Cooling A-glass

Example Heat + H2Ofe) —> HzO(1) (melting ice to cool a glass of tea)... 

You have just cooled a glass of tap water at 20°C by adding ice, at —10° C. The glass originally contains 400 mL of tap water, to which 100 g of ice is added. Assume that the glass is adiabatic. Calculate the change in entropy of the universe after thermal equUibrium has been obtained. For... 

If the apparatus has not been used for some time, i should be heated to about 140° to drive off any moisture. After cooling, a few crystals of the substance are placed on the glass slide G. A small cover glass,... 

If it is desired to observe the crystalline form of the osazone, draw up in a glass tube a few drops of the cold filtrate containing the fine crystals, and transfer to a microscope slide. Cover the drops with a slip and examine under the microscope unless the filtrate has been cooled very slowly and thus given moderately-sized crystals, the high power of the microscope will probably be required. Note the fine yellow needles aggregated in the form of sheaves. Compare with Fig. 63(A). 

Undergoes Cannizzaro s reaction, giving benzyl alcohol and benzoic acid (p. 229). Warm gently for several minutes, cool, add a few ml. of water and then cone. HCl, and cool again. Crystals of benzoic acid separate out on scratching the sides of the tube with a glass rod. 

Add dil. H2SO4 until the solution is acid to litmus. Cool, and scratch the sides of the vessel with a glass rod a white precipitate indicates an aromatic carboxylic acid or uric acid, or a solid phenol insoluble in water (e.g., i- or 2-naphthol). If a precipitate is obtained, filter off through a Buchner funnel, wash with water, recrystallise if necessary and identify. 

Cuprous bromide. The solid salt may be prepared by dissolving 150 g. of copper sulphate crystals and 87 5 g. of sodium bromide dihydrate in 500 ml. of warm water, and then adding 38 g. of powdered sodium sulphite over a period of 5-10 minutes to the stirred solution. If the blue colour is not completely discharged, a little more sodium sulphite should be added. The mixture is then cooled, the precipitate is collected in a Buchner funnel, washed twice with water containing a little dissolved sulphurous acid, pressed with a glass stopper to remove most of the liquid, and then dried in an evaporating dish or in an air oven at 100 120°. The yield is about 80 g. 

For alcohols of b.p. below 150°, mix 0- 5 g. of 3-nitrophthalic anhydride (Section VII,19) and 0-5 ml. (0-4 g.) of the dry alcohol in a test-tube fitted with a short condenser, and heat under reflux for 10 minutes after the mixture liquefies. For alcohols boiling above 150°, use the same quantities of reactants, add 5 ml. of dry toluene, heat under reflux until all the anhydride has dissolved and then for 20 minutes more remove the toluene under reduced pressure (suction with water pump). The reaction product usually solidifies upon cooling, particularly upon rubbing with a glass rod and standing. If it does not crystallise, extract it with dilute sodium bicarbonate solution, wash the extract with ether, and acidify. Recrystallise from hot water, or from 30 to 40 per cent, ethanol or from toluene. It may be noted that the m.p. of 3-nitrophthalic acid is 218°. 

Prepare a coil of copper wire by winding several turns around a glass tube. Heat the coil in the oxidising flame of a Bunsen burner for 1-2 minutes and plunge the spiral, whilst still red hot, into a test-tube containing a solution of 1 ml. of methyl alcohol and 5 ml. of water. Stopper the test-tube loosely, cool, remove the wire, and repeat the process two or three times. Observe the odour of the solution and use it (or formalin diluted with water) to carry out the following tests. 

The complete assembly for carrying out the catalytic decomposition of acids into ketones is shown in Fig. Ill, 72, 1. The main part of the apparatus consists of a device for dropping the acid at constant rate into a combustion tube containing the catalyst (manganous oxide deposited upon pumice) and heated electrically to about 350° the reaction products are condensed by a double surface condenser and coUected in a flask (which may be cooled in ice, if necessary) a glass bubbler at the end of the apparatus indicates the rate of decomposition (evolution of carbon dioxide). The furnace may be a commercial cylindrical furnace, about 70 cm. in length, but it is excellent practice, and certainly very much cheaper, to construct it from simple materials. 

Add 0 -5 ml. of phenyl isothiocyanate to the distillate and shake the mixture vigorously for 3-4 minutes. If no derivative separates, crystallisation may be induced by cooling the flask in ice and scratching the walls with a glass rod. Filter off the crude product, wash it with a little 50 per nent. ethanol, and recrystaUise from hot dilute alcohol. (See Table 111,123 for melting points of phenylthiourea derivatives of amines.)... 

Prepare the acetaldehyde solution by plunging a red hot oxidised copper coil (made by winding a copper wire round a glass tube and heating the resulting coil in a Bunsen dame) into 6 ml. of 60 per cent, alcohol in a Pyrex test-tube. Withdraw the coil, cool the test-tube under the tap, repeat the oxidation several times, and use the cooled solution for the test. 

Dissolve equivalent quantities of the reagent and of the amine in a small amount of rectified spirit. K no reaction appears to take place in the cold, reflux the mixture for 5-15 minutes. Upon cooling (and scratching with a glass rod, if necessary) the crystaUiiie thiourea separates. RecrystaUise it from rectified spirit or from 60-b0 per cent, alcohol. 

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