Radiochemical separation of zirconium from niobium with salicylhydroxamic acid

Salicylhydroxamic acid was employed (or the rapid radiochemical separation of zirconium from niobium. Neutron-deficient isotopes of the 2 elements formed in the spallation of niobium with 340-MeV protons were used as tracers.The method was employed in the study of short-lived zirconium and niobium activities using scintillation γ-spectrometry. The procedure is complete in about 7 min, and gives a chemical yield of the order of 50–60% and a decontamination factor of at least 5· 10⁴.     

Gravimetric estimation of zirconium by m-Ethyl phenoxyacetic acid

Summary m-Ethyl phenoxyacetic acid is found to be a selective reagent for the estimation of zirconium. Even 2.2 mg of zirconia can be easily estimated. The composition of the precipitate is somewhat variable and so direct weighing is not possible. The difficulty is overcome by igniting the precipitate and weighing it as oxide. Zn, Ca, Ba, Be, Mg, UO₂, Th, Mn, Co, Ni, Al, Ce, Ti, Fe, and Sn ions do not interfere in the precipitation of zirconium. Cr and V₂O₂ are coprecipitated with zirconium but they can be easily removed by double precipitation. Quantitative results are also obtained even in the presence of SO₄.     

Gravimetric determination of thorium and zirconium

Summary Thorium and zirconium can be quantitatively precipitated by quinaldinic acid atph 2.7 and 3, respectively. As the precipitates are of nonstoichiometric composition they are to be ignited to oxides. By this reagent thorium can be quantitatively separated from arsenic (As³⁺), mercury (Hg²⁺), rare earths, manganese, magnesium and alkaline earths and zirconium from all the aforesaid ions excepting rare earths which contaminate to a slight extent.     

Gravimetric determination of zirconium with a new azopyrazolone derivative

3-Methyl-5-oxo-1-phenyl-2-pyrazolin-4-ylazo-2'-(6',8'-naphthalenedisulfonic acid) (disodium salt) is proposed as a new reagent for the gravimetric determination of zirconium. The precipitate formed at pH 1–1.5 can be weighed directly and there are few interferences.     

Gravimetric determination of barium in zirconium metal and in certain zirconium salts

Barium may be determined gravimetrically in quantities ranging from 0.2 to 2.0 mg (± o.1 mg) in hydrated zirconyl chloride and in zirconium metal after complete separation of the zirconium. As much as 10 g of zirconium may be removed by a double precipitation in a (3 to 1) hydrochloric acid medium followed by a cupferron precipitation-chloroform extraction of the residual zirconium. The barium is then determined gravimetrically as barium sulfate in the iron-free, zirconium-free filtrate by precipitation with an excess of ammonium sulfate. As much as 0.015% barium has been found in impure zirconyl chloride, 0.004% in commercial “purified” zirconyl chloride, 0.000% barium in crystal bar zirconium metal and 0.003% barium in zirconium metal sheet. Reproducibility is 0.001%.     

Gravimetric determination of molybdenum and its separation from other metals with n-benzoylphenylhydroxylamine

N-Benzoylphenylhydroxylamine is employed as a precipitant for the determination of molybdenum (VI). The precipitate can be weighed either directly or as molybdenum trioxide after ignition. Molybdenum can be determined in the presence of appreciable amounts of iron(III), cobalt(II), copper(II), chromium(VI) and vanadium (V).     

Anion-exchange separation of uranium (VI) from thorium,zirconium, titanium,lanthanides and other elements in malonic and ascorbic acid media

Summary The anion-exchange behaviour of uranium (VI) has been studied extensively in various mineral acid media [1], but similar studies with organic acid solutions are lacking. Although the negatively charged complex of uranium in acetic acid was studied [2, 3], very small amounts of uranium could be separated and phosphate interfered. Such studies were further extended to non-aqueous media [4]. The anionic ascorbate complex of uranium and thorium were separated by selective elution with 1 mol dm^–3 hydrochloric acid and 3 mol dm^–3 sulphuric acid [5–7] respectively. Some attempts were also made to study complexes of uranium in formic and propionic acid [1] and it was separated from copper and thorium in oxalate media [4]. However systematic studies in malonate and to some extent in ascorbate media are lacking. This paper presents such studies.     

Oxide layers with titanium and zirconium phosphates

Oxide-phosphate layers 20 to 150 μm thick were obtained on titanium by plasma electrolytic deposition in individual and mixed aqueous electrolytes with polyphosphate complexes of zirconium(IV), barium(II), and copper(II). Formation features, thickness, elemental and phase compositions, and surface morphology of the films are presented. Depending on the electrolyte composition, synthesis conditions, and temperature of annealing in air, some simple and double phosphates of titanium and zirconium are formed, including ZrP₂O₇, NaTi₂(PO₄)₃, BaTi₂(P₂O₇)₂, Zr_0.2Ti_0.8P₂O₇, and CuTi₂(PO₄)₃.     

Gravimetric determination of selenium from perchloric acid solution with hydrazine

The gravimetric determination of selenium, by reduction of selenious acid in perchloric acid solution with hydrazine hydrate, has been studied in detail. Elemental selenium is completely precipitated in 3.2-5.1M perchloric acid at room temperature or 100 degrees C. One mole of selenious acid reacts with one mole of hydrazine hydrate to give elemental selenium.     

Determination of microamounts of zirconium(IV) and titanium(IV) with preliminary TLC separation

By the application of thin-layer chromatography on silica gel H and the solvent system consisting of 6 M HCl:acetylacetone: 9 M H₂SO₄ (60:2:1, v/v/v), zirconium and titanium have been quantitatively separated from each other, as well as from numerous other interfering ions. The efficiency of the chromatographic separation was evaluated by semiquantitative determination of zirconium and titanium by visual colorimetry of spots in situ, as well as by spectrophotometric determination of zirconium with rutin after its elution from silica gel H thin-layer.     

Ion-exchange separation of vanadium, zirconium, titanium, molybdenum, tungsten and niobium

Schemes for the separation of two or more of the elements vanadium, zirconium and/or titanium, molybdenum and tungsten from each other and from relatively large amounts of niobium have been developed, a strongly basic anion-exchange resin being used. Interference from niobium is avoided by using hydrofluoric acid to elute vanadium, zirconium, titanium and molybdenum. The application of coupled columns to improve the efficiency of separation of multicomponent mixtures is demonstrated. The use of an "interval" equation defining the volume interval between successively eluted solutes is proposed for calculating the column length required for a particular separation. This equation is especially useful for determining the extent to which a column must be lengthened when overlapping occurs because of high column loading.     

Cation-exchange separation of hafnium and zirconium from accompanying ions

Hafnium and zirconium are not retained on the strongly acidic cation-exchange resin Dowex 50 from a mixture consisting of methanol and 12M nitric acid (19:1) which is 0.1M in trioctylphosphine oxide. On the other hand most other elements investigated are strongly adsorbed on the resin from this medium so that they are readily separated from hafnium and zirconium. These elements include titanium, rare earths, alkali metals, alkaline earth metals, iron, cobalt, manganese and zinc. This separation technique has been found to be suitable for the separation of tracer and milligram amounts of hafnium and zirconium from accompanying metal ions. If in place of methanol other organic solvents such as acetone, tetrahydrofuran and methyl glycol are used the selectivity of the separation of zirconium and hafnium from the other elements is decreased. The same effect is observed when hydrochloric acid is used in the mixtures instead of nitric acid.     

Radiochemical separation of zirconium and hafnium from other radionuclides

Radiozirconium and radiohafnium may be separated from all other radionuclides except scandium and protactinium by precipitation with mandelic acid from 5-10 M hydrochloric acid, using commercial zirconyl chloride as carrier. Scandium and protactinium are removed by dissolving the precipitate in sodium carbonate, then adding barium nitrate to precipitate barium carbonate which acts as a scavenger. Zirconium mandelate is finally reprecipitated and the sample weighed and counted in this form. The method was checked by analysing commercial zirconyl chloride and standard rock samples for zirconium and hafnium by neutron-activation analysis.     

Cation chromatography on stannic tungstate papers: Quantitative separation of vanadium from iron,titanium, zirconium and thorium

Summary A systematic study of the chromatography of metal ions on stannic tungstate papers has been performed using acetone-HNO₃–H₂O systems. The effect of mole fractions of acetone, HNO₃ and H₂O on the R_f values of the metal ions has been discussed in detail and a relationship between R_f and mole fraction (X) of the solvent has been obtained as R_f=mX+C. The usefulness of the study has been demonstrated by the specific extraction of titanium and thorium in HNO₃H₂O (12) and HNO₃:acetone:H₂O (161) systems. In addition, some binary and ternary separations of metal ions have also been achieved on these papers.     

Gravimetric estimation of thorium with N-phenylanthranilic acid

Summary From nitric or hydrochloric acid medium thorium is quantitatively precipitated by N-phenylanthranilic acid in the range of pH 1.5–3.4 as a light yellow compound, which can be dried to a definite composition, Th(C₁₃H₁₀NO₂)₄, at 110° C. This has been utilized for the direct gravimetric estimation of thorium and its separation from uranium(VI), cerium(III), aluminium and iron at a pH of ca. 2.0–2.5.This method is superior to most of the existing methods for the estimation of thorium since quantitative precipitation occurs at a relatively low pH and the thorium compound, which has a high molecular weight, can be weighed directly, thus making possible the determination of rather small quantities (ca. 5 mg) of thorium with fair accuracy (error less than 1%).

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Zusammenfassung Thorium kann aus salpeter-oder salzsaurer Lösung im pH-Bereich 1,5–3,4 mit Hilfe von N-Phenylanthranilsäure als hellgelber Niederschlag quantitativ ausgefällt werden. Der Mederschlag kann bei 110°C zu definierter Zusammensetzung getrocknet werden [Th(C₁₃H₁₀NO₂)₄]. Diese Fällung wurde zur direkten gravimetrischen Bestimmung von Thorium und seiner Trennung von Uran(VI), Cer(III), Aluminium und Eisen bei pH 2,0–2,5 benutzt. Das Verfahren ist den meisten bekannten Methoden überlegen, das die Fällung bei relativ niedrigem pH durchgeführt und die Thoriumverbindung (die ein hohes Molekulargewicht hat) direkt gewogen werden kann. Kleine Mengen Thorium (etwa 5 mg) können mit recht guter Genauigkeit bestimmt werden (Fehler kleiner als 1%).

     

Gravimetric determination of cadmium with N-phenylbenzohydroxamic acid

A quantitative gravimetric determination of cadmium in presence of Ag(+), Be(2+), Pb(2+), Mn(2+), Ni(2+), Cu(2+), Zn(2+), Hg(2+), Pd(2+), Ga(3+), Al(3+), Bi(3+), Sb(3+), La(3+), Ti(4+), Zr(4+), V(5+), Mo(6+) and U(6+) was made by selective precipitation with N-phenylbenzohydroxamic acid from a solution containing 6-15 mg of cadmium acetate at pH 5.8-6.5. The precipitate was weighed directly after drying at 110-120 degrees . The cadmium complex is curdy white, granular and melts at 225 degrees. The analytical results indicate the complex to be (C(13)H(10)NO(2))(2)Cd.