Ammonia solutions products

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 ... 

Gyanoacetamide. Place 150 ml. of concentrated aqueous ammonia solution (sp. gr. 0-88) in a 500 ml. wide-mouthed conical flask and add 200 g. (188 ml.) of ethyl cyanoacetate. Shake the cloudy mixture some heat is evolved and it becomes clear in about 3 minutes. Stand the loosely stoppered flask in an ice-salt mixture for 1 hour, filter rapidly with suction, and ash the solid with two 25 ml. portions of ice-cold ethanol. Dry in the air the yield of pale yellow cyanoacetamide is 110 g. (1). Recrystallise from 190 ml. of 95 per cent, ethanol a colourless product, m.p. 119-120 , is deposited with practically no loss. 

Alternatively, grind 10 g. of p-toluenesulphonyl chloride to a fine powder and add it to 30 ml. of concentrated ammonia solution (sp. gr. 0-88). Heat the mixture to boiling (FUME CUPBOARD) and cool. Filter and recrystallise the p-toluenesulphonamide from boiling water (add 1 g. of decolourising carbon, if necessary). The yield of pme product, m.p. 138°, is almost theoretical. 

Nitrogen solutions consist of fertilizer product combinations, eg, ammonium nitrate —ammonia, urea—ammonium nitrate—ammonia, urea—ammonium nitrate, and urea—ammonia solutions. Mixed fertilizers cover a broad range and can be loosely defined as fertilizers which contain chemically mixed nitrogen, phosphoms, and potassium (N—P—K). Examples are ammonium phosphate—potash mixtures and ammonium phosphate nitrates. 

Manufacture. Historically, ammonium nitrate was manufactured by a double decomposition method using sodium nitrate and either ammonium sulfate or ammonium chloride. Modem commercial processes, however, rely almost exclusively on the neutralization of nitric acid (qv), produced from ammonia through catalyzed oxidation, with ammonia. Manufacturers commonly use onsite ammonia although some ammonium nitrate is made from purchased ammonia. SoHd product used as fertilizer has been the predominant form produced. However, sale of ammonium nitrate as a component in urea—ammonium nitrate Hquid fertilizer has grown to where about half the ammonium nitrate produced is actually marketed as a solution. 

Because dimethyl sulfate looks like water, operations are preferably not performed when water is present, eg, wet floors or rain. Any spills or leaks should not be left unattended they should be contained, and mnoff to sewers should be avoided. Minor spills should be flooded with water to dilute and hydroly2e the dimethyl sulfate. The area should then be covered with a dilute (2—5 wt %) caustic solution or a dilute (2—5 wt %) ammonia solution, or soda ash may be sprinkled over the neat liquid and the mix wetted with a gende spray of water. The neutrafi2ing agent should remain on the affected area for 24 h and then should be washed away. Only personnel wearing protective equipment should perform these operations. The product bulletins should be consulted for procedures to be followed for more severe spills. Concentrated ammonia should not be used with neat dimethyl sulfate because explosions have resulted after their contact (128). 

ThioglycoHc acid can be identified by its in spectmm or by gas chromatography. Most of the by-products and self-esterification products are also detected by liquid chromatography, eg, thiodiglycolic acid, dithiodiglycolic acid, linear dimers, and polymers. Iron content can be assayed by the red sensitive complex of 1,10-phenanthroline [66-71-7] and ferrous ion of a mineralised sample. Ferric ion turns an aqueous ammonia solution deep red-violet. 

The mauve colored cobalt(II) carbonate [7542-09-8] of commerce is a basic material of indeterminate stoichiometry, (CoCO ) ( (0 )2) H20, that contains 45—47% cobalt. It is prepared by adding a hot solution of cobalt salts to a hot sodium carbonate or sodium bicarbonate solution. Precipitation from cold solutions gives a light blue unstable product. Dissolution of cobalt metal in ammonium carbonate solution followed by thermal decomposition of the solution gives a relatively dense carbonate. Basic cobalt carbonate is virtually insoluble in water, but dissolves in acids and ammonia solutions. It is used in the preparation of pigments and as a starting material in the preparation of cobalt compounds. 

Cobalt(II) oxalate [814-89-1], C0C2O4, is a pink to white crystalline material that absorbs moisture to form the dihydrate. It precipitates as the tetrahydrate on reaction of cobalt salt solutions and oxaUc acid or alkaline oxalates. The material is insoluble in water, but dissolves in acid, ammonium salt solutions, and ammonia solution. It is used in the production of cobalt powders for metallurgy and catalysis, and is a stabilizer for hydrogen cyanide. 

Coppet(II) oxide [1317-38-0] CuO, is found in nature as the black triclinic tenorite [1317-92-6] or the cubic or tetrahedral paramelaconite [71276-37 ]. Commercially available copper(II) oxide is generally black and dense although a brown material of low bulk density can be prepared by decomposition of the carbonate or hydroxide at around 300°C, or by the hydrolysis of hot copper salt solutions with sodium hydroxide. The black product of commerce is most often prepared by evaporation of Cu(NH2)4C02 solutions (35) or by precipitation of copper(II) oxide from hot ammonia solutions by addition of sodium hydroxide. An extremely fine (10—20 nm) copper(II) oxide has been prepared for use as a precursor in superconductors (36). 

Particulate emissions from zinc processing are collected in baghouses or ESPs. SO2 in high concentrations is passed directly to an acid plant for production of sulfuric acid by the contact process. Low-concentration SO2 streams are scrubbed with an aqueous ammonia solution. The resulting ammonium sulfate is processed to the crystalline form and marketed as fertilizer. 

When sinomenine is heated with hydrochloric acid and the product treated with ammonia solution, Z)w-demethylsinomenylidene, (CjgH,jO,N), is formed,which crystallises from chloroform, has m.p. > 312°,... 

Metal-ammonia solutions reduce conjugated enones to saturated ketones and reductively cleave a-acetoxy ketones i.e. ketol acetates) to the unsubstituted ketones. In both cases the actual reduction product is the enolate salt of a saturated ketone this salt resists further reduction. If an alcohol is present in the reaction mixture, the enolate salt protonates and the resulting ketone is reduced further to a saturated alcohol. Linearly or cross-conjugated dienones are reduced to enones in the absence of a proton donor other than ammonia. The Birch reduction of unsaturated ketones to saturated alcohols was first reported by Wilds and Nelson using lithium as the reducing agent. This metal has been used almost exclusively by subsequent workers for the reduction of both unsaturated and saturated ketones. Calcium has been preferred for the reductive cleavage of ketol acetates. 

Eq. (4e)] is not reduced by metal-ammonia solutions so that the existence of this equilibrium cannot lead to further reduction of the saturated ketonic product only protonation on carbon can result in further reduction (see page 39). 

Reaction times of from 5 to 60 minutes have been employed for the reduction of conjugated enones. Although the longer times apparently do not seriously diminish the yields of products, they usually are not necessary. If a conjugated enone is sufficiently soluble in the reaction medium, it is reduced almost instantly when added to lithium-ammonia solutions. 

Then, as described in U.S. Patent 2,55416, the 2-acetylamido-5-mercapto-1,3,4-thiadiazole is converted to the sulfonyl chloride by passing chlorine gas into a cooled (5°-10°C) solution in 33% acetic acid (66 parts to 4 parts of mercapto compound) used as a reaction medium. Chlorine treatment is continued for two hours. The crude product can be dried and purified by recrystallization from ethylene chloride. The pure compound is a white crystalline solid, MP l94°C,with decomposition, when heated rapidly. The crude damp sulfonyl chloride is converted to the sulfonamide by addition to a large excess of liquid ammonia. The product is purified by recrystallization from water. The pure compound is a white, crystalline solid, MP 259°C, with decomposition. The yield of sulfonamide was 85% of theory based on mercapto compound. 

A solution of 438 mg of diac in methanol (20 ml) and ammonia solution (SG 0.88 20 ml) was iodinated at 0°C with 1.8 ml 1 N iodine solution. The product was isolated in almost theoretical yield in a manner similar to that described for tetrac. After crystallization from 50% (v/v) methanol, triac was obtained as colorless needles which melted over the range 65°C to 90°C according to the rate of heating. The molten form resolidified at about 110°C and finally melted at 180 C to 181°C without decomposition. The compound, dried at 25°C/3 mm over silica gel, contains methanol of crystallization. 

The point X] represents 0.092 mol NHs/mol H2O, which is equivalent to 8 wt% ammonia solution. If a weaker product were desired fewer transfer units would be required. 

The opposite process, i.e. pouring the strip solution into the ammonia solution, significantly reduces the fluorine concentration in the hydroxides formed. Bludssus et al. [495] developed a process comprising the introduction of tantalum- or niobium-containing acid solution to an ammonia solution until achieving pH = 9. It is reported that this method enables the production of tantalum or niobium hydroxides with fluoride contents as low as 0.5% wt. with... 

Application of an excessive amount of ammonia solution in the precipitation of tantalum and niobium hydroxides from strip solutions usually ensures good quality of the products. Nevertheless, the method has two general problems. First, hydroxides containing low levels of fluorine contamination... 

The subsequent steps in the production of tantalum and niobium are washing and thermal treatment of the precipitated hydroxides. For effective washing of precipitated hydroxides, Vaicenberg et al. [490] recommended the use of a 2% wt. ammonia solution that is added at a solid-liquid volumetric ratio of 1 15. It is reported that the above conditions ensure the preparation of dry hydroxides with fluorine contents of less than 2%. Sheka et al. [491] proposed precipitation with ammonia at pH = 8.7-9 (20-40°C) and the subsequent use of 0.5-10% NH4OH with a solid-liquid volumetric ratio of 1 5 for washing (re-pulping). This method enables to reduce the fluorine content in the dry hydroxides to 0.2% wt. 

Consider now a somewhat different type of complex ion formation, viz. the production of a complex ion with constituents other than the common ion present in the solution. This is exemplified by the solubility of silver chloride in ammonia solution. The reaction is ... 

Popova and colleagues47 carried out TLC of oxidation products of 4,4 -dinitrodiphenyl sulphide (the sulphoxide and sulphone) on silica gel + a fluorescent indicator, using hexane-acetone-benzene-methanol(60 36 10 l) as solvent mixture. Morris130 performed GLC and TLC of dimethyl sulphoxide. For the latter, he applied a 6% solution of the sample in methanol to silica gel and developed with methanol-ammonia solution(200 3), visualizing with 2% aqueous Co11 thiocyanate-methanol(2 1). HPLC separations of chiral mixtures of sulphoxides have been carried out. Thus Pirkle and coworkers131-132 reported separations of alkyl 2,4-dinitrophenyl sulphoxides and some others on a silica-gel (Porosil)-bonded chiral fluoroalcoholic stationary phase, with the structure ... 

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