Beschreibung
One of the very best things about organic chemistry is actually doing experimental work at the beneh. This applies not only at the profes sionallevel but also from the earliest stages of apprenticeship to the craft as a student. The fascination sterns from the nature of the sub ject itself, with its vast array of different types of reaction and its al most infinite variety of different chemical compounds. Each reaction and each new compound pose their own particular problems to chal lenge the skill and ingenuity of the chemist, whether working in a first-year teaching la bora tory or at the frontiers of research. This book is intended to provide basic guidance in the essential experimental techniques used in a typical undergraduate course. It gives concise coverage of the range of practical skills required, from first-year level when students may have no previous experience, up to final-year level when students are usually involved in more complex and dem an ding experimental work in supervised research projects. Our objective was to produce a handbook of techniques that could be used with a variety of practical courses throughout a student's whole period of study. Those who run practical courses generally have strong feelings about what particular experiments or exercises are appropriate for their own students, and it is rare that a book of experiments suitable for one department is acceptable to another.
Autorenporträt
Inhaltsangabe1 Introduction.- 1.1 The range of experimental techniques.- 1.2 Good laboratory practice.- 1.3 Safety in the laboratory.- 1.3.1 Chemical hazards.- 1.3.2 Fire hazard.- 1.3.3 Vacuum and pressure work.- 1.4 Keeping records.- 1.4.1 Recording experimental data.- 1.4.2 Final reports.- 1.5 Samples and spectra.- 2 Carrying out reactions.- 2.1 Basic techniques.- 2.1.1 Apparatus.- 2.1.2 Addition of reactants.- 2.1.3 Stirring reaction mixtures.- 2.1.4 Temperature control.- 2.1.5 Reactions under anhydrous conditions and inert atmospheres.- 2.2 Special techniques.- 2.2.1 The use of air-and water-sensitive reagents.- 2.2.2 Reactions in liquid ammonia.- 2.2.3 Catalytic hydrogenation.- 2.2.4 Photochemistry.- 2.2.5 Flash vacuum pyrolysis.- 3 Isolation and purification of reaction products.- 3.1 Primary work-up procedures.- 3.1.1 General considerations.- 3.1.2 Removal of solvent by rotary evaporator.- 3.1.3 Extraction procedures.- 3.1.4 Drying organic solutions.- 3.1.5 Separation of the target product(s).- 3.2 Crystallization.- 3.2.1 General principles.- 3.2.2 Melting point as a criterion of purity.- 3.2.3 Methods of crystallization.- 3.2.4 Choosing the crystallization solvent.- 3.2.5 Special topics.- 3.3 Melting point.- 3.3.1 General principles.- 3.3.2 Determination of melting point.- 3.3.3 Other methods.- 3.4 Distillation.- 3.4.1 General considerations.- 3.4.2 Simple distillation.- 3.4.3 Fractional distillation.- 3.4.4 Small-scale distillation.- 3.4.5 Molecular distillation.- 3.4.6 Steam distillation.- 3.4.7 Sublimation of solids.- 3.4.8 Appendices.- 4 Separation of organic mixtures by chromatography.- 4.1 Analytical methods.- 4.1.1 Thin-layer chromatography.- General description.- TLC plates and adsorbents.- Application of the sample.- Running (developing) the chromatogram.- Examining the chromatogram.- The use of TLC for qualitative analysis.- Choosing the developing solvent.- 4.1.2 Gas-liquid chromatography.- General description.- The instrument.- Injecting the sample.- Running the chromatogram.- Identification by GLC.- Quantitative analysis.- Recording GLC data.- Selection of the stationary phase and other operating parameters.- Setting up the instrument, some general points.- 4.1.3 High-performance liquid chromatography.- General description.- Equipment.- Operation of the equipment.- Qualitative and quantitative analysis.- Retention and resolution - basics.- Optimizing the separation.- Selection of the chromatographic mode.- Liquid - solid (adsorption) chromatography (LSC).- Liquid - liquid chromatography (LLC) on bonded phases.- 4.2 Preparative methods.- 4.2.1 Preparative thin-layer chromatography.- 4.2.2 Column chromatography.- General description.- Choosing the method.- Flash chromatography.- Dry-column flash chromatography.- Medium-pressure liquid chromatography.- Gravity-elution chromatography.- 4.3 Appendices.- 4.3.1 General principles of chromatographic separation.- 4.3.2 Control of adsorbent activity.- 4.3.3 Preparation of TLC plates.- Preparation of samples for spectroscopy.- 5.1 Infra-red.- 5.2 Nuclear magnetic resonance.- 5.3 Mass spectrometry.- 5.4 Ultraviolet.- Finding chemical information.- 6.1 Physical properties.- 6.2 Spectroscopic properties.- 6.3 Beilstein's Handbuch.- 6.4 Chemical Abstracts.
