Thermometer water

Fit the three-necked, round-bottomed flask with a thermometer, water-cooled condenser and close the remaining opening with a septum. Place a drying tube containing CaCI2 on top of the condenser. 

Apparatus A 25-mL round-bottom flask, Claisen adapter, thermometer, water-cooled condenser, ice-water bath, apparatus for magnetic stirring and flameless heating. 

Fahrenheit and Celsius are not absolute scales of measurement in the sense that they were chosen somewhat arbitrarily. Gabriel Fahrenheit (1686-1736) chose as 0° the coldest temperature he could get in his laboratory. When he marked off the degrees on his thermometer, water boiled at 212°. When Anders Celsius (1701-44) invented his temperature scale, he chose the freezing point of water to be 0° and water s boiling point to be 100°. 

Round-bottomed flasks (Fig. 22(A)) of various sizes and having necksof various lengths and widths. They can be closed with stoppers (Fig. 22(B)), or fitted with any of the following units reflux air-condensers (Fig. 22(C)) or water condensers (Fig. 22(D)) distillation heads, of the simple knee-tube type (Fig. 22(E)), or with a vertical joint (Fig. 22(F)) for thermometers, etc., or with... 

Now filter the ether through a fluted filter-paper directly into a 100 ml. distilling-flask, and then equip the latter with a 100° thermometer and a double-surface condenser to the end of the latter attach a receiver with a rubber delivery-tube precisely as before. Place the flask cautiously in a water-bath, the contents of which have previously been heated to about 60° at some distance from the apparatus arrange the depth of the flask in the water-bath so that the ether distils slowly over. Collect the fraction boiling between 34-39°. Yield, 25 g. (35 ml.). Not more than a verv small residue of etlianol should remain in the flask. 

Prepare a solution of 12 5 g. of hydroxylamine hydrochloride in 20 ml. of water contained in a too ml. conical flask. Dissolve 7 g. of powdered sodium hydroxide in 20 ml. of water, cool the solution in ice-water, and then add it to that of the hydroxylamine hydrochloride. Place a thermometer in the mixed solution, and chill the flask in ice-water until the temperature of the solution is between 5 and 10 . Now add 12 ml. (9 5 gO of dry acetone (preferably from a burette to ensure... 

After about 20 minutes, when the liquid should be dry, filter it through a small fluted filter-paper into a 100 ml. distilling-flask attached to a water-condenser. Add some fragments of unglazed porcelain to the ethyl acetate, fit a 100° thermometer to the flask, and place the latter on a cold water-bath, which is then brought to the boil. Some ether is always formed as a by-product with the ethyl acetate, and by these means is carefully distilled off as a... 

Use the apparatus shown in Fig. 38, p. 63, using a thermometer reading to 100° and with water running through the vertical condenser. Place in the 25 ml. pear-shaped flask 5 ml. of ethanol, 5 ml. of glacial acetic acid and add carefully with shying i ml. of concentrated sulphuric acid. Attach the flask to the reflux condenser and boil the mixture gently for 10 minutes. 

Fit the flask with a 100° thermometer and a water-condenser, and distil the ethyl iodide carefully from a water-bath, collecting the fraction which distils between 68° and 73°. Yield, about 24 g. 

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 in the flask 2 g. of benzophenone, 15 ml. of isopropanol and 2 5 g. of aluminium isopropoxide. This mixture has now to be heated gently under reflux so that the temperature registered by the thermometer in the column does not exceed 80°, i.e., so that only acetone distils. For this purpose, the flask should preferably be heated in an oil-bath direct heating, even over an asbestos sheet, may cause local overheating and decomposition the use of a water-bath on the other hand may make the column undesirably damp. 

Dissolve 15 ml. (15-4 g.) of aniline in a mixture of 40 ml. of concentrated hydrochloric acid and 40 ml. of water contained in a 250 ml. conical flask. Place a thermometer in the solution, immerse the flask in a mixture of ice and water, and cool until the temperature of the stirred solution reaches 5°. Dissolve I2 5 g. of powdered sodium nitrite in 30 ml. of water, and add this solution in small quantities (about 2-3 ml. at a time) to the cold aniline hydrochloride solution, meanwhile keeping the latter well stirred by means of a thermometer. Heat is evolved by the reaction, and therefore a short interval should be allowed between consecutive additions of the sodium nitrite, partly to allow the temperature to fall again to 5°, and partly to ensure that the nitrous acid formed reacts as completely as possible with the aniline. The temperature must not be allowed to rise above 10°, otherwise appreciable decomposition of the diazonium compound to phenol will occur on the other hand, the temperature... 

Then, while the diazonium solution is standing in ice-water, dissolve 55 g. of powdered copper sulphate (CuS04,5Ha0) in 200 ml. of water contained in a 1500 ml. flat-bottomed flask, for which a steam-distillation fitting is available for subsequent use. Place a thermometer in the copper sulphate solution and warm the latter to 60-65 . Now cautiously add a solution of 60 g. of powdered potassium cyanide in too ml. of water to the copper... 

Cyclohexanone oxime. Add 20 g. (21 ml.) of cyclohexanone to a solution of 17 g. of hydroxylamine hydrochloride in 40 ml. of water, and cool the mixture in ice-water. Add a solution of 13 g. of anhydrous sodium carbonate in 40 ml. of water slowly to the mixture, stirring the latter with a 100° thermometer, and maintaining the temperature of the mixture at 20-25° meanwhile. The oxime rapidly separates. Stir the complete mixture at intervals, and after 10 minutes filter the oxime at the pump, drain thoroughly and dry it in a (vacuum) desiccator. Yield of crude oxime, 20 g. Recrystallise from petroleum (b.p. 100-120 ) and dry over paraffin wax (p. 19). Yield of pure oxime, 16 g., m.p. 88°. 

Place 20 g. of dry powdered benzoic acid in C, add 15 ml. (25 g., i.e., a 30% excess) of thionyl chloride and some fragments of porcelain, and then clamp the apparatus on a boiling water-bath as shown so that no liquid can collect in the side-arm of C. Heat for one hour (with occasional gentle shaking), by which time the evolution of gas will be complete. Cool the flask C, detach the condenser and fit it to the side-arm for distillation, using a 360° thermometer for the neck of C. To the lower end of the condenser fit a small conical flask G (Fig. 67(B)) by a cork carrying also a calcium chloride tube. 

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