Separation potassium

Fig. 3-137. Dependence of the retention of monovalent cations on the ionic strength of the eluent for sodium, ammonium, and potassium. - Separator column IonPac CS1 eluent HC1 flow rate 2.3 mL/min detection suppressed conductivity.

Fig. 6-19. Indirect photometric detection of sodium, ammonium, and potassium. - Separator column Dowex 50 eluent 0.005 mol/L copper sulfate flow rate 0.7 mL/min detection UV (252 nm, indirect) injection volume 20 pL solute concentrations 230 ppm sodium, 180 ppm ammonium, and 391 ppm potassium (taken from [29]).

If, for example, a membrane selective for potassium separates a compartment of high-concentration potassium chloride solution from another of lower concentration, there is a diffusion-driven current J ff across the membrane. The value of this is given by a version of Pick s law ... 

Using sodium tetraphenylborate solution, caesium is precipitated together with rubidium and potassium, separated off, dissolved in a mixture of acetone and methyl isobutyl ketone and determined by atomic absorption analysis. 

KCl —NaCl —MgS04) and in many brines. Separated by fractional crystallization, soluble water and lower alcohols. Used in fertilizer production and to produce other potassium salts. 

A first approach to testing, ASTM D 1094, is to create, using a potassium phosphate reagent, a separation between two layers, hydrocarbon and aqueous. The degree of separation of the two phases is estimated by attributing a grade from 1 to 3 and the appearance of the interface by five levels of observation 1, lb, 2, 3, and 4. The specifications establish both the quality of separation (2 is the maximum) and the appearance of the interface (lb maximum). 

Hydrolysis of Potassium Ethyl Sulphate. Dissolve about i g. of the crystals in about 4 ml. of cold distilled water, and divide the solution into two portions, a) To one portion, add barium chloride solution. If pure potassium ethyl sulphate were used, no precipitate should now form, as barium ethyl sulphate is soluble in water. Actually however, almost all samples of potassium ethyl sulphate contain traces of potassium hydrogen sulphate formed by slight hydrolysis of the ethyl compound during the evaporation of its solution, and barium chloride almost invariably gives a faint precipitate of barium sulphate. b) To the second portion, add 2-3 drops of concentrated hydrochloric acid, and boil the mixture gently for about one minute. Cool, add distilled water if necessary until the solution has its former volume, and then add barium chloride as before. A markedly heavier precipitate of barium sulphate separates. The hydrolysis of the potassium ethyl sulphate is hastened considerably by the presence of the free acid Caustic alkalis have a similar, but not quite so rapid an effect. 

Place 0 5 ml. of acetone, 20 ml. of 10% aqueous potassium iodide solution and 8 ml. of 10% aqueous sodium hydroxide solution in a 50 ml. conical flask, and then add 20 ml. of a freshly prepared molar solution of sodium hypochlorite. Well mix the contents of the flask, when the yellow iodoform will begin to separate almost immediately allow the mixture to stand at room temperature for 10 minutes, and then filter at the pump, wash with cold w ater, and drain thoroughly. Yield of Crude material, 1 4 g. Recrystallise the crude iodoform from methylated spirit. For this purpose, place the crude material in a 50 ml. round-bottomed flask fitted with a reflux water-condenser, add a small quantity of methylated spirit, and heat to boiling on a water-bath then add more methylated spirit cautiously down the condenser until all the iodoform has dissolved. Filter the hot solution through a fluted filter-paper directly into a small beaker or conical flask, and then cool in ice-water. The iodoform rapidly crystallises. Filter at the pump, drain thoroughly and dry. 

Add 5 g. of potassium hydrogen tartrate and 5 g. of antimony trioxide (each being finely powdered) to 30 ml. of water contained in a small flask, and boil the mixture under a reflux water-condenser for 15 minutes. Then filter hot, using a Buchner funnel and flask which have been preheated by the filtration of some boiling distilled water. Pour the clear filtrate into a beaker and allow to cool. Potassium antimonyl tartrate separates as colourless crystals. Filter, drain and dry. Yield, 5 g. The product can be recrystallised from hot water, but this is usually not necessary. 

The crude acetonitrile contains as impurity chiefly acetic acid, arising from the action of phosphoric acid on the acetamide. Therefore add to the nitrile about half its volume of water, and then add powdered dry potassium carbonate until the well-shaken mixture is saturated. The potassium carbonate neutralises any acetic acid present, and at the same time salts out the otherwise water-soluble nitrile as a separate upper layer. Allow to stand for 20 minutes with further occasional shaking. Now decant the mixed liquids into a separating-funnel, run off the lower carbonate layer as completely as possible, and then pour off the acetonitrile into a 25 ml, distilling-flask into which about 3-4 g. of phosphorus pentoxide have been placed immediately before. Fit a thermometer and water-condenser to the flask and distil the acetonitrile slowly, collecting the fraction of b.p. 79-82°. Yield 9 5 g. (12 ml.). 

If only 100 ml. separating-funnels are available, the distillate must be divided into two portions and each extracted with ether as described, the final ether extracts being united for drying with potassium hydroxide. 

To the cold solution, add about 2 ml. of 10% potassium iodide solution. A brisk effervescence of nitrogen occurs, and iodobenzene separates, usually as drops so small that in spite of their density they float on the surface. 

Now transfer the cold distillate to a separating-funnel, and shake vigorously with about 50-60 ml. of ether run oflF the lower aqueous layer and then decantf the ethereal solution through the mouth of the funnel into a 200 ml. conical flask. Replace the aqueous layer in the funnel, and extract similarly twice more with ether, combining the ethereal extracts in the conical flask. Add 3-4 g. of dry powdered potassium carbonate to the ethereal solution, securely cork the flask and shake the contents gently. The ethereal solution of the phenol... 

Add 5 g. of powdered potassium cyanide to a mixture of 20 ml. of water and 50 ml. of ethanol contained in a 200 ml. conical flask, and then add 25 mi. (26 g.) of freshly distilled benzaldehyde. Fit the flask with a reflux water-condenser, and boil the mixture gently on a water-bath for 30 minutes, a clear solution being rapidly obtained. Then pour the solution into a beaker and cool the benzoin separates as a crystalline mass... 

Dissolve 5 g. of benzii in 15 ml. of boiling ethanol in a conical flask fitted with a reflux water-condenser. Then add a solution of 5 g. of potassium hydroxide in 10 ml. of water, and heat the mixture (which rapidly develops a purple colour) on a boiling water-bath for about 15 minutes. Cool and stir the solution, from which the potassium benzii ate separates in fine cr> stals. 

To obtain the free acid, dissolve the potassium salt in 50 ml. of cold water, filter the solution if a small undissolved residue remains, and then boil the clear solution gently whilst dilute sulphuric acid is added until the separation of the acid is complete. Cool the solution and filter off the pale orange-coloured crystals of the benzilic acid wash the crystals on the filter with some hot distilled water, drain well, and then dry in a desiccator. Yield of crude acid, 4 g. Recrystallise from benzene (about 50 ml.) to which a small quantity of animal charcoal has been added, filtering the boiling solution through a preheated funnel fitted w ith a fluted filter-paper, as the benzilic acid readily crystallises as the solution cools alternatively, recrystallise from much hot water. The benzilic acid is obtained as colourless crystals, m.p. 150°. 

Extract the dimethylaniline by shaking the distillate in a separating-funnel with a few ml. of ether, and then dry the ethereal solution over potassium carbonate distil the filtered ethereal solution from a small distilling-flask e.g, Fig. 36, p. 63) with the usual precautions, and finally the dimethylaniline, b.p. 193°. Yield, almost theoretical. 

Transfer the quinoline chlorozincate to a beaker, add a small quantity of water, and then add 10% sodium hydroxide solution until the initial precipitate of zinc hydroxide completely redissolves, and the free quinoline separates. Transfer the mixture to a separating-funnel, wash out the beaker with ether, adding the washings also to the solution in the funnel, and then extract the quinoline twice with ether. Dry the united ethereal extracts by adding an ample quantity of powdered potassium hydroxide and... 

In preparing this mixture, the lactose and the potassium nitrate should be powdered separately and then mixed solely by shying. They should not be ground together in a mortar. 

This type of extraction depends upon the use of a reagent which reacts chemically with the compound to be extracted, and is generally employed either to remove small amounts of impurities in an organic compound or to separate the components of a mixture. Examples of such reagents include dilute (5 per cent.) aqueous sodium or potassium hydroxide solution, 5 or 10 per cent, sodium carbonate solution, saturated sodium bicarbonate solution (ca. 5 per cent.), dilute hydrochloric or sulphuric acid, and concentrated sulphuric acid. 

Method 2 (from potassium bromide and sulphuric acid). Potassium bromide (240 g.) is dissolved in water (400 ml.) in a litre flask, and the latter is cooled in ice or in a bath of cold water. Concentrated sulphuric acid (180 ml.) is then slowly added. Care must be taken that the temperature does not rise above 75° otherwise a little bromine may be formed. The solution is cooled to room temperature and the potassium bisulphate, which has separated, is removed by flltration through a hardened Alter paper in a Buchner funnel or through a sintered glass funnel. The flltrate is distilled from a litre distilling flask, and the fraction b.p. 124 127° is collected this contains traces of sulphate. Pure constant boiling point hydrobromic acid is obtained by redistillation from a little barium bromide. The yield is about 285 g. or 85 per cent, of the theoretical. 

Bromine. The commercial product may be dried (and partially purified) by shaking with an equal volume of concentrated sulphuric acid, and then separating the acid. Chlorine, If present, may be removed by fractionation in an all-glass apparatus from pure potassium bromide the b.p. is 59°/760 mm. The analytical reagent grade is satisfactory for most purposes where pure bromine is required. 

Silver nitrite. Warm concentrated solutions of silver nitrate (containing 48 g. of AgNOj) and potassium nitrite (containing 30 g. of KNOj) are mixed, and the mixture is allowed to cool. The silver nitrite which separates is filtered off and washed with water. It may be recrystallised from water at 70°, and is dried either in a vacuum desiccator or in an air oven at about 40° the yield is about 90 per cent. Silver nitrite should be stored in an tightly-stoppered amber bottle. 

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