Shake cleaning

During any separations, if the phases do not immediately separate, c. 5 per cent v/v methanol should be added. After very brief shaking, clean phase separation generally occurs, leaving an almost clear organic phase below a milky aqueous phase. 

Food containing >70% fat dissolve sample in isooctane and shake clean-up On florisil column... 

Collection in brown Winchester bag addition of 20% aqueous MeOH with shaking clean-up on Sep-Pak C-j 3 cartridge column... 

Saponification extraction with hexane addition of DMSO shaking clean-up on silica gel... 

Shake cleaning, as the name implies, involves switching off the exhaust fan and flexing the filter elements (or sleeves) with the aid of a shaking mechanism, either manually, as in traditional units, or automatically. In both cases the effect is to release the dust, which then falls into a hopper for collection and removal (Fig. 3.3). In this type of collector, the filter sleeves, which may be up to 10 m in length, are suspended under controlled tension from the arm of a flexing mechanism, which effects the cleaning action. 

The design requirements include resistance to stretching from the mass of the dust cake, resistance to flex fatigue from the shake cleaning mechanism, a surface that will facilitate efficient dust release, and a construction that will affect maximum particle capture whilst at the same time providing minimum resistance to gas flow. 

Mercury-mercurous chloride. This is probably the most widely used reference electrode. It is reversible to chloride ion and is usually made up in saturated aqueous potassium chloride solution, although Irnoldm " and O.lmoldm solutions are also common. In commercial electrodes, the solution is often retained with a porous plug or ceramic frit saturated aqueous KCl, being very dense, easily leaks out. A separate compartment will therefore be necessary for the reference electrode if chloride ions must be kept out of the working solution. Calomel electrodes can easily be prepared by shaking clean dry mercury with the powdered mercurous chloride which forms a skin around the mercury. The chloride ion solution is then carefully poured on top to complete the electrode. Home-made calomel electrodes can have a very low resistance and high performance. 

First place about 5 g. of clean dry sand in A, and then 45 ml. (3 S ) rectified spirit cool the flask in ice-water and cautiously add 40 ml. (74 g.) of concentrated sulphuric acid, shaking the mixture thoroughly during the addition to ensure a... 

Reactions of Aspirin, (i) Distinction from Salicylic acid. Shake up with water in two clean test-tubes a few crystals of a) salicylic acid, (0) aspirin, a very dilute aqueous solution of each substance being thus obtained. Note that the addition of i drop of ferric chloride solution to (a) gives an immediate purple coloration, due to the free —OH group, whereas (b) gives no coloration if the aspirin is pure. 

Prepare the acetylating mixture by adding i volume of acetic anhydride to 4 volumes of pure anhydrous pyridine, and shaking thoroughly. Immediately before use, transfer the mixture to a clean dry burette having a welUfitting glass tap, and then close the top of the burette by means of a soda-lime tube. 

In practice, it is best to purify a quantity, say one Winchester quart bottle, of technical 0 720 ether to cover the requirements of a group of students. The Winchester quart of ether is divided into two approximately equal volumes, and each is shaken vigorously in a large separatory funnel with 10-20 ml. of the above ferrous solution diluted with 100 ml. of water. The latter is removed, the ether transferred to the Winchester bottle, and 150-200 g. of anhydrous calcium chloride is added. The mixture is allowed to stand for at least 24 hours with occasional shaking. Both the water and the alcohol present are thus largely removed. The ether is then filtered through a large fluted filter paper into another clean dry Winchester bottle (CAUTION all flames in the vicinity must be... 

Xanthhydrol. Prepare an amalgam from 9 0 g. of clean sodium and 750 g. (55 ml.) of mercury (Section 11,50,7, Method 1), and warm it to 50° in a 500 ml. Pyrex bottle. Add a cold suspension of 25 g. of xanthone in 175 ml. of rectified spirit, stopper the bottle and shake vigorously raise the stopper from time to time to release the pressure. The temperature rises rapidly to 60-70°, the sohd xanthone passes into solution, and a transient blue colour is developed. After about 5 minutes the alcoholic solution is clear and almost colourless. Shake for a further 10 minutes, separate the mercury, and wash it with 15 ml. of alcohol. Filter the... 

In a 2 litre round-bottomed flask, fitted with a double surface reflux condenser, place 11-5 g. of clean sodium. Add 250 ml. of absolute alcohol in one portion if the reaction is unduly vigorous, immerse the flask momentarily in ice. When all the sodium has reacted, add 80 g. (76 ml.) of ethyl malonate (Section 111,153), followed by a solution of 30 g. of dry urea in 250 ml. of hot (ca. 70°) absolute alcohol. Shake the mixture well, fit a calcium chloride (or cotton wool) guard tube to the top... 

---