v
Contents
List of Figures ................................................................................................. xiii
List of Tables ....................................................................................................xxi
Preface ............................................................................................................ xxiii
Authors ............................................................................................................xxv
Chapter 1 General introduction .................................................................. 1
Chapter 2 Safety ............................................................................................. 3
2.1 Safety is your primary responsibility ................................................... 3
2.2 Safe working practice .............................................................................. 4
2.3 Safety risk assessments ........................................................................... 4
2.4 Common hazards .................................................................................... 5
2.4.1 Injuries caused by use of laboratory
equipment and apparatus ........................................................5
2.4.2 Toxicological and other hazards caused
bychemicalexposure ................................................................5
2.4.3 Chemical explosion and re hazards .....................................6
2.5 Accident and emergency procedures ................................................. 10
Bibliography ...................................................................................................... 10
Chapter 3 Keeping records of laboratory work ..................................... 13
3.1 Introduction ............................................................................................ 13
3.2 The laboratory notebook ....................................................................... 13
3.2.1 Why keep a lab book? ............................................................. 13
3.2.2 Laboratory records, experimental validity, and
intellectual property ............................................................... 14
3.2.3 How to write a lab book: Paper or electronic ...................... 15
3.2.4 Paper lab notebook: Suggested lab notebook format ......... 17
3.2.5 Electronic laboratory notebooks ............................................ 20
3.3 Keeping records of data ........................................................................ 21
3.3.1 Purity, structure determination, and characterization ...... 22
3.3.2 What types of data should be collected? ..............................22
3.3.3 Organizing your data records ............................................... 27
vi Contents
3.4 Some tips on report and thesis preparation ...................................... 29
3.4.1 Sections of a report or thesis .................................................. 31
3.4.2 Planning a report or thesis ..................................................... 31
3.4.3 Writing the report or thesis ....................................................33
Bibliography ...................................................................................................... 40
Chapter 4 Equipping the laboratory and the bench ............................. 41
4.1 Introduction ............................................................................................ 41
4.2 Setting up the laboratory ...................................................................... 41
4.3 General laboratory equipment .............................................................42
4.3.1 Rotary evaporators .................................................................. 42
4.3.2 Refrigerator and/or freezer .................................................... 42
4.3.3 Glass-drying ovens ................................................................. 42
4.3.4 Vacuum oven ............................................................................43
4.3.5 Balances .....................................................................................43
4.3.6 Kugelrohr bulb-to-bulb distillation apparatus ...................43
4.3.7 Vacuum pumps ........................................................................ 43
4.3.8 Inert gases ................................................................................. 44
4.3.9 Solvent stills ..............................................................................45
4.3.10 General distillation equipment ..............................................46
4.3.11 Large laboratory glassware .................................................... 47
4.3.12 Reaction monitoring ................................................................ 48
4.4 The individual bench ............................................................................ 48
4.4.1 Routine glassware ................................................................... 49
4.4.2 Additional personal items ......................................................50
4.4.3 Specialized personal items ..................................................... 50
4.4.3.1 Double manifold .....................................................50
4.4.3.2 Three-way Quickt gas inlet T taps ..................... 53
4.4.3.3 Filtration aids ...........................................................54
4.4.3.4 Glassware for chromatography ............................ 56
4.5 Equipment for parallel experiments ................................................... 58
4.5.1 Simple reactor blocks that attach to magnetic
stirrerhot plates ....................................................................... 59
4.5.2 Stand-alone reaction tube blocks...........................................60
4.5.3 Automated weighing systems ............................................... 60
4.5.4 Automated parallel dosing and sampling systems ............ 61
4.6 Equipment for controlled experimentation ....................................... 61
4.6.1 Jacketed vessels ........................................................................ 61
4.6.2 Circulating heater-chillers...................................................... 62
4.6.3 Peltier heater-chillers ..............................................................63
4.6.4 Syringe pumps ......................................................................... 63
4.6.5 Automated reaction control systems ....................................63
4.6.6 All-in-one controlled reactor and calorimeter systems .....63
viiContents
Chapter 5 Purication and drying of solvents ...................................... 65
5.1 Introduction ............................................................................................ 65
5.2 Purication of solvents ......................................................................... 65
5.3 Drying agents ......................................................................................... 66
5.3.1 Alumina, Al
2
O
3
........................................................................ 67
5.3.2 Barium oxide, BaO ................................................................... 67
5.3.3 Boric anhydride, B
2
O
3
.............................................................. 67
5.3.4 Calcium chloride, CaCl
2
.......................................................... 67
5.3.5 Calcium hydride, CaH
2
........................................................... 68
5.3.6 Calcium sulfate, CaSO
4
........................................................... 68
5.3.7 Lithium aluminum hydride, LiAlH
4
..................................... 68
5.3.8 Magnesium, Mg ....................................................................... 68
5.3.9 Magnesium sulfate, MgSO
4
.................................................... 68
5.3.10 Molecular sieves ....................................................................... 68
5.3.11 Phosphorus pentoxide, P
2
O
5
................................................... 69
5.3.12 Potassium hydroxide, KOH .................................................... 69
5.3.13 Sodium, Na ............................................................................... 69
5.3.14 Sodium sulfate, Na
2
SO
4
.......................................................... 70
5.4 Drying of solvents ................................................................................. 70
5.4.1 Solvent drying towers ............................................................. 70
5.4.2 Solvent stills .............................................................................. 71
5.4.3 Procedures for purifying and drying
common solvents ..................................................................... 74
5.4.4 Karl Fisher analysis of water content .................................... 79
References ......................................................................................................... 79
Chapter 6 Reagents: Preparation, purication, and handling ........... 81
6.1 Introduction ............................................................................................ 81
6.2 Classication of reagents for handling ............................................... 81
6.3 Techniques for obtaining pure and dry reagents ............................. 82
6.3.1 Purication and drying of liquids ........................................83
6.3.2 Purifying and drying solid reagents .................................... 85
6.4 Techniques for handling and measuring reagents ........................... 87
6.4.1 Storing liquid reagents or solvents under an
inertatmosphere ...................................................................... 87
6.4.2 Bulk transfer of a liquid under inert
atmosphere(cannulation) ....................................................... 89
6.4.3 Using cannulation techniques to transfer measured
volumes of liquid under inert atmosphere .......................... 91
6.4.4 Use of syringes for the transfer of reagents or
solvents ...................................................................................... 94
6.4.5 Handling and weighing solids under
inert atmosphere .................................................................... 102

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