Melting water filter

The acetamide often contains a minute amount of impurity having an odour resembling mice excrement this can be removed by washing with a small volume of a 10 per cent, solution of ethyl alcohol in ether or by recrystallLsation. Dissolve 5 g. of impure acetamide in a mixture of 5 ml. of benzene and 1 5 ml. of dry ethyl acetate warm on a water bath until all is dissolved and cool rapidly in ice or cold water. Filter oflF the crystals, press between Alter paper and dry in a desiccator. The unpleasant odour is absent and the pure acetamide melts at 81°. Beautiful large crystals may be obtained by dissolving the acetamide (5 g.) in warm methyl alcohol (4 ml.), adding ether (40 ml.) and allowing to stand. 

Place 50 g. of ammonium thiocyanate in a small round-bottomed flask and immerse a thermometer in the substance. Heat in an oil bath until the temperature rises to 170° and maintain it at this temperature for 1 hour. Allow the melt to cool and extract it with 60-70 ml. of hot water. Filter the solution and allow to cool when crude thiourea separates the unchanged ammonium thiocyanate remains in the solution. Filter ofiF the crude product and recrystallise it from a little hot water. The yield of thiourea, m.p. 172°, is 8 g. 

Dissolve 10 g. of lactose (1) in 100 ml. of nitric acid, sp. gr. 115, in an evaporating dish and evaporate in a fume cupboard until the volume has been reduced to about 20 ml. The mixture becomes thick and pasty owing to the separation of mucic acid. When cold, dilute with 30 ml. of water, filter at the pump and set the filtrate A) aside. Wash the crude acid with cold water. Purify the mucic acid by dissolving it in the minimum volume of dilute sodium hydroxide solution and reprecipitating with dilute hydrochloric acid do not allow the temperature to rise above 25°. Dry the purified acid (about 5 g.) and determine the m.p. Mucic acid melts with decomposition at 212-213°. 

Cautiously add 250 g. (136 ml.) of concentrated sulphuric acid in a thin stream and with stirring to 400 ml. of water contained in a 1 litre bolt-head or three-necked flask, and then dissolve 150 g. of sodium nitrate in the diluted acid. Cool in a bath of ice or iced water. Melt 94 g. of phenol with 20 ml. of water, and add this from a separatory funnel to the stirred mixture in the flask at such a rate that the temperature does not rise above 20°. Continue the stirring for a further 2 hours after all the phenol has been added. Pour oflF the mother liquid from the resinous mixture of nitro compounds. Melt the residue with 500 ml. of water, shake and allow the contents of the flask to settle. Pour oflF the wash liquor and repeat the washing at least two or three times to ensure the complete removal of any residual acid. Steam distil the mixture (Fig. II, 40, 1 or Fig. II, 41, 1) until no more o-nitrophenol passes over if the latter tends to solidify in the condenser, turn oflF the cooling water temporarily. Collect the distillate in cold water, filter at the pump, and drain thoroughly. Dry upon filter paper in the air. The yield of o-nitrophenol, m.p. 46° (1), is 50 g. 

Benzyl-5-(2-hydroxyethyl)-4-inethyl-l,3-thia2ol1iim chloride. The product was isolated by pouring the ethanolic solution into well-stirred, ice-cold water, filtering, and recrystallizing from aqueous ethanol. The solutions should be ice-cold for the isolation of the low-melting acyloins. The products may also be Isolated by extraction as described for butyroin. 

Preparation of Silicic Acid Anhydride. Dissolve a small amount of potassium silicate in a minimum amount of water, filter the solution if necessary, and add a 37 % hydrochloric acid solution up to a strongly acidic reaction. Transfer the solution into a porcelain bowl and evaporate it until dry in a sand bath. Wash the dry residue with warm water until the chloride ions are removed, then roast it and see how it reacts with solutions of an alkali and hydrofluoric acid in a lead bowl in a jum cupboard ). Write the equations of the reactions. What is obtained when silicic acid anhydride is melted with alkalies ... 

Preparation of Potassium Chromate. (Perform one experiment on each table.) Melt a mixture of 1 g of potassium carbonate, 1 gof potassium hydroxide, and 2 g of potassium nitrate in an iron crucible by heating with the flame of a burner. While stirring the melt with an iron wire, introduce 1 g of finely comminuted chromite or -0.8 g of chromium oxide into the crucible. Roast the mixture for 5-10 minutes on a blowpipe. Treat the cooled melt with water. Filter the solution and evaporate it until a crystalline film appears. What is the composition of the formed crystals Why was potassium carbonate introduced into the reaction Write the equation of the reaction. 

Method I.—Intimately mix 36 g. of antimony sulfide (or powdered stibnite), Sb2S3 43 g. of anhydrous sodium sulfate and 16 g. of fine charcoal in a clay crucible, which should be about half filled with the mixture. Cover with a little charcoal and heat in the furnace to quiet fusion and then for 10 min. longer. Pour out on sheet iron or on a large iron pan. Powder the cold melt and boil it half an hour with 7 g. of sulfur and 300 cc. of water. Filter, add a little sodium hydroxide, and evaporate to crystallization in a porcelain dish. Because of hydrolysis, the crystals cannot be washed with water. Collect on glass wool or on a bare Witte plate and wash with alcohol containing a little sodium hydroxide. Obtain several crops of crystals. Finally,... 

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