Determination of 14 rare earth impurities in Y2O3 by petroleum sulfoxide extraction chromatography

Petroleum sulfoxide-NH4SCN extraction chromatography was developed for the separation of Y from other rare earth elements. Some chromatographic parameters were chosen and separation factors between Y and other rare earth elements were determined. A column of resin coated with petroleum sulfoxide was used. The Y in the sample was eluted with NH4SCN, then titrated with EDTA. The recovery was 67%-120% and relative standard deviation +/-4.0%-19.4%. This method can be applied to the determination of trace amounts of rare earth impurities in Y2O3 with a purity of 99.999 9%-99. 999 99%.

Determination of rare-earth impurities in ultra-highly pure Er2O3 and Ho2O3 by [HEH(HEP)] extraction chromatography-atomic emission spectrometry

This article applied [HEH(HEP)] (2-ethyhexyldrogen-2-ethylhexyl phosphonate)extraction chromatography to separate 14 rare earth impurities from ultra-highly pure Er2O3 and Ho2O3, and then the impurities were determined by atomic emission spectrometry. The average percentage recovery for each element is in the range of 70%similar to 140%. The relative standard deviations of the determination are +/-3.3%similar to 2.2%. This method can be applied to the determination of the trace amounts of rare eath impurities in Er2O3 and Ho2O3 with a purity of 99.999 9%-99.999 99%.

Separation of Th4+ and RE3+ with hollow fiber extraction

Separation of Th4+ and RE3+ was investigated by hollow fiber membrane extraction with N1923 in countercurrent recirculating operation. The effect of Hf concentration in aqueous phase and flow rates of aqueous and organic phases on mass transfer coefficient was tested. Then the extraction of Th4+ from RE sulfate obtained from Baotou ore was carried out. The results obtained show that the mass transfer coefficient of Th4+ changes with the flow rate of aqueous phase, but does not change with the flow rate of organic phase and H+ concentration in aqueous phase, which suggests that the mass transfer rate of Th4+ is controlled bg that in the water critical layer, The mass transfer rate of RE3+ does not change with the flow rate of water phase, changes a little with the flow rate of organic phase, and changes with H+ concentration, which suggests that the mass transfer rate is controlled by their reaction rate with N1923. Th4+ could be extracted completely in 8 h from RE sulfate solution of Baotou ore with relatively less extraction of RE3+. So the separation of radioactive element under the sealed condition could be done.

High efficient extraction of M@C-2n (M = La, Ce) by a high pressure and high temperature method

A high pressure and high temperature method was used to efficiently extract on a large scale metallofullerenes M@C-2n (M=La,Ce) in a closed vessel under argon gas protection. With pyridine as the HPHT solvent, about 60-80% M@C-2n and 30-55% M@C-82 can be enriched, M@C-82 is dissolved selectively; With toluene as the HPHT solvent, M@C-2n can also be efficiently extracted, especially M@C-74, which is a new member of M@C-2n soluble species. (C) 1998 Elsevier Science Ltd. All rights reserved.

High temperature and high pressure extraction of lanthanofullerenes by using different solvents

The traditional Soxhlet extraction of lanthanofullerenes was improved and the high temperature and high pressure method with different extraction solvents was used. It's found that La@C-2n can be efficiently extracted with toluene and pyridine from the insoluble part of the soot after the toluene Soxhlet extraction. Pyridine can more efficiently and selectively extract lanthofullerenes, especially La@C-82, while toluene can extract La@C-74, which is a new member added to the soluble species to lanthanofullerenes.

Separation of Ce(IV) and RE(III) with hollow fiber membrane-based extraction

Separation of Ce(IV) and RE(III) was investigated by hollow fiber membrane-based extraction with contercurrent recirculating operation. The mass transfer coefficients of Ce(IV) and RE(III) and the effective factors to them were tested. The results show the mass transfer coefficient of Ce(IV) is larger than that of RE(III), and their mass transfer mechanism is different. The mass transfer of Ce(IV) was controlled by the resistance in water critical layer due to its more rapid interfacial reaction rate and larger distribution coefficient, which was different from RE(III) mass transfer with a slow interfacial reaction rate and small distribution coefficient. Ce(IV) was separated from the mixed solution of Ce(IV) and RE(III) by means of the difference of their mass transfer rates.

Solvent extraction of scandium(III) by Cyanex 923 and Cyanex 925

The extraction equilibria of Sc(III), Zr(IV), Ti(IV), Th(IV), Fe(III) and Lu(III) from sulphuric or hydrochloric acid media by Cyanex 923 (mixture of straight chain alkylated phosphine oxides) and Cyanex 925 (mixture of branched chain alkylated phosphine oxides) were studied at various aqueous acidities. The extractant Cyanex 923 demonstrated better scandium loading and selectivity for TI(IV). Fe(III) and Lu(III) than Cyanex 925. The effects of extractant concentration on the extractions of sulphuric acid and Sc(III) by Cyanex 923 were examined. The stoichiometries of the extraction reactions were postulated based on slope analysis. The experimental results indicate that Cyanex 923 can be employed to recover scandium directly from the hydrolytic mother solution arising from TiO2 production via the sulphate process. The parameters studied were scandium loading capacity, phase ratio, concentrations of Ti(IV) scrubbing and Sc(III) stripping agents. A new solvent extraction technology of scandium recovery was developed. The purity of the final Sc(III) product is above 95% with a yield > 94%. (C) 1998 Elsevier Science B.V.

Extraction and separation of heavy rare earth (III) with Extraction Resin containing di(2,4,4-trimethyl pentyl) phosphinic acid (Cyanex 272)

Extraction resins, of the type of;levextrel, (which is a collective term for styrene/divinylbenzene based copolymers of predominantly macroporous structure that contain a selective extractant) are important for the recovery and separation of metal ions, as they combine features of solvent extraction and ion exchange resins. This paper presents the results of the adsorption of heavy rare earth ions (Ho(III), Er(III), Tm(III), Yb(III), Lu(III) and Y(III)) from hydrochloric acid solutions at 0.2 mol/L ionic strength and 50 degrees C by the extraction resin containing di (2,4,4-trimethyl pentyl) phosphinic acid (Cyanex 272) and the chromatographic separation of (Er(III), Tm(III) and Yb(III)). Technological separation products, with purity and yield of Tm2O3 >99.97%, >80%, Er2O3 >99.9%, >94% and Yb2O3 >99.8%, >80% respectively, have been obtained from a feed having the composition Tm2O3 60%, Er2O3 10%, and Yb2O3 3%, the others 27%. The distribution coefficients, extraction equilibrium constants and separation factors have been determined as a function of acidity, loading of the resin and rare earths, flow rates and column ratios. The resolutions and efficiencies of separation of Er/Tm/Yb each other have been calculated. The stoichiometry of the extraction of rare earth ions has been suggested as well.

Studies on extraction and mass transfer of samarium and neodymium in hollow fiber membrane (HFM) with HEH/EHP

The membranes of polyvinylidene fluoride, which were synthesized by our laboratory, were used to study the transfer and extraction performances of Nd(III) and Sm(III) with the extraction system of HEH/EHP-kerosene. The results show that the membrane material was suitable to the study on membrane extraction, and could offer a good transfer performance in the membrane construction parameters selected, The extraction reaction in the membrane module was the same as that in liquid-liquid process, HEH/EHP ammoniated for increasing the mass transfer coefficient was almost the same with increasing the concentration of HEH/EHP, and H+ was still transferred first at higher pH range of feed solution when HEH/EHP was ammoniated, The controlling model of the membrane extraction process was the diffusion model accompanied by interfacial reaction, The controlling function of interfacial reaction would increase gradually with the increasing of the membrane pore size. The mass transfer coefficient increased when extraction and stripping were carried out simultaneously.

Synthesis, extraction and electronic structure of Ce@C-2n

In view of the growing interest in endohedral lanthanide fullerenes, Ce, as a typical +4 oxidation state lanthanide element, has been systematically studied. The synthesis, extraction and electronic structure of Ce@C-2n are investigated. Soot containing Ce@C-2n was synthesized in high yield by carbonizing CeO2-containing graphite rods and are back-burning the CeC2-enriched cathode deposit in a DC are plasma apparatus. Ce@C-2n, dominated by Ce@C-82, can be efficiently extracted from the insoluble part of the soot after toluene Soxhlet extraction by pyridine at high temperature and high pressure in a closed vessel. About 60% Ce@C-2n (2n = 82,80,78,76) and 35% Ce@C-82 can be enriched in the pyridine extract. This fact is identified by desorption electron impact mass spectrometry (DEI MS). The electronic structure of Ce@C-2n is analyzed by using X-ray photoemission spectroscopy (XPS) of pyridine-free film. It is suggested that the encapsulated Ce atom is in a charge state close to +3 and was effectively protected from reaction with water and oxygen by the enclosing fullerene cage. Unlike theoretical expectation, the electronic state of Ce@C-82 is formally described as Ce+3@C-82(3-). (C) 1997 Elsevier Science Ltd.

Studies on synergistic extraction of Sc(III) with HBTMPTP and Cyanex 925

The synergistic extraction of Sc(III) from H2SO4 solution with bis(2, 4, 4-trimethylpentyl)monothiophosphinic acid(HBTMPTP, HL) and branched chain alkyl phosphine oxide mixture (Cyanex 925, B) in n-hexane has been investigated, The results indicated that synergistic effect was showed in low acidity (c(H2SO4) < 0.25 mol/L). The composition of the extracted complex of Sc(III) has been determined to be Sc(HL2)(2)B-3(SO4)(1/2) by the method of slope analysis, The mechanism of the synergistic extraction of Sc(III) may be : Sc3+ + 2(HL)(2(O)) + 3B((O)) + 1/2SO(4)(2-)reversible arrow(K12)Sc(HL2)(2)B-3(SO4)(1/2(O)) + 2H(+) ScL(HL2)(2(O)) + 3B((O)) + H+ + 1/2SO(4)(2-)reversible arrow(beta')Sc(HL2)(2)B-3(SO4)(1/2(O)) + 1/2(HL)(2(O)) Sc(SO4)(1.5)B-2(O) + B-(O) + 2(HL)(2(O))reversible arrow(beta')Sc(HL2)(2)B-3(SO4)(1/2(O)) + 2H(+) + SO42- Their equilibrium constants have been calculated to be lgK(13)=6.77+/-0.12, lg beta'=7.71, lg beta '' = 0.10, respectively, The IR spectra and FAB-MS of the saturated synergistic extraction complex of Sc(III) have been discussed as well.

High-yield extraction of endohedral rare-earth fullerenes

The technique of high-temperature high-pressure extraction with pyridine has been successfully utilized to extract a wide variety of endohedral rare-earth fullerenes of the type Ln@C-2n (Ln = La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb). Ln@C-80, Ln@C-82, and Ln(2)@C-80 for most of the rare-earth metals can be produced with high-yield and selectively extracted from the carbon-are evaporation soot. Metallofullerenes containing Sm, Eu, and Yb (which could have +2 oxidation states) are especially difficult to extract. Some possible reasons for the high-yield extraction are discussed. The laser desorption mass spectrometric characterization results indicate a relationship between the extraction yields of metallofullerenes and the oxidation states and ionic radii of the rare-earths.

Studies on synergistic extraction of rare earths(III) with HBTMPTP and primary amine N1923

The synergistic extraction of rare earths(III) with binary systems containing HBTMPTP and primary amine N1923 from sulfuric acid medium was observed, The syner gistic extraction factor(R) decreased with increasing atomic number of lanthanides. Through the methods of slope analysis, constant mole and saturation titration, the synergistic extraction stoichiometry was obtained, The thermodynamic function was calculated, The IR spectra of the saturated synergistic extraction completely confirmed the mechanism.

High-yield synthesis and extraction of endohedral metallofullerenes Dy@C-2n

The successful encapsulation of dysprosium(Dy) into fullerene cages by activating the Dy2O3 containing graphite rods in situ, ''back-burning'' carbon-arc evaporation with a high-yield of pyridine extraction technique is reported.