Buch, Englisch, 384 Seiten, Format (B × H): 210 mm x 280 mm, Gewicht: 1102 g
A Comprehensive Laboratory Experience
Buch, Englisch, 384 Seiten, Format (B × H): 210 mm x 280 mm, Gewicht: 1102 g
ISBN: 978-0-471-61996-3
Verlag: John Wiley & Sons
This text is intended to provide students with instruction and valuable laboratory experience in the often neglected area of inorganic chemistry. Divided into four main parts, the book covers chemistry of the main group elements, chemistry of the transition metals, organometallic chemistry, and bioinorganic chemistry. Recognizing the high cost of materials, difficulties in waste disposal, and dangers of toxicity, the authors have adopted a ``microscale'' approach to experiments in the book, thereby also reducing the time students spend in preparation. With over 45 experiments, Microscale Inorganic Chemistry incorporates the use of a broad sampling of elements and also covers such topics as laboratory safety, equipment, report writing, and literature searching.
Autoren/Hrsg.
Weitere Infos & Material
List of Tables xvii
Introduction 1–3
A. A Brief History of Inorganic Chemistry 1
B. The Microscale Approach 2
C. A Word to the Student 3
Chapter 1 Safety in the Laboratory 5–17
1.A General Safety Rules 5
1.A.1 Introduction 5
1.A.2 Before the Laboratory 6
1.A.3 Safety Rules in the Laboratory 6
1.B Planning for Chemicaly Safety 8
1.B.1 Introduction 8
1.B.2 Use of MSD Sheets 8
1.B.3 The Merck Index 12
1.B.4 Compressed Gas Cylinders and Lecture Bottles 13
1.B.5 Fire Safety 16
Chapter 2 Laboratory Equipment 19–29
2.A Glassware 19
2.B Other Locker Equipment 21
2.C Measuring Quantities of Chemicals 22
2.C.1 Weighing 22
2.C.2 Liquid Volumes 22
2.D Heating Methods 25
2.D.1 The Microburner 25
2.D.2 Steam Bath 25
2.D.3 Oil Baths 25
2.D.4 Infrared Lamp 26
2.D.5 Sand Bath or Aluminum Block with Magnetic Stirring Hot Plate 26
2.E Stirring 27
2.F Reflux and Distillation 27
Chapter 3 Writing Laboratory Reports 31–35
3.A Introduction 31
3.B Maintenance of the Laboratory Notebook 31
3.C The Laboratory Report 34
3.D Proper Citation and Plagiarism 35
Chapter 4 Literature Searching and the Inorganic Literature 37–47
4.A Literature Searching 37
4.A.1 Chemical Abstracts Method 37
Searching a Topic in Chemical Abstracts 38
Use of the Formula Index 38
Use of the General Subject Index 40
CAS Online 40
Advantages and Disadvatages of Chemical Abstracts 40
4.A.2 Use of the Science Citation Index 41
Searching Using the Printed Science Citation Index 41
Searching Using the Compact Disc Science Citation Index 42
Searching Using the Citation Index 42
Advantages and Disadvatages of the Science Citation Index 44
4.A.3 Comparison of the Two Methods 44
4.B The Inorganic Chemical Literature 44
4.B.1 Introduction 44
4.B.2 Purely Inorganic Journals 44
4.B.3 General Coverage Journals 45
4.B.4 Review Journals and Monographs Covering Inorganic Chemistry 45
4.B.5 Major Comprehensive Books on Inorganic Chemistry 46
Chapter 5 Inorganic Microscale Laboratory Techniques 49–105
5.A Microscale Determination of Magnetic Susceptibility 49
5.A.1 Introduction 49
5.A.2 Measurement of Magnetic Susceptibility 50
5.A.3 Calculation of Magnetic Moment from Magnetic Susceptibility 52
5.A.4 Operation of the Evans–Johnson Matthey Balance for Solids 54
5.A.5 Operation for Liquids and Solutions 55
5.A.6 Determining Magnetic Susceptibility by NMR Spectroscopy 56
5.B Thermal Analysis 57
5.B.1 Introduction 57
5.B.2 Differential Scanning Calorimetry and Differential Thermal Analysis 57
5.B.3 Thermogravimetric Analysis 58
5.B.4 Variables in Thermal Analysis 58
5.B.5 Analysis of the Thermogram 59
5.B.6 Theoretical Aspects 60
5.B.7 Applications 61
5.C Vacuum and Inert Atmosphere Techniques 62
Introduction 62
5.C.1 Purging with an Inert Gas 62
5.C.2 Use of Manifold for Inert Gas or Vacuum 64
Rough Pump 64
Cold Trap 64
Manifold 65
Multiple Vacuum Lines in Series 65
Use and Operation of Manifolds 65
5.C.3 Cannula Techniques 66
5.D Crystallization Techniques 67
5.D.1 Introduction 67
5.D.2 Crystallization from Solution 67
5.D.3 Isolation of Crystalline Products (Suction Filtration) 69
5.D.4 The Craig Tube Method 69
5.D.5 Recrystallization Pipet 70
5.D.6 Removal of Suspended Particles from Solution 71
5.D.7 Washing of the Collected Crystals 71
5.D.8 Decolorization 72
5.D.9 Drying Techniques 73
5.E Determination of Melting Points 74
5.E.1 Introduction 74
5.E.2 Theory 74
5.E.3 Mixture Melting Point Determination 75
5.E.4 Correcting Melting Points 76
5.E.5 Determination of the Melting Point Range 77
5.E.6 Melting Point Apparatus 78
The Thiele Tube 78
The Mel-Temp Apparatus 78
The Fisher–Johns Apparatus 78
The Thomas–Hoover Apparatus 81
5.F Concentration of Solutions 81
5.F.1 Introduction 81
5.F.2 Evaporation Techniques 81
5.F.3 Removal of Solvent Under Reduced Pressure 81
5.G Chromatography 82
5.G.1 Introduction 82
5.G.2 Thin-Layer Chromatography 84
5.G.3 Gas Chromatography: Introduction 86
Components of the Gas Chromatograph 87
5.G.4 Liquid Chromatography 89
Ion and Ion Exchange Chromatography 89
High-Performance Liquid Chromatography 90
5.H Sublimation 92
5.H.1 Introduction 92
5.H.2 Theory 93
5.H.3 Sublimation Technique 93
5.I Solvent Extraction 94
5.I.1 Introduction 94
5.I.2 Theory 94
5.I.3 Extraction Procedures: Simple Extraction 97
Use of the Separatory Funnel 97
Pasteur Filter Pipet Extractions 99
5.I.4 Continuous Extraction 100
5.I.5 Drying of the Wet Organic Layer 100
5.I.6 Drying of Organic Solvents 101
5.J Conductivity Measurements 102
5.J.1 Introduction 102
5.J.2 Experimental Procedure 104
5.J.3 Non-Aqueous Solutions 105
Chapter 6 Spectroscopy 107–146
6.A Introduction 107
6.A.1 Spectrometer Components 108
6.B Visible Spectroscopy 109
6.B.1 Introduction and Theory 109
6.B.2 The Visible Spectrum 110
6.B.3 Molar Absorbance and Color 111
6.B.4 Size of the Crystal Field Splitting 112
6.B.5 Energy Level Diagrams l12
6.C Infrared Spectroscopy 114
6.C.1 Introduction 114
6.C.2 Sample Handling 115
6.C.3 Bond Vibrations 1l6
6.C.4 Vibrational Modes 119
6.C.5 Inorganic Functional Groups 121
6.C.6 Synergistic Effects 121
6.C.7 Interpretation of IR Sp
