Potassium precipitation methods

A disadvantage of the conventional precipitation method in which the supersaturation was allowed to decrease during the reactions, was that different calcium phosphate phases could form and subsequently dissolve during the course of the reactions. In the present work, the constant composition method was used to investigate the influence of sodium chloride, potassium chloride, and potassium nitrate, as background electrolyte upon the rate of crystallization of HAP in solutions supersaturated only with respect to this phase. These experiments were made in solutions containing totaj... 

Bychkova and Shvarev [16] recently prepared nanosensors (0.2-20 pm) for sodium, potassium and calcium using the precipitation method. Similarly to the previous works, the plasticized poly(vinyl chloride) included a phenoxazine chro-moionophore, a lipophilic ion exchanger and a cation-selective ionophore. The dynamic range of the very selective sensors was 5 x 10 4-0.5 M for sodium, 1 x 10 5-0.1 M for potassium and 2 x 10 4 - 0.05 M for calcium. As was demonstrated by Bakker and co-workers [45] a particle caster can be used can be used for preparation of much larger beads (011 pm). 

Bis[2-benzoylphcnyl] Ditellurium [Potassium Hydroxide Method]3 To 200 ml of ethanolic potassium hydroxide are added 16.5 g (48 mmol) of 2-benzoylphenyl tellurium chloride and the mixture is heated until the reddish color disappears and potassium chloride precipitates. The mixture is poured into cold water and the ditellurium compound is extracted with chloroform. The extract is dried, evaporated to dryness, and the residue is recrystallized from benzene yield 12.3 g (83%) m.p. 139°. 

Special attention is to be paid to alkali metals. Their reduction potentials are very negative (above -2V vs. SCE) and the electrolyte components must be reducible at very high negative potentials. The tetra-alkylammonium bases or salts are very convenient for such purposes these must be pure. The small variability of the half-wave potential of the reduction of sodium, potassium, rubidium and caesium ions makes impossible their polarographic discrimination. The half-wave potential of lithium is about 200 mV more negative than that of sodium or potassium and therefore it can be determined in the presence of up to a 10-fold excess of sodium or potassium. Some methods for separate determination of sodium and potassium have been described [17]. This procedure is based on the preliminary separation of the potassium by the perchlorate precipitation. 

The catalysts were prepared by co-precipitation method from aqueous solution of metal nitrates of Cu, Zn, Fe, and Cr and NaOH aqueous solution. Potassium was impregnated to the precipitate with KjCOj aqueous solution. The composition of catalysts were as follows CAT A K/Cu-Zn-Fe=0.077/l-l-3, CAT B K/Cu-Zn-Fe-Cr=0.077/l-l-3-0.1. The hydrogenation of CO2 was performed with a conventional flow reactor for about 150 hours at 300 °C and 7.0MPa. The structures of catalysts were identified by means of Rigaku RINT 2000 X-ray diffractometer. The observation of catalyst particles and the microanalysis of their compositions were carried out by means of Hitachi HF-2000 field emission transmission electron microscope and Kevex DELTA plus 1 energy-dispersive X-ray spectrometer. 

The better known methods for the removal of cerium from rare earth mixtures depend upon the ease of oxidation of cerium and the subsequent precipitation of cerium(IV) compounds by hydrolysis. Among these are the permanganate-phosphate/ the permanganate-cerium dioxide, the electrolytic, and the potassium bromate methods. The method of G. F. Smith, in which ammonium-cerium(IV) nitrate is crystallized from a nitric acid solution of the rare earths in the presence of an excess of ammonium nitrate, is particularly valuable as a commercial method for the production of large amounts of very pure cerium compounds. 

The principal commercial source of rubidium is accumulated stocks of a mixed carbonate produced as a byproduct in the extraction of lithium salts from lepidohte. Primarily a potassium carbonate, the byproduct also contains ca. 23 wt.% rubidium and 3 wt.% cesium carbonates. The primary difficulty associated with the production of either pure rubidium or pure cesium is that these two elements are always found together in nature and also are mixed with other alkali metals because these elements have very close ionic radii, their chemical separation encounters numerous issues. Before the development of procedures based on thermochemical reduction and fractional distillation, the elements were purified in the salt form through laborious fractional crystallization techniques. Once pure salts have been prepared by precipitation methods, it is a relatively simple task to convert them to the free metal. This is ordinarily accomplished by metallothermic reduction with calcium metal in a high-temperature vacuum system in which the highly volatile alkali metal is distilled from the solid reaction mixture. Today, direct reduction of the mixed carbonates from lepidolite purification, followed by fractional distillation, is perhaps the most important of the commercial methods for producing rubidium. The mixed carbonate is treated with excess sodium at ca. 650 C, and much of the rubidium and cesium passes into the metal phase. The resulting crude alloy is vacuum distilled to form a second alloy considerably richer in rubidium and cesium. This product is then refined by fractional distillation in a tower to produce elemental rubidium more than 99.5 wt.% pure. 

In neutral solution, the indicator is potassium chromate(VI). In acid solution the CrOj" ion changes to CrjO (p. 378). and since silver dichromatefVI) is soluble, chromate(VI) is not a suitable indicator other methods can be used under these conditions. (In alkaline solution, silverfl) oxide precipitates, so silver(I) nitrate cannot be used under these conditions.)... 

Saponification of esters. Aqueous sodium hydroxide method. To hydrolyse an ester of an alcohol, reflux 5-6 g. with 50 ml. of 20 per cent, sodium hydroxide solution for 1-2 hours or until the ester layer disappears. Distil the alkahne mixture and collect about 6 ml. of distillate. This will contain any volatile alcohol formed in the saponification. If the alcohol does not separate, i.e., is water-soluble, saturate the distillate with sohd potassium carbonate an upper layer of alcohol is then usually formed. (The alcohol may be subsequently identified as the 3 5-dinitrobenzoate see Section 111,27,2.) Cool the residual alkahne mixture, and acidify it with dilute sulphuric acid. If no crystalline acid is precipitated, the acid may frequently be isolated by ether extraction, or it may be distilled from the acidified solution and isolated from (or investigated in) the distfllate. (The acid may be subsequently identified, e.g., as the S benzyl wo-thiuronium salt see Section 111,85,2.)... 

After 5 hours the reaction is stopped and the flask cooled. The formyl-MDA can be isolated and hydrolyzed by any of the ways Strike just mentioned a few paragraphs back, but this method offers a third, very convenient way which should be tried. What the chemist does is forget about letting the flask and its contents cool. Instead, she removes the oil bath, places the flask back on the stirplate (distillation setup still attached), attaches a vacuum and distills off all the formamide. What remains is a dark, heavy formyl-MDA precipitate that is allowed to cool down while the chemist makes up a solution of 150g potassium hydroxide (KOH), 500mL ethanol and 125mL dH20. This solution is poured into the... 

Fluorozirconate Crystallization. Repeated dissolution and fractional crystallization of potassium hexafluorozirconate was the method first used to separate hafnium and zirconium (15), potassium fluorohafnate solubility being higher. This process is used in the Prinieprovsky Chemical Plant in Dnieprodzerzhinsk, Ukraine, to produce hafnium-free zirconium. Hafnium-enriched (about 6%) zirconium hydrous oxide is precipitated from the first-stage mother Hquors, and redissolved in acid to feed ion-exchange columns to obtain pure hafnium (10). 

Soluble sulfides such as sodium sulfide, potassium sulfide, and calcium polysulfides have been used to precipitate mercury salts from alkaline solutions. When this procedure is used, exercise of caution is requked to maintain the pH within a given alkaline range so as to prevent evolution of H2S. Because the solubiUty of mercuric sulfide in water is 12.5 flg/L at 18°C or 10.7 ppb of mercury, use of this method for removal of mercury is adequate for most purposes. However, the presence of excess alkah, such as sodium hydroxide or sodium sulfide, increases the solubiUty of mercuric sulfide as shown ... 

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