Manipulation semi-micro

The preparations of all the derivatives, and all the hydrolyses of esters, anilides, etc., described in Part III, provide excellent practice in semi-micro manipulation. 

Two simple methods for the semi-micro estimation of halogens are available, (a) the Carius method, and (b) the Parr bomb method. It should be emphasised that there are other methods available for these estimations on the true micro scale, but they do not lend themselves, by virtue of the balances, apparatus and manipulation required, to semi-micro work, or to the intermittent usage which class-work necessarily entails. 

First, considerably greater emphasis has been placed on semimicro techniques and their application to preparations, separations, analysis and physical determinations such as those of molecular weight. We have therefore greatly expanded the section on Manipulation on a semi-micro scale which was in the Third Edition, and we have described many more preparations on this scale, some independent and others as alternatives to the larger-scale preparations which immediately precede them. Some 40 separate preparations on the semi-micro scale are described in detail, in addition to specific directions for the preparation of many classes of crystalline derivatives required for identification purposes. The equipment required for these small-scale reactions has been selected on a realistic basis, and care has been taken not to include the very curious pieces of apparatus sometimes suggested as necessary for working on the semi-micro scale. 

We have also added an entirely new section dealing with semi-microanalysis. In our original Introduction (p. ix) we justified the retention of macro-methods of quantitative analysis on the grounds that they formed an excellent introduction to micromethods and also afforded a valuable training in exact manipulation generally. By now, however, the macro-estimation particularly of carbon and hydrogen and of nitrogen has disappeared entirely from most laboratories. On the other hand, the micro-... 

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