Manipulation on a Semi-micro Scale

Introduction. When only very small quantities of organic materials are available their manipulation must necessarily be carried out on a correspondingly small scale. This occurs frequently in research problems, but small-scale preparative work is often of value to the student because considerable economy of materials and of time can be achieved. It is emphasised, however, that the proper training for the organic chemist must rest upon the correct understanding and thorough practice of the manipulations on the macro-scale already described, and that he should consider small-scale work as a sequel to and not as a replacement of the above standard techniques. 

Preparative work is sometimes divided into three categories. This division is entirely arbitrary and the categories overlap, but they may conveniently be classified thus  

The difficulties of working with small quantities of liquids are much greater than with small quantities of solids. For example a competent worker can, and does in fact, often work with 100 mg, of solid without any special apparatus. With liquids this is often not practicable because of the much greater losses entailed, particularly when it is realised that one ordinary-sized drop weighs about 50-100 mg. The account which follows gives details of modifications of standard apparatus suitable for the semi-micro scale defined above. 

General Considerations. With liquids and solutions the most serious losses are due to (a) transference from spherical flasks and difficulties of drainage, (b) retention by filter-papers, (c) absorption by large corks. As containers for small quantities of liquids it is therefore often convenient to use pear-shaped flasks A and conical test-tubes or centrifuge-tubes B (Fig. 29). (In this and subsequent figures, approximate dimensions are given to indicate a convenient size.) 

The transference of a liquid from one vessel to another is best carried out by means of a dropping pipette A (Fig. 30). For measuring out a definite volume of liquid it is obviously an advantage to have a calibrated pipette B (Fig. 30) of i or 5 ml. total capacity. Alternatively, semi-micro burettes reading to 0 02 ml. are particularly convenient for class work. 

---

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. 

---