Glass ground

Ensure that all the individual components in the assembly are adequately supported when in position the friction between contiguous ground-glass surfaces does not provide adequate support. Therefore always use clamps, the claws of which are lined with rubber or other soft material. When assembling apparatus, allow some play in the clamps until the individual parts are in position, and then secure the position of the assembly by gently increasing the pressure of the clamps. 

It is often advisable to lubricate ground-glass joint surfaces with an extremely thin film of vaseline. This applies particularly to joints employed in assemblies for distillation under reduced pressure. For distillations under greatly reduced pressures or at very high temperatures it is essential to employ a special lubricant, e.g., silicone grease. 

Although apparatus employing ground-glass joints is excellent for work on a macro scale, it is not always suitable for very small-scale work as the joints are often disproportionately large compared with the rest of the assembly. The semi-micro apparatus described on pp. 59-72 can therefore be considered as being of general utility for this scale of work, especially as the use of corks has been reduced to a minimum. 

Units. Some of the chief units employed for reasonably simple ground glass assemblies are ... 

This brief account is intended to give only a general indication of the types of apparatus available. The firm which has pioneered the design and manufac ture of ground- glass apparatus is Quickfit and Quartz, Ltd., Quickfit Works,... 

The distillation heads Fig. 22(F) and Fig. 22(G) can be fitted with thermometers having a ground-glass cone just above the bulb (Fig. 22(M)). These are expensive, and it is usually more convenient to fit a thermometer pocket (Fig. 22(N)) which consists of a small well , fitting as shown into the neck of the flask. A small volume of mercury is placed in the well just to cover the bulb of a conventional thermometer, and thus provides excellent thermal contact between the thermometer and the sides of the pocket. 

Spray. For most purposes a simple spray device, based on the ordinary scent-spray, suffices. A finer and less intermittent spray can be obtained using the apparatus shown in Fig. 26. A narrow glass cylinder J has a ground-glass... 

The latter is connected above to a water-condenser and below to a flask which contains a liquid of appropriate boiling-point. The inner tube is connected to a water-pump. A more satisfactory pistol (Fig. 48(B)) consists of a wide glass tube A closed at each end by ground-glass caps. 

In most of these prcpiirations. the corks or rubber-bungs can be replaced by ground-glass joints (pp. 42-47). 

Fit a 500 ml. bolt-head flask F with a well-fitting cork which is free from flaws, and which carries a dropping-funnel D and a delivery tube (or knee-tube ) T, the latter being connected to a water-condenser C (Fig. 52). Attach an adaptor A to the lower end of the condenser. (Alternatively, use a ground-glass flask (Fig. 22(a), p. 43) with a distillation-head (Fig. 22(F)) the dropping-funnel can be fitted into the distillation-head, the side-arm of which is connected to a condenser as in Fig. 23(0), p. 45.)... 

The absolute ethanol obtained in this way should have d., o 794, It is very hygroscopic, and the bottle in which it is stored should preferably have a well fitting ground-glass stopper alternatively, the bottle can be closed with a tightly fitting rubber stopper but not with a cork, as corks contain appreciable quantities of water. 

Dissolve 1 g. of powdered benzophenone in 6-7 ml. of cold isopropanol with shaking, add 1 drop of glacial acetic acid, and then confine the solution either in a glass receiver having a ground-glass stopper, or in a tube which is sealed... 

This preparation must be performed in a fume-cupboard, because nitrous fumes are evolved during the nitration. A ground-glass flask and air condenser (Fig. 22(a) and (c), p. 43) should preferably be used. 

Both the primary amine (D) and the tertiary amine (E) are reasonably strong bases, and will absorb carbon dioxide if exposed to the air. They should therefore be stored in ground-glass stoppered bottles or in sealed tubes. 

For this preparation, which must be performed in the fume-cupboard, assemble the apparatus shown in Fig. 67(A). C is a 150 ml. distilling-flask, to the neck of which is fitted a reflux single-surface water-condenser D, closed at the top E by a calcium chloride tube. The side-arm of C carries a cork F which fits the end E of the condenser for subsequent distillation. The side-arm of C is meanwhile plugged by a small rubber cork, or by a short length of glass rod. (Alternatively, use the ground-glass flask and condenser (Fig. 22 (a) and (c), p. 43), and... 

Fit two similar 250 ml. conical flasks, A and B, with reflux water-condensers (using ground-glass joints or rubber stoppers) and connect the condensers in series as before over two water-baths. Prepare a mixture of 2 volumes of acetic anhydride and i volume of glacial acetic acid,... 

Apparatus. The apparatus is made of Pyrex glass, in one piece. It consists of a shaped bulb A (Fig. 89 of about 30 ml. capacity in which the reaction takes place, provided with an inclined inlet B at the side and a vertical ascension tube D. B serves not only as an inlet for the admission of the carrier gas but also as the route by which the reagents and test sample are introduced into the apparatus. B ends in a small ground-glass joint into which fits ajoint carrying a capillary-tube which projects well down into the bulb A (the end of the capillary should be just above the liquid level when the apparatus is charged for the determination). The upper extension of this capillary beyond the joint is provided with a tap C to control the rate of flow of the carrier gas. 

Some simple apparatus, suitable for high vacuum distillation, are collected in Figs. 11, 26, 1-4. Fig. 11, 26, 1 represents an apparatus, which is particularly well adapted for solids the ground glass joint must be lubricated with a grease of negligible vapour pressure. Hickman s vacuum still is shown in Fig. 11, 26, 2 it is about 60 mm. in diameter. 

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