Description
This 1989 book describes the physico-chemical principles of the high vacuum techniques used by chemists. It is a guide to the choice of suitable equipment, the methods of constructing the systems, and the ways of using them. Professor Plesch's book is the only up-to-date work on the type of high vacuum systems (HVS) used by chemists and it is the first ever to describe in detail the actual construction, manifold uses, method of operation, and final dismantling of an HVS. It includes descriptions of a very wide range of devices for making measurements (conductivity, spectra, kinetics, etc.) in vacuum. The author draws on over 40 years of his own experiences and those of others in many parts of the world, and many of the tricks and gadgets have not been published before. The book will be an essential companion on the bench of every chemist involved in the synthesis of, or measurements on, air-sensitive compounds.
Chapter
1.1. Reasons for using high vacuum techniques
1.1.2. The Inert gas blanket
1.1.3. Dry-bag and dry-box
1.2. Theoretical considerations
1.2.3. General structure of a high vacuum system
1.2.5. Some physico-chemical features peculiar to closed systems
1.3. Essential skills and equipment
1.3.3. Some unconventional devices
1.4. General comments on safety
2.1.1. Guiding principles
2.1.2. The foundations: the bench and the frame
2.2. Individual components
2.2.3. The main manifold or trunk line
2.3. Building, operating, testing and dismantling the vacuum line
2.3.1. Building and operating
2.3.2. Hunting and repairing leaks
2.4. The PlEgli and Krummenacher valves
3. APPLIANCES AND PROCEDURES
3.1. Measuring devices and related manipulations
3.1.3. Calibrated vessels with glass break-seals
3.1.4. Phial filler for large volumes
3.1.5. Metering compounds by volume of vapour
3.1.8. UV-vis. spectroscopic measurements
3.1.10. Conductance and other electrical measurements
3.2. Combined measuring devices
3.2.1. General considerations
3.2.2. Isothermal reactors
3.2.3. Adiabatic reactors (reaction calorimeters)
4. PURIFICATION, INCLUDING DRYING
4.2. Definitions, relevance and measures of purity
4.2.1. Definitions and relevance
4.2.2. Measures of purity
4.3. Cleaning the apparatus
4.4. The cleaning of solvents and reagents
4.4.1. General introduction
4.4.4. Purification of catalysts
4.5. Determination of purity
4.5.2. Effects on physical properties
4.5.4. Electroanalytical methods
4.5.5. Detection and estimation of impurities by separation
4.5.6. Functional tests of purity
4.6. What is so special about drying?
4.6.1. The drying process
4.6.2. Some drying agents
4.6.3. The special hazards of drying
5. CHEMICAL OPERATIONS WITH HIGH VACUUM SYSTEMS
5.2.1. Sodium ethoxide by the cascade method
5.2.2. n-Butoxytitanium trichloride
5.2.3. Tertiary silyl lithium compounds
5.2.4. 1,3-Dioxolenium salts
5.2.5. Electrochemical preparation of stannic chloride
5.2.6. Aluminium chloride
5.3.1. Electrical conductivity and UV measurements
5.3.2. Combined UV and ESR spectroscopy
5.3.4. Polymerisation kinetics by gel permeation chromatography (GPC)
5.3.5. Precision calorimetry
Appendix Suppliers of vacuum equipment
High Vacuum Techniques for Chemical Syntheses and Measurements
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