Organic Chemistry, published by Wiley....