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Laboratory Methods of Organic Chemistry - Sciencemadness Dot Org

Laboratory Methods of Organic Chemistry - Sciencemadness Dot Org

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CONTENTS<br />

A. SOME GENERAL LABORATORY RULES<br />

Reaction Velocity and Temperature . . . . . .<br />

PAGE<br />

1<br />

Purification <strong>of</strong> <strong><strong>Org</strong>anic</strong> Substances . . . . . . 3<br />

Crystallisation . . . . . . . . 4<br />

Chromatographic adsorption . . . . . . 14<br />

Distillation . . . . . . . . . 15<br />

Sublimation . . . . . . . . . 26<br />

Distillation with Steam . . . . . . . 27<br />

Evaporation <strong>of</strong> Solvents . . . . . . . 29<br />

Extraction . . . . . . . . . 32<br />

Working with Compressed Gases . . . . . .35<br />

Heating under Pressure . . . . . . . 37<br />

Stirring and Shaking . . . . . . . . 38<br />

Determination <strong>of</strong> the Melting Point . . . . . . 40<br />

B. ORGANIC ANALYTICAL METHODS<br />

Detection <strong>of</strong> Carbon, Hydrogen, Nitrogen, Sulphur, and the Halogens . 43<br />

<strong><strong>Org</strong>anic</strong> Elementary Analysis . . . . . . 46<br />

I. Determination <strong>of</strong> Nitrogen by Dumas' Method . . .47<br />

II. Determination <strong>of</strong> Carbon and Hydrogen by Liebig's Method . 55<br />

III. Determination <strong>of</strong> Halogen, Sulphur, and other Elements . . 69<br />

1. Determination <strong>of</strong> halogen by the Carius method, p. 69; 2.<br />

Argentometric determination <strong>of</strong> chlorine and bromine, p. 73;<br />

3. Iodine determination by the Leipert-Munster method, p. 76;<br />

4. Determination <strong>of</strong> sulphur by the Carius method, p. 77; 5. Determination<br />

<strong>of</strong> sulphur by combustion, p. 78; 6. Simultaneous<br />

determination <strong>of</strong> halogen and sulphur, p. 79; 7. Determination<br />

<strong>of</strong> other elements, p. 79.<br />

IV. Determination <strong>of</strong> <strong><strong>Org</strong>anic</strong> Groups . . . . .80<br />

1. Volumetric determination <strong>of</strong> methoxyl and ethoxyl, p. 80;<br />

2. Determination <strong>of</strong> the acetyl and benzoyl groups, p. 82; 3.<br />

Determination <strong>of</strong> active hydrogen by the method <strong>of</strong> Tschugaeff<br />

and Zerevitin<strong>of</strong>f, p. 84.<br />

V. Determination <strong>of</strong> Molecular Weight . . . . .86

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