Water ammonia mixtures with

TABLE 4. Measured and Correlated pH of Water-Ammonia Mixtures with no Acid Gas Present, 25°C... 

TABLE 15. Measured and Correlated Ammonia Mixtures with 0. Mole of NH3> 80°C pH of Water-258 Mole of H2S/ ... 

In order to improve the performance of the absorption chiller, a counter-current heat recovery exchanger is used (see T-Q diagram presented in Fig. 5.89 for details), where the rich solution pumped to the boihng pot is warmed up by the lean solution flowing to the absorber. When the water/ammonia mixture exchanges heat with the water it generates very non-linear T-Q charts with the heat transfer equipment. In contrast, T-Q has linear characteristics when the heat exchanger works with the mixture at both sides. 

Dissolve 5 g. of finely-powdered diazoaminobenzene (Section IV,81) in 12-15 g. of aniline in a small flask and add 2-5 g. of finely-powdered aniline hydrochloride (1). Warm the mixture, with frequent shaking, on a water bath at 40-45° for 1 hour. Allow the reaction mixture to stand for 30 minutes. Then add 15 ml. of glacial acetic acid diluted with an equal volume of water stir or shake the mixture in order to remove the excess of anihne in the form of its soluble acetate. Allow the mixture to stand, with frequent shaking, for 15 minutes filter the amino-azobenzene at the pump, wash with a little water, and dry upon filter paper Recrystallise the crude p-amino-azobenzene (3-5 g. m.p. 120°) from 15-20 ml. of carbon tetrachloride to obtain the pure compound, m.p. 125°. Alternatively, the compound may be recrystaUised from dilute alcohol, to which a few drops of concentrated ammonia solution have been added. 

Figure 3 illustrates the shift and methanation conversion. The resulting methane is inert and the water is condensed. Thus purified, the hydrogen-nitrogen mixture with the ratio of 3H2 pressed to the pressure selected for ammonia synthesis. 

The general reaction procedure and apparatus used are exactly as described in Procedure 2. Ammonia (465 ml) is distilled into a 2-liter reaction flask and to this is added 165mlofisopropylalcoholandasolutionof30g(0.195 mole) of 17/ -estradiol 3-methyl ether (mp 118.5-120°) in 180 ml of tetrahydrofuran. The steroid is only partially soluble in the mixture. A 5 g portion of sodium (26 g, 1.13 g-atoms total) is added to the stirred mixture and the solid dissolves in the light blue solution within several min. As additional metal is added, the mixture becomes dark blue and a solid (matted needles) separates. Stirring is inefficient for a few minutes until the mass of crystals breaks down. All of the sodium is consumed after 1 hr and 120 ml of methanol is then added to the mixture with care. The product is isolated as in Procedure 4h 2. After being air-dried, the solid weighs 32.5 g (ca. 100% for a monohydrate). A sample of the material is dried for analysis and analyzed as described in Procedure 2 enol ether, 91% unreduced aromatics, 0.3%. The crude product may be crystallized from acetone-water or preferably from hexane. 

The requisite intermediate. 10-(3-chloropropyl)-2-acety(phenothiazine is prepared as follows To a suspension of sodamide (from 3 grams of sodium) in 300 ml of liquid ammonia is added 30 grams of 2-acetylphenothiazine. After stirring for one hour, there is added 19 grams of 1-bromo-3-chloropropane. The ammonia is allowed to evaporate and the residue is diluted with 200 ml of water. The mixture is extracted with ether and the ether solution is dried over anhydrous sodium sulfate, filtered and concentrated. 

One gram of 6,7-dihydro-5H-dibenz[c,e] azepine hydrochloride was dissolved in water, made alkaline with concentrated ammonia, and the resultant base extracted twice with benzene. The benzene layers were combined, dried with anhydrous potassium carbonate, and mixed with 0.261 g of allyl bromide at 25°-30°C. The reaction solution became turbid within a few minutes and showed a considerable crystalline deposit after standing 3 A days. The mixture was warmed VA hours on the steam bath in a loosely-stoppered flask, then cooled and filtered. The filtrate was washed twice with water and the benzene layer evaporated at diminished pressure. The liquid residue was dissolved in alcohol, shaken with charcoal and filtered. Addition to the filtrate of 0.3 gram of 85% phosphoric acid in alcohol gave a clear solution which, when seeded and rubbed, yielded 6-allyl-6,7-dihydro-5H-dlbenz[c,e] azepine phosphate, MP about 211°-215°C with decomposition. 

In about 250 cc of liquid ammonia (cooled with dry ice and acetone) are dissolved about 7.5 g of potassium and into the solution acetylene is passed until the blue color has disappeared (about 3 hours). Then slowly a solution or suspension of 3 g of estrone in 150 cc of benzene and 50 cc of ether is added. The freezing mixture is removed, the whole allowed to stand for about 2 hours and the solution further stirred overnight. Thereupon the reaction solution is treated with ice and water, acidified with sulfuric acid to an acid reaction to Congo red and the solution extracted five times with ether. The combined ether extracts are washed twice with water, once with 5% sodium carbonate solution and again with water until the washing water is neutral. Then the ether is evaporated, the residue dissolved in a little methanol and diluted with water. The separated product is recrystallized from aqueous methanol. The yield amounts to 2.77 g. The 17-ethiny I-estradiol-3,17 thus obtained melts at 142°C to 144°C . 

Preparation of J-Methy/ Lumilysergic Acid 8-Methyl Ester-10-Methyt Ether into a suspension of 10 grams of 1-methyi-iumiiysergic acid in 600 cc of absoiute methanoi a stream of anhydrous hydrogen chloride is bubbied for 1.5 hours with strong cooiing. The stream of hydrogen chloride is stopped and the mixture is aiiowed to stand for 30 minutes at 0°C, and is evaporated in vacuo to dryness. The residue is taken up with ice-cooied water made aikaiine with concentrated ammonia and extracted with chioroform. The combined chioro-form extracts are washed first with a 5% aqueous solution of sodium bicarbonate, then with water, and are thereafter dried over anhydrous sodium sulfate and finally evaporated in vacuo to dryness. 

Thebaine is dissolved in aqueous formic acid and treated with 30% HjO neutralization with aqueous ammonia gives 14-hydroxycodeinone. It is hydrogenated to give oxycodone. 90 ml of concentrated hydrobromic acid are heated to 90°C. 9 grams of 14-hydroxydi-hydrocodeinone (oxycodone) are then added under stirring and the mixture is quickly heated to 116°C and kept at this temperature under reflux condenser for 20 minutes, with continued stirring. The resulting brown solution Is diluted with about 90 ml of water and chilled with ice. Aqueous 10% sodium hydroxide solution is now added to alkaline reaction and the liquid is extracted 3 times with 100 cc portions of chloroform. The layers are separated and the aqueous phase is fiitered and acidified by the addition of concentrated aqueous hydrochloric acid, treated with charcoal and filtered. 

From Figure 9-73 the experimental Hqg be picked based on ammonia from a mixture with air absorbing in water. Assume an 18 O.D. tower (pipe) which has an I.D. of 16.8 in. 

Procedure. Dissolve a weighed amount of ferro-manganese (about 0.40 g) in concentrated nitric acid and then add concentrated hydrochloric acid (or use a mixture of the two concentrated acids) prolonged boiling may be necessary. Evaporate to a small volume on a water bath. Dilute with water and filter directly into a 100 mL graduated flask, wash with distilled water and finally dilute to the mark. Pipette 25.0 mL of the solution into a 500 mL conical flask, add 5 mL of 10 per cent aqueous hydroxylammonium chloride solution, 10 mL of 20 per cent aqueous triethanolamine solution, 10-35 mL of concentrated ammonia solution, about 100 mL of water, and 6 drops of thymolphthalexone indicator solution. Titrate with standard 0.05M EDTA until the colour changes from blue to colourless (or a very pale pink). 

A solution of 2.25 g (25 mmol) of D-glyccraldehyde in 300 mL of water is combined with a solution of 20 mmol of dihydroxyacetonc phosphate (DIIAP) in 200 mL of water freshly adjusted to pH 6.8. The mixture is incubated with 100 U of L-rhamnulose 1-phosphate aldolase at r.t. for 24 h with monitoring of conversion by TLC (2-propanol/sat. ammonia/water 6 4 2) and by enzymatic assay for DHAP55. 

Ammonia is absorbed in water from a mixture with air using a column operating at I bar and 295 K. The resistance to transfer may be regarded as lying entirely within the gas phase. At a point in the column, the partial pressure of the ammonia is 7.0 kN/m2. The back pressure at the water interface is negligible and the resistance to transfer may be regarded as lying in a stationary gas film 1 mm thick. If the diffusivity of ammonia in air is 2.36 x 10 5 m2/s, what is the transfer rate per unit area at that point in the column How would the rate of transfer be affected if the ammonia air mixture were compressed to double the pressure ... 

The situation does not improve with mixtures with the hydrides of the elements. Thus, a detonation occurred during contact between water and chlorine due to an accidental spark. Phosphine, silane and diborane all combust spontaneously in chlorine (their behaviour is the same in oxygen). With hydrogenated nitrogenous compounds ammonia, hydrazine, hydroxylamine, ammonium salts (especially ammonium chloride), and also sulphamic acid (these last two in an acid medium) there is ignition or even detonation. 

When it is mixed with small quantities of sulphuric acid and in the presence of water traces, it is thought to form permanganic acid, HMn04, which is very unstable and a violent oxidant. Thus, this system incandesces in the presence of ammonia. Mixtures of potassium permanganate /peroxomonosulphuric acid have also been used to measure sulphur in the presence of carbon. However, this is not recommended since it is highly likely to detonate. 

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