Solution ammonia

BP Ammonia solution, concentrated PhEur Ammoniae solution concentrata USPNF Strong ammonia solution 

Ammoniaca ammoniacum aqua ammonia concentrated ammonia solution spirit of hartshorn stronger ammonia water. 

On exposure to the air, ammonia solution rapidly loses ammonia. Ammonia solution should be stored in a well-closed container, protected from the air, in a cool, dry place. The storage temperature should not exceed 20°C. 

Ammonia solution is typically not used undiluted in pharmaceutical applications. Generally, it is used as a buffering agent or to adjust the pH of solutions. Most commonly, ammonia solution (the concentrated form) is used to produce more dilute ammonia solutions. 

Therapeutically, dilute ammonia solution is used as a reflex stimulant in smelling salts , as a rubefacient, and as a counterirritant to neutralize insect bites or stings.  

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C. A typical aromatic amine. Best prepared by the prolonged action of concentrated ammonia solution at a high temperature upon anthraquinone-l-sulphonic acid in the presence of BaClj and by reduction of the corresponding nitro compound or by amination of the chloroanthraquinone. 

Prepared by stirring phthalimide with cold concentrated ammonia solution. Hydrolysed to phlhalic acid with dilute acids. Dehydration with ethanoic anhydride gives first n-cyano-benzamide and then phthalonitrile. 

Schweizer s reagent The dark blue solution obtained by dissolving Cu(OH)2 in concentrated ammonia solution. Used as a solvent for cellulose, the cellulose is precipitated on acidification. Used in the cuprammonium process for the manufacture of rayon. 

Silver f) oxide, Ag20, is obtained as a brown amorphous precipitate by the action of alkali on AgN03 solution. It cannot be obtained pure and is soluble in ammonia solution. 

For this second reaction Kjgs = 181 x 10" and hence pK, for ammonia solution is 4.75. The entity NHj. H2O is often referred to as ammonium hydroxide, NH4OH, a formula which would imply that either nitrogen has a covalency of five, an impossible arrangement, or that NH4OH existed as the ions NH4 and OH". It is possible to crystallise two hydrates from concentrated ammonia solution but neither of these hydrates is ionic. Hence use of the term ammonium hydroxide is to be discouraged in favour of ammonia solution . 

Because of ammine formation, when ammonia solution is added slowly to a metal ion in solution, the hydroxide may first be precipitated and then redissolve when excess ammonia solution is added this is due to the formation of a complex ammine ion, for example with copper(II) and nickel(II) salts in aqueous solution. 

Addition of silver nitrate to a solution of a chloride in dilute nitric acid gives a white precipitate of silver chloride, AgCl, soluble in ammonia solution. This test may be used for gravimetric or volumetric estimation of chloride the silver chloride can be filtered off, dried and weighed, or the chloride titrated with standard silver nitrate using potassium chromate(VI) or fluorescein as indicator. 

Silver nitrate soJuiion No ppt. White ppt., soluble in dil. ammonia solution Cream ppt., soluble in cone, ammonia solution Yellow ppt.. almost insoluble in cone, ammonia solution... 

When cobalt(II) chloride was dissolved in water, a pink solution A was formed. The addition of concentrated hydrochloric acid to A gave a blue solution B. If solution A was treated with concentrated ammonia solution a blue-green precipitate was formed upon addition of further ammonia solution followed by the passage of air through the mixture, an orange-red solution C was produced. 

Method (1) is most frequently used for aliphatic acid amides, while Methods (2a), (2b) and (zc) are used most frequently for aromatic acid amides. Of the last three methods, the Acid Chloride Method (zb) is the most rapid and certain. The Ester Method (za) is practicable only when the amide is insoluble in water, and even then is often very slow unless the ester itself is appreciabb soluble in the aqueous ammonia solution. 

Oxamide differs from most aliphatic acid amides in being almost insoluble in water, and therefore can be readily prepared from the diethyl ester by Method 2(a). Place a mixture of 5 ml. of concentrated [d o-88o) ammonia solution and 5 ml. of water in a 25 ml. conical flask, for which a welTfitting cork is available. (The large excess of... 

Succinamide. NHoCOCH2 CH2CONH2. (Method 2(a)). Add 5 ml. (5 8 g.) of dimethyl succinate to a mixture of 50 ml. of water and 25 ml. of concentrated [dy o-88o) aqueous ammonia solution in a 150 ml. conical flask. Cork the flask and shake the contents the dimethyl succinate rapidly dissolves to give a clear solution. Allow the solution to stand after about i hour the succinamide starts to crystallise, and then continues to separate for some time. Next day, filter off the succinamide at the pump, wash with cold water, and drain. Recrystallise from water, from which the succinamide separates as colourless crystals the latter soften at 240° and melt at 254 -255° with... 

Add 15 g, of chloroacetic acid to 300 ml. of aqueous ammonia solution d, o-88o) contained in a 750 ml. conical flask. (The manipulation of the concentrated ammonia should preferably be carried out in a fume-cupboard, and great care taken to avoid ammonia fumes.) Cork the flask loosely and set aside overnight at room temperature. Now concentrate the solution to about 30 ml. by distillation under reduced pressure. For this purpose, place the solution in a suitable distilling-flask with some fragments of unglazed porcelain, fit a capillary tube to the neck of the flask, and connect the flask through a water-condenser and receiver to a water-pump then heat the flask carefully on a water-bath. Make the concentrated solution up to 40 ml. by the addition of water, filter, and then add 250 ml. of methanol. Cool the solution in ice-water, stir well, and set aside for ca. I hour, when the precipitation of the glycine will be complete. 

B) Preparation of the Cuprous Solution, Add 85 ml. of concentrated ammonia solution (d, o-o88) to a solution of 50 g. of crystalline copper sulphate in 200 ml. of water, and cool to 10 . Dissolve 14 5 g. of hydroxylamine hydrochloride (or 17-4 g. of the sulphate) in 50 ml. of water, cool to 10 , and add a solution of 9 g. of sodium hydroxide in 30 ml. of water. Without delay add this hydroxylamine solution with stirring to the copper solution, which will be immediately reduced, but will retain a blue colour. 

Experiments involving the use of dimethyl sulphate should be carried out by students only under immediate supervision. Not only is the vapour of dimethyl sulphate highly poisonousy but the cold liquid itself is absorbed easily through the skin, with toxic results individual susceptibility to ditnethyl sulphate poisoning varies and may be very high. If the sulphate is splashed on to the hands, wash immediately with plenty of concentrated ammonia solution in order to hydrolyse the methyl sulphate before it can be absorbed through the skin (see p. 528). 

Place 5 ml. of benzaldehyde in a wide-necked stout-walled bottle of about 100 ml. capacity (a conical flask is too fragile for this purpose) and add 50 ml. of concentrated dy 0 880) ammonia solution. Cork the bottle securely, shake vigorously, and then allow to stand for 24 hours, by which time the layer of benzaldehyde at the bottom of the bottle will have been converted into a hard mass of hydrobenzamide. (If after 24 hours the crude hydrobenzamide is still syrupy, shake the mixture vigorously and allow to stand for another hour, when the conversion will be complete.) Break up the solid pellet with a strong spatula, filter at the pump, wash with water and drain thoroughly. Recrystallise from ethanol methylated spirit should not be used, as it contains sufficient water to cause partial hydrolysis back to benzaldehyde and ammonia. Hydrobenzamide is obtained as colourless crystals, m.p. 101° (and not 110° as frequently quoted) yield, 4 g. 

To determine which halogen is present, take 1-2 ml. of the filtrate from the sodium fusion, and add dilute sulphuric acid until just acid to litmus. Add about 1 ml. of benzene and then about 1 ml. of chlorine water and shake. A yellowish-brown colour in the benzene indicates bromine, and a violet colour iodine. If neither colour appears, the halogen is chlorine. The result may be confirmed by testing the solubility of the silver halide (free from cyanide) in dilute ammonia solution silver chloride is readily soluble, whereas the bromide dissolves with difficulty, and the iodide not at all. 

Colorations or coloured precipitates are frequently given by the reaction of ferric chloride solution with.(i) solutions of neutral salts of acids, (ii) phenols and many of their derivatives, (iii) a few amines. If a free acid is under investigation it must first be neutralised as follows Place about 01 g. of the acid in a boiling-tube and add a slight excess of ammonia solution, i,e., until the solution is just alkaline to litmus-paper. Add a piece of unglazed porcelain and boil until the odour of ammonia is completely removed, and then cool. To the solution so obtained add a few drops of the "neutralised ferric chloride solution. Perform this test with the following acids and note the result ... 

Reduction of ammoniacal silver nitrate. Place about 5 ml. of AgNOj solution in a thoroughly clean test-tube, and add 2-3 drops of dil. NaOH solution. Add dil. ammonia solution, drop by drop, until the precipitated silver oxide is almost redissolved, then add 2 - 3 drops of formaldehyde or acetaldehyde. A silver mirror is formed. 

Place about 0 5 g. of the acid in a boiling-tube and add a slight excess of ammonia solution until just alkaline to litmus-paper. Add a piece of unglazed porcelain and boil until the odour of ammonia is completely removed. (See also p. 332.) To the cold neutral solution add a few drops of neutral FeCl, solution. 

Since the silver salts of the carboxylic acids are usually soluble in dilute nitric acid, they must be prepared by treating an aqueous solution of a neutral salt of the acid (and not the free acid itself) with silver nitrate solution. It is not practicable to attempt to neutralise the acid with sodium or potassium hydroxide solution, because the least excess of alkali would subsequently cause the white silver salt to be contaminated with brown silver oxide. The general method used therefore to obtain a neutral solution j to dissolve the acid in a small excess of ammonia solution, and then to boil the solution until all free... 

Ammonia. Small quantities of ammonia may be prepared with the aid of the apparatus depicted in Fig. II, 48,4. Concentrated ammonia solution (sp. gr. 0-88) is gently heated in the flask surmounted by an efficient reflux condenser. The gas is dried by passage through the tower which is loosely packed with soda lime or quicklime, and is then passed... 

Add dilute ammonia solution dropwise to 1 ml. of 0- N silver nitrate solution until the precipitate which forms just redissolves, and then dilute with 3 ml. of water. 

Dissolve 3 g. of copper sulphate pentahydrate and 1 g. of sodium chloride in 12 ml. of hot water, and add a solution of 1 g. of sodium bisulphite in 10 ml. of 5 per cent, sodium hydroxide solution. Shake, cool under the tap, and wash the precipitated wlute cuprous chloride with water by decantation. Dissolve the cuprous chloride in a few ml. of concentrated ammonia solution and dilute with water to 10 ml. 

Upon heating the polymers, anhydrous gaseous formaldehyde is produced (compare Section 111,17). By allowing a mixture of concentrated ammonia solution and formalin to evaporate, hexamethylenetetramine (also called hexamine, vrotropine) CjHjjNj is formed ... 

Mix 50 ml. of formalin, containing about 37 per cent, of formaldehyde, with 40 ml. of concentrated ammonia solution (sp. gr. 0- 88) in a 200 ml. round-bottomed flask. Insert a two-holed cork or rubber stopper carrying a capillary tube drawn out at the lower end (as for vacuum distillation) and reaching almost to the bottom of the flask, and also a short outlet tube connected through a filter flask to a water pump. Evaporate the contents of the flask as far as possible on a water bath under reduced pressure. Add a further 40 ml. of concentrated ammonia solution and repeat the evaporation. Attach a reflux condenser to the flask, add sufficient absolute ethyl alcohol (about 100 ml.) in small portions to dissolve most of the residue, heat under reflux for a few minutes and filter the hot alcoholic extract, preferably through a hot water fuimel (all flames in the vicinity must be extinguished). When cold, filter the hexamine, wash it with a little absolute alcohol, and dry in the air. The yield is 10 g. Treat the filtrate with an equal volume of dry ether and cool in ice. A fiulher 2 g. of hexamine is obtained. 

Do not heat the silver solution or allow it to stand even for a few hours, since explosive silver fulminate may be formed. The ammoniacal solution of silver nitrate is prepared by treating 3 ml. of 0-lN silver nitrate solution with very dilute ammonia solution dropwise until the precipitate which is first formed just redissolves. 

It is preferable to use Tollen s ammoniacal silver nitrate reagent, which is prepared as follows Dissolve 3 g. of silver nitrate in 30 ml. of water (solution A) and 3 g. of sodium hydroxide in 30 ml. of water (solution B). When the reagent is requir, mix equal volumes (say, 1 ml.) of solutions A and JB in a clean test-tube, and add dilute ammonia solution drop by drop until the silver oxide is just dissolved. Great care must be taken in the preparation and use of this reagent, which must not be heated. Only a small volume should be prepared just before use, any residue washed down the sink with a large quantity of water, and the test-tubes rinsed with dilute nitric acid. 

The by-products are both gaseous and the excess of thiouyl chloride (b.p. 78°) may be readily removed by distillation. Interaction of the acid chloride with ammonia solution, aniline or p-toluidiiie yields the amide, anilide or p-toluidide respectively ... 

Amides. TVeat the acid chloride cautiously with about 20 parts of concentrated ammonia solution (sp. gr. 0 - 88) and warm for a few moments. If no solid separates on cooling, evaporate to dryness on a water bath. Recrystallise the crude amide from water or dilute alcohol. 

Preparation of silver maleate. Dissolve 65 g. of pure maleic acid (Section 111,143) in the calculated quantity of carefully standardised 3-5N aqueous ammonia solution in a 1-htre beaker and add, whilst stirring mechanically, a solution of 204 g. of silver nitrate in 200 ml. of water. Filter oflf the precipitated silver maleate at the pump, wash it with distilled water, and press well with the back of a large flat glass stopper. Dry in an electric oven at 50-60° to constant weight. The yield of the dry silver salt is 150 g. Store in a vacuum desiccator in the dark. 

Of the common esters, methyl oxalate (solid, m.p. 54°) and ethyl oxalate (liquid) give amides almost immediately upon shaking with concentrated ammonia solution. The resulting oxamide, m.p. 417°, is valueless as a derivative. The esters may, however, be easily hydrolysed and identified as above. 

By the action of concentrate aqueous ammonia solution upon esters. This process is spoken of as ammonolysls of the ester, by analogy with hydrolysis applied to a similar reaction with water. If the amide is soluble in water, e.g., acetamide, it may be isolated by distillation, for example ... 

Succinamide. Add 5 g. (4-8 ml.) of dimethyl succinate to 25 ml. of concentrated ammonia solution (sp. gr. 0-88) in a 100 ml. conical flask. Cork the flask and shake the contents for a few minutes aUow to stand for 24 hours with occasional shaking. Filter off the crystals of succinamide, and wash with a Uttle cold water. RecrystaUise from a little hot water. Dry in the steam oven and determine the m.p. The yield is 3-5 g. Pure succinamide melts at 254° with decomposition. 

Place 125 ml. of concentrated ammonia solution (sp. gr. 0-88) in a 600 ml. beaker and surround the latter with crushed ice. Stir the ammonia solution mechanically, and introduce the n-caproyl chloride slowly by means of a suitably supported separatory funnel with bent stem. The rate of addition must be adjusted so that no white fumes are lost. The amide separates immediately. Allow to stand in the ice water for 15 minutes after all the acid chloride has been introduced. Filter oflF the amide at the pump use the flltrate to assist the transfer of any amide remaining in the beaker to the Alter (2). Spread the amide on sheets of Alter or drying paper to dry in the air. The crude n-capro-amide (30 g.) has m.p. 98-99° and is sufficiently pure for conversion into the nitrile (Section 111,112) (3). Recrystallise a small quantity of the amide by dissolving it in the minimum volume of hot water and allowing the solution to cool dry on filter paper in the air. Pure n-caproamide has m.p. 100°. 

To 5 ml. of water add 1-2 drops of the secondary amine if it does not dissolve, add a drop or two of concentrated hydrochloric acid. Place 1 ml. of the reagent in a test-tube, add 0 -5-1 ml. of concentrated ammonia solution, followed by 0-5-1 ml. of the above amine solution, A precipitate indicates a secondary amine. A shght turbidity points to the presence of a secondary amine as an impurity. 

Amino acids may be prepared by the action of a large excess of concentrated ammonia solution upon a-chloro- or a-bromo-acids the presence of a considerable amount of ammonium carbonate often increases the yield of monoamino acid, for example ... 

Two compounds, which may be prepared from ethyl cyanoacetate and also find application in synthetical work, may be included here. Cyanoacetamide, prepar from ethyl cyanoacetate and concentrated ammonia solution ... 

Dissolve 180 g. of commercial ammonium carbonate in 150 ml. of warm water (40-50°) in a 700 ml. flask. Cool to room temperature and add 200 ml. of concentrated ammonia solution (sp. gr. 0 88). Introduce slowly, with swirling of the contents of the flask, a solution of 50 g. of chloroacetic acid (Section 111,125) in 50 ml. of water [CAUTION do not allow chloroacetic acid to come into contact with the skin as unpleasant burns will result]. Close the flask with a solid rubber stopper and fix a thin copper wire to hold the stopper in place do not moisten the portion of the stopper in contact with the glass as this lubrication will cause the stopper to slide out of the flask. Allow the flask to stand for 24-48 hours at room temperature. Transfer the mixture to a distilling flask and distil in a closed apparatus until the volume is reduced to 100-110 ml. A convenient arrangement is to insert a drawn-out capillary tube into the flask, attach a Liebig s condenser, the lower end of which fits into a filter flask (compare Fig.//, 1) and connect the... 

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