Separation barium

We wish to separate barium ions from calcium ions by selective precipitation. Which anion, fluoride or carbonate, would be the better choice for achieving this precipitation Why ... 

Generally impurities in the oxidizers or other inorganic materials disturb the flame colour. Strontium salts usually contain some barium salt as an impurity which produces the undesirable spectrum BaCl or BaOH band and disturbs the colour of the flame. Accordingly it is necessary to use strontium salts of high purity to obtain a good red flame. Strontium and barium belong to the same group of elements, and it is difficult to separate barium and strontium salts industrially, but in a laboratory strontium salts can be purified until they have a barium content of less... 

An outline of the method used for determination of radiostrontium in various materials by nitrate precipitation is as follows. The ashed material is dissolved in nitric acid in the presence of strontium and barium carriers. The nitric acid concentration is then increased to precipitate all the strontium and barium (and part of the calcium) as nitrates. After further nitric acid separations, barium chromate and iron hydroxide scavenges are carried out. The subsequent treatment depends somewhat on the circumstances but the following is normal practice. 

Interferences from fission of uranium which might not have been removed by the preirradiation procedure were checked by separating barium from the irradiated samples and looking for La-activi-... 

Figure 66. ISS spectra from a tungsten surface containing oxygen and barium, using a mixture of He and Ne to analyze for oxygen as well as separate barium and tungsten 1215]...

Other inorganic reagents may be used in some cases in order to carry out the fractional precipitation of some metallic ions. Such is the case of chromate ion Cr042 , which permits us to precipitate and separate barium and strontium ions from each other (see the following exercise). 

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. 

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. 

Mix 200 g. of adipic acid intimately with 10 g. of finely-powdered, crystallised barium hydroxide. Place the mixture in a 1-litre distilling flask, fitted with a thermometer reaching to within 5 mm. of the bottom connect the flask with a condenser and receiver. Heat the mixture gradually in an air bath (1) to 285-295° during about 90 minutes and maintain it at this temperature mitil only a small amount of dry residue remains in the flask this requires a further 2 hours. The temperature must not be allowed to rise above 300°, since at this temperature the adipic acid distils quite rapidly the best working temperature is 290°. The cycZopentanone distils slowly accompanied by a little adipic acid. Separate the ketone from the water in the distillate, and dry it with anhydrous potassium carbonate this treatment simultaneously removes the traces of adipic acid present. Finally distil from a flask of suitable size and collect the cycZopentanone at 128-131°. The yield is 92 g. 

The most significant commercial product is barium titanate, BaTiO, used to produce the ceramic capacitors found in almost all electronic products. As electronic circuitry has been rniniaturized, demand has increased for capacitors that can store a high amount of charge in a relatively small volume. This demand led to the development of highly efficient multilayer ceramic capacitors. In these devices, several layers of ceramic, from 25—50 ]lni in thickness, are separated by even thinner layers of electrode metal. Each layer must be dense, free of pin-holes and flaws, and ideally consist of several uniform grains of fired ceramic. Manufacturers are trying to reduce the layer thickness to 10—12 ]lni. Conventionally prepared ceramic powders cannot meet the rigorous demands of these appHcations, therefore an emphasis has been placed on production of advanced powders by hydrothermal synthesis and other methods. 

Laser isotope separation techniques have been demonstrated for many elements, including hydrogen, boron, carbon, nitrogen, oxygen, sHicon, sulfur, chlorine, titanium, selenium, bromine, molybdenum, barium, osmium, mercury, and some of the rare-earth elements. The most significant separation involves uranium, separating uranium-235 [15117-96-1], from uranium-238 [7440-61-1], (see Uranium and uranium compounds). The... 

The fused product contains about 60—85% barium sulfide, unreacted barium sulfate, and impurities present in barite and ash. The soluble barium sulfide is extracted from the mixture with water and separated from the insoluble impurities by filtration. 

The properties of hydrated titanium dioxide as an ion-exchange (qv) medium have been widely studied (51—55). Separations include those of alkaH and alkaline-earth metals, zinc, copper, cobalt, cesium, strontium, and barium. The use of hydrated titanium dioxide to separate uranium from seawater and also for the treatment of radioactive wastes from nuclear-reactor installations has been proposed (56). 

The classical analytical method of deterruination of barium ion is gravimetric, by precipitating and weighing insoluble barium sulfate. Barium chromate, which is more insoluble than strontium chromate in a slightly acidic solution, gives a fairly good separation of the two elements. 

Alkaline-earth metals are often deterruined volumetricaHy by complexometric titration at pH 10, using Eriochrome Black T as indicator. The most suitable complexing titrant for barium ion is a solution of diethylenetriaminepentaacetic acid (DTPA). Other alkaline earths, if present, are simultaneously titrated, and in the favored analytical procedure calcium and strontium are deterruined separately by atomic absorption spectrophotometry, and their values subtracted from the total to obtain the barium value. 

Barium can also be deterruined by x-ray fluorescence (XRF) spectroscopy, atomic absorption spectroscopy, and flame emission spectroscopy. Prior separation is not necessary. XRF can be appHed directly to samples of ore or products to yield analysis for barium and contaminants. AH crystalline barium compounds can be analy2ed by x-ray diffraction. 

The chemical identities of the fission products determine their subsequent redistribution, those elements which are in the gaseous state at the temperature of the operation migrating to the cooler exterior of the fuel rods, and die less voltile elements undergoing incorporation in the fuel rod in solid solution. Thus caesium and iodine migrate to the gas fill which sunounds the fuel rod, and elements such as the rare earths and zirconium are accommodated in solid solution in UO2 without significant migration along the fuel rod radius. Strontium and barium oxidize to form separate islands which can be seen under the microscope. 

Physovenine, Cl4Hig03N2, was obtained by Salway from the mother liquors left after the separation of eseramine. It crystallises from a mixture of benzene and light petroleum in small, colourless prisms, m.p. 123°. Its salts are dissociated by water. With barium hydroxide physovenine liberates carbon dioxide and assumes a deep red colour, and, owing to the similarity of this behaviour with that of physostigmine, Salway suggested that physovenine may be an intermediate product in the formation of eseroline from physostigmine. 

Two grams of the oU are saponified the portion insoluble in water separated by shaking with ether, and the aqueous solution neutralised with acetic acid. The solution is dUuted to 50 c.c. and 10 c.c. of cold saturated solution of barium chloride added. It is then warmed for two hours on a water-bath and allowed to cool. If a crystalline deposit is formed, the oil is to be considered adulterated, as the acids contained in normal lavender oil, acetic and butyric acids, give soluble barium salts. It is evident that this test will only detect those acids whose barium salts are insoluble. A more comprehensive test is therefore needed, as several other esters have since been employed for adulteration purposes. Glycerin acetate, prepared by the acetylation of glycerine, was first de-... 

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