Funnel Volume

Fig 5. 47 Relationship between funnel volume and quantity of explosive in the in—sand test of Enoki No. 2 dynamite... 

Cuvettes, 1, 2 and 5 cm Separating funnel, volume approx. 250 ml Measuring flask, volume 50 ml Phosphate solution ... 

For these sequences the value of Gj, is less than a certain small value g. For such sequences the folding occurs directly from the ensemble of unfolded states to the NBA. The free energy surface is dominated by the NBA (or a funnel) and the volume associated with NBA is very large. The partition factor <6 is near unify so that these sequences reach the native state by two-state kinetics. The amplitudes in (C2.5.7) are nearly zero. There are no intennediates in the pathways from the denatured state to the native state. Fast folders reach the native state by a nucleation-collapse mechanism which means that once a certain number of contacts (folding nuclei) are fonned then the native state is reached very rapidly [25, 26]. The time scale for reaching the native state for fast folders (which are nonnally associated with those sequences for which topological fmstration is minimal) is found to be... 

Ethyl bromide soon distils over, and collects as heavy oily drops under the water in the receiving flask, evaporation of the very volatile distillate being thus prevented. If the mixture in the flask A froths badly, moderate the heating of the sand-bath. When no more oily drops of ethyl bromide come over, pour the contents of the receiving flask into a separating-funnel, and carefully run oflF the heavy lower layer of ethyl bromide. Discard the upper aqueous layer, and return the ethyl bromide to the funnel. Add an equal volume of 10% sodium carbonate solution, cork the funnel securely and shake cautiously. Owing to the presence of hydrobromic and sulphurous acids in the crude ethyl bromide, a brisk evolution of carbon dioxide occurs therefore release the... 

The crude acetonitrile contains as impurity chiefly acetic acid, arising from the action of phosphoric acid on the acetamide. Therefore add to the nitrile about half its volume of water, and then add powdered dry potassium carbonate until the well-shaken mixture is saturated. The potassium carbonate neutralises any acetic acid present, and at the same time salts out the otherwise water-soluble nitrile as a separate upper layer. Allow to stand for 20 minutes with further occasional shaking. Now decant the mixed liquids into a separating-funnel, run off the lower carbonate layer as completely as possible, and then pour off the acetonitrile into a 25 ml, distilling-flask into which about 3-4 g. of phosphorus pentoxide have been placed immediately before. Fit a thermometer and water-condenser to the flask and distil the acetonitrile slowly, collecting the fraction of b.p. 79-82°. Yield 9 5 g. (12 ml.). 

Place the distillate in a separating-funnel and extract the benzonitrile twice, using about 30 ml. of ether for each extraction. Return the united ethereal extracts to the funnel and shake with 10% sodium hydroxide solution to eliminate traces of phenol formed by decomposition of the benzenediazonium chloride. Then run off the lower aqueous layer, and shake the ethereal solution with about an equal volume of dilute sulphuric acid to remove traces of foul-smelling phenyl isocyanide (CaHjNC) which are always present. Finally separate the sulphuric acid as completely as possible, and shake the ether with water to ensure absence of acid. Run off the water and dry the benzonitrile solution over granular calcium chloride for about 20 minutes. 

Filter the dried extract, and then distil off the ether from a small flask, using the customary precautions if the volume of ether is large, fit a dropping-funnel to the flask so that the ethereal extract can be run into the flask as the ether distils off cf. Fig. 23(E), p. 45). When the ether has been removed, replace the water-condenser by an air-condenser, and continue... 

If no solid precipitate is obtained but the solution becomes cloudy, a low-melting or liquid phenol is indicated this will, of course, be revealed also by the characteristic phenolic odour. Transfer to a separating-funnel and extract with an equal volume of ether. Separate and dry with anhydrous sodium sulphate. Distil off the ether and identify the residue. 

Add a known volume ofo oaM.AgNOj solution (in excess) and boil the solution until the silver chloride has coagulated. Filter through a conical 5 cm. funnel, ensuring that the filter-paper does not protrude above the r m of the funnel. Wash the silver chloride and the filter-paper several times with a fine jet of distilled water. To the united filtrate and washings add i ml. of saturated ferric alum solution. The solution should be almost colourless if it is more than faintly coloured, add a few drops of concentrated nitric acid. Then titrate with 0 02M-ammonium thiocyanate solution until the permanent colour of ferric thiocyanate is just perceptible. (Alternatively the chloride may be determined potentiometrically.)... 

If crystallisation commences as soon as the solvent cools or if large quantities of hot solution are to be filtered, the funnel (and fluted filter paper) should be warmed externally during the filtration (hot water funnel). Three types of hot water funnel are illustrated in Fig. 11,1, 6 no flames should be present whilst inflammable solvents are being filtered through the funnel of Fig. 11, 1, 6, a. Alternatively, the funnel may be surrounded by an electric heating mantle (see Section 11,57) the heat input may be controlled by a variable transformer. When dealing with considerable volumes of aqueous or other solutions which do not deposit crystals rapidly on cooling, a Buchner funnel may be used for filtration (see detailed account in Section 11,1 and Fig. 11 1, 7, c). The filter paper... 

The set-up of Fig. 11, 41, 3 ensures the complete condensation of the steam when a rapid flow of steam is necessary for satisfactory results, and is useful in the distillation of large volumes of liquids of low vapour pressure, such as nitrobenzene. Thus the flask A containing the mixture may be of 3-litre capacity and B may be a 1-litre flask the latter is cooled by a stream of water, which is collected in a funnel and conducted to the sink. The receiver C must be of proportionate size all stoppers... 

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... 

About 150 ml. of concentrated sulphuric acid is placed in the larger funnel and 100 ml. of concentrated hydrochloric acid in the smaller separatory funnel. The latter is raised until the capillary tube is above the sulphuric acid, the capillary tube is filled with concentrated hydrochloric acid, and the stopper replaced. The rate of evolution of hydrogen chloride is controlled by regulation of the supply of hydro chloric acid this will continue until a volume of hydrochloric acid equal to that of the concentrated sulphuric acid has been used. The diluted sulphuric acid should then be removed and the apparatus recharged. The yield is 31-33 g. of hydrogen chloride per 100 ml. of concentrated hydro chloric acid. If more than an equal volume of hydrochloric acid is employed, the yield of gas decreases and continues to be formed for a tune after the stopcock has been closed. 

Mix 40 g. (51 ml.) of isopropyl alcohol with 460 g. (310 ml.) of constant boiling point hydrobromic acid in a 500 ml. distilling flask, attach a double surface (or long Liebig) condenser and distil slowly (1-2 drops per second) until about half of the liquid has passed over. Separate the lower alkyl bromide layer (70 g.), and redistil the aqueous layer when a further 7 g. of the crude bromide will be obtained (1). Shake the crude bromide in a separatory funnel successively with an equal volume of concentrated hydrochloric acid (2), water, 5 per cent, sodium bicarbonate solution, and water, and dry with anhydrous calcium chloride. Distil from a 100 ml. flask the isopropyl bromide passes over constantly at 59°. The yield is 66 g. 

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