Nitrate separation from

It may be prepared by mixing a solution of eobaltous nitrate with a mixture of ammonium carbonate and ammonia solution and allowing the liquid to stand for some time. Dark red crystals separate and are collected and recrystallised from hot water. In order to obtain the salt in a pure state it is transformed into the iodide by treating with hydr-iodie acid, the iodide precipitated from solution with alcohol, crystallised from water, and transformed into the nitrate by the addition of a concentrated solution of silver nitrate to an aqueous solution. The silver iodide is filtered oft and the nitrate separated from the filtrate by the addition of alcohol. The salt does not give the normal reactions for a carbonate and is unstable towards acids.2... 

Cross-flow filters behave in a way similar to that normally observed in crossflow filtration under ambient conditions increased shear-rates and reduced fluid-viscosity result in an increased filtrate number. Cross-microfiltration has been applied to the separation of precipitated salts as solids, giving particle-separation efficiencies typically exceeding 99.9%. Goemans et al. [30] studied sodium nitrate separation from supercritical water. Under the conditions of the study, sodium nitrate was present as the molten salt and was capable of crossing the filter. Separation efficiencies were obtained that varied with temperature, since the solubility decreases as the temperature increases, ranging between 40% and 85%, for 400 °C and 470°C, respectively. These workers explained the separation mechanism as a consequence of a distinct permeability of the filtering medium towards the supercritical solution, as opposed to the molten salt, based on their clearly distinct viscosities. 

Another reason for discussing the mechanism of nitration in these media separately from that in inert organic solvents is that, as indicated above, the nature of the electrophile is not established, and has been the subject of controversy. The cases for the involvement of acetyl nitrate, protonated acetyl nitrate, dinitrogen pentoxide and the nitronium ion have been advocated. 

Despite the fact that solutions of acetyl nitrate prepared from purified nitric acid contained no detectable nitrous acid, the sensitivity of the rates of nitration of very reactive compounds to nitrous acid demonstrated in this work is so great that concentrations of nitrous acid below the detectable level could produce considerable catalytic effects. However, because the concentration of nitrous acid in these solutions is unknown the possibility cannot absolutely be excluded that the special mechanism is nitration by a relatively unreactive electrophile. Whatever the nature of the supervenient reaction, it is clear that there is at least a dichotomy in the mechanism of nitration for very reactive compounds, and that, unless the contributions of the separate mechanisms can be distinguished, quantitative comparisons of reactivity are meaningless. 

Uranium Purification. Subsequent uranium cycles provide additional separation from residual plutonium and fission products, particularly zirconium— niobium and mthenium (30). This is accompHshed by repeating the extraction/stripping cycle. Decontamination factors greater than 10 at losses of less than 0.1 wt % are routinely attainable. However, mthenium can exist in several valence states simultaneously and can form several nitrosyl—nitrate complexes, some for which are extracted readily by TBP. Under certain conditions, the nitrates of zirconium and niobium form soluble compounds or hydrous coUoids that compHcate the Hquid—Hquid extraction. SiUca-gel adsorption or one of the similar Hquid—soHd techniques may also be used to further purify the product streams. 

Use of mercuric catalysts has created a serious pollution problem thereby limiting the manufacture of such acids. Other catalysts such as palladium or mthenium have been proposed (17). Nitration of anthraquinone has been studied intensively in an effort to obtain 1-nitroanthraquinone [82-34-8] suitable for the manufacture of 1-aminoanthraquinone [82-45-1]. However, the nitration proceeds so rapidly that a mixture of mono- and dinitroanthraquinone is produced. It has not been possible, economically, to separate from this mixture 1-nitroanthraquinone in a yield and purity suitable for the manufacture of 1-aminoanthraquinone. Chlorination of anthraquinone cannot be used to manufacture 1-chloroanthraquinone [82-44-0] since polychlorinated products are formed readily. Consequentiy, 1-chloroanthraquinone is manufactured by reaction of anthraquinone-l-sulfonic acid [82-49-5] with sodium chlorate and hydrochloric acid (18). 

Dioitroanthraquiaoae and 1,8-dinitroanthraquinone can also be prepared by nitration of anthraquiaone ia coaceatrated nitric acid (70). The 1,5-isomer can then be easily separated from the reaction mixture by filtration, since 1,8- or other isomers than 1,5-dinitroanthraquinone are completely dissolved in concentrated nitric acid. However, this process is unsuitable for industrial production for safety reasons the mixture of dinitroanthraquiaone and concentrated nitric acid forms a detonation mixture (71). Addition of sulfuric acid makes it possible to work outside the detonation area. 

The salt is dissolved in 800 cc. of water (Note 3) and transferred to a 5-I. round-bottom flask. To the solution is added with constant stirring a solution of 200 g. of lead nitrate (0.6 mole) in 400 cc. of water. Lead sulfide separates as a heavy brown precipitate which soon turns black. The mixture is then distilled with steam into a receiver containing 5-10 cc. of. i N sulfuric acid as long as any oil comes over (Note 4). About 2-3 1. of distillate is collected. The product is separated from the water and weighs 63-66 g. 

The term manufacture also includes coincidental production of a toxic chemical (e.g., as a byproduct or impurity) as a result of the manufacture, processing, use, or treatment of other chemical substances. In the case of coincidental production of an impurity (i.e., a chemical that remains in the product that is distributed in commerce), the de minimis limitation, discussed on page 11, applies. The de minimis limitation does not apply to byproducts (e.g., a chemical that is separated from a process stream and further processed or disposed). Certain listed toxic chemicals may be manufactured as a result of wastewater treatment or other treatment processes. For example, neutralization of acid wastewater can result in the coincidental manufacture of ammonium nitrate (solution). 

While the direct halogenation of toluene gives a mixture of isomers that is difficult to separate into the pure isomers, the isomeric o- and /r-nitrotoluenes 6a and 6b, formed by nitration, are easy to separate from each other. Thus reduction of the single o- or /j-nitrotoluene 6 to the o- or /j-toluidine 7a or 7b respectively, followed by conversion into the corresponding diazonium salt 8 and a subsequent Sandmeyer reaction leads to the pure o- or /j-halotoluene 9. 

It has been prepared synthetically by Ewins in the following manner Meta-oxybenzoic acid is converted with the aid of dimethyl sulphate into m-methoxybenzoic acid, which is then nitrated, and from the nitration products 2-nitro-3-methoxybenzoic acid is separated. This is reduced to 2-amino-3-methoxybenzoic acid which on heating with methyl iodide, yields 2-methylamino-3-methoxybenzoic acid. On warming this with freshly precipitated silver chloride it yields damascenine hydrochloride. 

Note in making up the chromic acid solution it is advisable to dissolve the silver nitrate separately and add it to the boiling chromic acid to prevent excessive crystallisation of the silver chromate. The chromic acid must be free from sulphate to avoid attack on the zinc. Immerse each specimen for 15 s in a 6% solution of hydriodic acid at room temperature to remove the remaining corrosion products. Immediately after immersion in the acid bath, wash the samples first in tap water and then in absolute methanol, and dry in air. This procedure removes a little of the zinc and a correction may be necessary. 

Prepare an approximately 0.1 M silver nitrate solution. Place 0.1169 g of dry sodium chloride in the beaker, add 100 mL of water, and stir until dissolved. Use a silver wire electrode (or a silver-plated platinum wire), and a silver-silver chloride or a saturated calomel reference electrode separated from the solution by a potassium nitrate-agar bridge (see below). Titrate the sodium chloride solution with the silver nitrate solution following the general procedure described in Experiment 1 it is important to have efficient stirring and to wait long enough after each addition of titrant for the e.m.f. to become steady. Continue the titration 5 mL beyond the end point. Determine the end point and thence the molarity of the silver nitrate solution. 

Na nitrate occurs native in large deposits in the rainless districts of Chile, hence it is often called Chile saltpeter or Chile niter . The Na nitrate in the deposits constitutes from 20 to 50% in a distinct stratum of earth known as caliche . The caliche is crushed and lixiviated in large tanks of w heated by steam. The settled soln is run off to crystallizers, where crude nitrate separates, the mother liquors being run back to the lixiviators. The crysts are washed with a little w and dried in the sun they contain 95—96% Na nitrate (Ref 1)... 

It is obvious that the nitrated product must be separated from the acid in equil with it (spent acid). If the product and the spent acid form two immiscible liq phases, eg, NG, EGDN, or molten TNT, separation is effected by gravity or centrifuging. If the product and spent acid form a solid and a liq phase, eg PA, NC or PETN, separation is effected by centrifuging (PA NC) or filtration (PETN). If the nitration is carried in the vapor phase (NM), separation is effected by distillation... 

Ridd et a/.48 have studied the nitration of aniline by nitricacid in 82.0-100.0 wt. % sulphuric acid, and the second-order rate coefficients were separated (from product analysis) into those appropriate for ortho, meta, and para substitution (Table 5). 

Many ionic compounds can have water molecules incorporated into their solid structures. Such compounds are called hydrates. To emphasize the presence of discrete water molecules in the chemical structure, the formula of any hydrate shows the waters of hydration separated from the rest of the chemical formula by a dot. A coefficient before H2 O indicates the number of water molecules in the formula. Copper(II) sulfate pentahydrate is a good example. The formula of this beautiful deep blue solid is C11SO4 5 H2 O, indicating that five water molecules are associated with each CuSOq unit. Upon prolonged heating, CuSOq 5 H2 O loses its waters of hydration along with its color. Other examples of hydrates include aluminum nitrate nonahydrate, A1 (N03)3 9 H2 O,... 

When a salt containing polyatomic ions dissolves In water, the cations separate from the anions, but each polyatomic ion remains intact. An example Is ammonium nitrate, composed of NH4 polyatomic cations and NO3 polyatomic anions. Ammonium nitrate dissolves In water to give a solution containing NH4 cations and NO3 anions, as Figure 3-21 Illustrates. 

Molecular view of an aqueous solution of ammonium nitrate. Ammonium ions separate from nitrate ions, but both these species remain intact as polyatomic clusters. 

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