Ammonia-Water at 10 and

Heavy Metals. — Dissolve 5 gm. of ammonium fluoride in 25 cc. of water, add to the solution a few drops of hydrochloric acid, and 10 cc. of hydrogen sulphide water. No change should appear. Now add ammonia water to alkalinity, and a few drops of ammonium sulphide solution at most a slight greenish coloration may develop, but a precipitate should not form. 

Alumina, Calcium, and Heavy Metals. — 5 gm. of sodium hydroxide should afford a clear and colorless solution with 20 cc. of water. Dilute the solution to 100 cc., and then add 30 cc. of acetic acid (sp. gr. 1.041) and 10 cc. of ammonia water. At most a slight turbidity should develop within five minutes, but no flocculent precipitate of aluminum hydroxide should form nor should an immediate change in appearance occur on the addition of ammonium oxalate and ammonium sulphide solution. 

The ODH of propane over titanium and vanadium containing zeolites and nonzeolitic catalysts revealed that Ti-silicalite was the most active. The addition of water caused an increase in selectivity, probably due to a competitive adsorption on the active sites. The reaction is proposed to occur on the outer surface of the Ti-silicalite crystallites on Lewis acid sites, and a sulfation of the catalyst, which increases the acidity of these sites, results in a further increase of the catalytic activity. The maximum conversion obtained was 17% with a propene selectivity of up to 74% [65]. Comparison of propane oxidation and ammoxidation over Co-zeolites shows an increase in conversion and propene selectivity during ammoxidation. For a conversion of 14%, 40% propene selectivity was obtained with ammonia, whereas, at 10% conversion the propene selectivity was only 12% with oxygen. The increase in activity and selectivity can be due to the formation of basic sites via ammonia adsorption [38]. 

Boil 5 ml. (5-1 g.) of benzonitrile and 75 ml. of 10% aqueous sodium hydroxide in a 200 ml. flask under a reflux water condenser until no more oily drops of unchanged nitrile run down from the condenser (usually about 40 minutes). Th detach the condenser and boil the solution in the open flask for a few minutes to remove free ammonia, Cool the liquid, and add concentrated hydrochloric acid cautiously until precipitation of benzoic acid is complete. Cool the mixture again thoroughly, filter off the benzoic acid at the pump, and wash well with cold water. Yield, 5 8 g. (almost theoretical). Confirm the identity of the benzoic acid by the tests given on p. 347. The benzoic acid obtained in this way should be pure and have m.p. 121 a portion may if desired be recrystallised from hot water. 

Heat a mixture of 15 g. of p-nitroacetanilide and 75 ml. of 70 per cent, sulphuric acid (1) under a reflux water condenser for 20-30 minutes or until a test sample remains clear upon dilution with 2-3 times its volume of water. The p-nitroaniline is now present in the hquid as the sulphate. Pour the clear hot solution into 500 ml. of cold water and precipitate the p-nitroanihne by adding excess of 10 per cent, sodium hydroxide solution or of concentrated ammonia solution. When cold (cool the mixture in ice water, if necessary), filter the yellow crystalline precipitate at the pump, wash it well with water, and drain thoroughly. Recrystallise it from a mixture of equal volumes of rectified (or methylated) spirit and water or from hot water. Filter, wash and dry. The yield of p-nitroanihne, m.p, 148°, is 11 g. 

The special reducing agent (a solution containing cupro-ammonia ions) is first prepared. Dissolve 63 g. of crystallised copper sulphate in 250 ml. of water in a 1-Utre heaker, add 100 ml. of concentrated ammonium hydroxide solution (sp. gr. 0-88), and cool the solution to 10°. Dissolve 17 8 g. of hydroxylammonium chloride or 21 g. of hydroxylammonium sulphate in 60 ml. of water, cool to 10°, and add 42 -5 ml. of QN sodium hydroxide solution if the resulting solution of tydroxylamine is not clear, filter it at the pump. Without delay add the hydroxylamine solution, with stirring, to the ammoniacal cupric sulphate solution. Reduction occurs at once, a gas is evolved, and the solution assumes a pale blue colour. Protect the reducing agent from the air if it is not used immediately. 

Dissolve 1 0 g. of the compound in 5 ml. of dry chloroform in a dry test-tuhe, cool to 0°, and add dropwise 5g. (2-8 ml.) of redistilled chloro-sulphonic acid. When the evolution of hydrogen chloride subsides, allow the reaction mixture to stand at room temperature for 20 minutes. Pour the contents of the test-tube cautiously on to 25 g. of crushed ice contained in a small beaker. Separate the chloroform layer and wash it with a httle cold water. Add the chloroform layer, with stirring, to 10 ml. of concentrated ammonia solution. After 10 minutes, evaporate the chloroform on a water bath, cool the residue and treat it with 5 ml. of 10 per cent, sodium hydroxide solution the sulphonamide dissolves as the sodium derivative, RO.CgH4.SO,NHNa. Filter the solution to remove any insoluble matter (sulphone, etc.), acidify the filtrate with dilute hydrochloric acid, and cool in ice water. Collect the sulphonamide and recrystallise it from dilute alcohol. 

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