Activation analysis of rare earths : Separation of rare earths from accompanying elements

A scheme for the separation of rare-earth elements from gadolinite and tantalocolumbite minerals is discussed. The possibility of interference from traces of nonseparated elements in the subsequent separation of rare-earth elements from each other by cation exchange with α-hydroxyisobutyrate as the eluting agent is investigated.     

Activation analysis of rare earths : The determination of rare earths in minerals by the single comparator technique

The determination of rare earths in minerals by activation analysis is described. The rare earths are separated as a group from the bulk of the material before irradiation. After irradiation the rare earths are separated from each other by gradient elution with ammonium α-hydroxyisobutyrate on a cation-exchange column. The elements are determined by the single comparator technique. This method permits a practical application of activation analysis to the routine determination of rare earths in complex matrices,     

Determination of yttrium in rare earths by photon activation analysis

The determination of yttrium in the presence of large amounts of the rare earths by the thermal neutron reaction (89)Y(n, gamma)(90)Y is complicated because of frequent problems of sample self-shielding from major constituents of the sample, and the difficulty of separating (90)Y, a pure beta-emitter, from other elements which are very similar chemically. A non-destructive photon activation analysis method has been developed for this determination. Bremsstrahlung from a 35-muA beam of 35-MeV electrons induces the photonuclear reaction (89)Y(gamma, n)(88)Y. Optimum sensitivity is obtained by coincidence counting of the 0.90 and 1.84 MeV gamma-rays associated with the decay of (88)Y. The detection limit is less than 1 mug of yttrium.     

Substoichiometric determination of heavy rare earths by isotopic dilution analysis

A substoichiometric method for the determination of heavy rare earths (holmium, thulium) has been developed. After the addition of a substoichiometric amount of EDTA to the test sample of rare earth labelled with its radioactive isotopes, the negatively charged complex formed was separated by passage through a column of Dowex 50 x 8. Interfering metals can be removed by preliminary cupferron and diethylammonium diethyldithiocarbamate extraction. Concentrations of rare earth down to 4 x 10(-7)g 5 ml have been determined.     

Neutron activation analysis of heavy rare earths

A method of nondestructive activation analysis of heavy rare earth elements (Sm−Lu) is described. Intensities of γ-ray peaks are compared to that of an internal reference after irradiations by both thermal and fission spectrum neutrons. Results are obtained from computer comparisons of peak areas. Work was performed at the Ames Laboratory of the U.S. Atomic Energy Commission. Contribution No. 2895.     

Determination of rare earths in rare-earth concentrates by neutron activation analysis

Neutron activation analysis was applied to the determination of La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Yb, Lu and Th in rare-earth concentrates resulting from minerals. High-resolution gamma-ray spectrometry with a Ge(Li) detector was used for the non-destructive determination, and a single comparator method using Co as flux monitor was applied.     

Determination of rare earths in geological samples by neutron activation analysis

The significance of rare earth distribution patterns in trace element geochemistry is briefly reviewed. Established methods for their determination at the Reactor Centre by instrumental and radiochemical techniques are described, and examples of recent applications discussed.     

Analysis of low levels of rare earths by radiochemical neutron activation analysis

A procedure for the radiochemical neutron-activation analysis for the rare earth elements (REE) involves the separation of the REE as a group by rapid ion-exchange methods and determination of yields by reactivation or by energy dispersive X-ray fluorescence (EDXRF) spectrometry. The U. S. Geological Survey (USGS) standard rocks, BCR-1 and AGV-1, were analyzed to determine the precision and accuracy of the method. We found that the precision was ±5–10% on the basis of replicate analysis and that, in general the accuracy was within ±5% of accepted values for most REE. Data for USGS standard rocks BIR-1 (Icelandic basalt) and DNC-1 (North Carolina diabase) are also presented.     

241Am-XRF analysis of rare earths in geological samples

Rare earths in sediments are analyzed by X-ray fluorescence using²⁴¹Am as an excitation source. The analytical sensitivity lies in the ppm range.     

Separation of rare earths by an ion-exchange method

Establishment of a generalized method of separating and analyzing trace impurities of high-purity rare earth oxides was attempted by neutron irradiation. The amount of the target materials and the size of the ion-exchange columns used for the analysis were made uniform. The element with atomic number lower by one was added to the irradiated target solution, prior to the cation-exchange separation, in an amount comparable to that of the carrier. α-Hydroxyisobutyrate solutions of various concentrations were used as eluent, the pH value always being kept constant at 3. 77. By this method, impurities of Gd, Dy, Ho and Er in Tb₄O₇, Dy, Er and Yb in Ho₂O₃, and Sc, Eu, Tb and Tm in Yb₂O₃ were determined.     

Electrodeposition studies of rare earths

The combination of neutron activation analysis (NAA) and electrochemistry has been used to study the deposition behavior of rare earth elements, as it is reported that excepting La, no other rare earths are electrodeposited. The radiotracers of rare earth elements were electrolyzed in an aqueous medium on a graphite electrode by varying the voltage and time of electrodeposition, thereby optimizing the final experimental conditions for quantitative deposition of rare earth elements. The observations are reported in this work.     

Determination of traces of rare earths in high-purity thorium dioxide by neutron activation analysis

The use of thorium dioxide as a nuclear fuel requires the determination of individual rare earth impurities at 0.08–1 mg kg^?1 levels. Neutron activation is sufficiently sensitive but separation from the matrix is essential. In the proposed method, thorium dioxide (5–20 g) is dissolved in concentrated nitric acid with a little hydrofluoric acid; after evaporation, thorium is complexed with ammonium carbonate and the solution is passed through a small column of Chelex-100 resin which retains the rare earths quantitatively without retaining thorium. The rare earth elements are eluted with dilute nitric acid, concentrated, and irradiated with standards; after irradiation the rare earth are collected on a lanthanum carrier and measured by γ-ray spectrometry. The recoveries of rare earths were checked with tracers and by standard addition to thorium dioxide matrices. The reproducibility for La, Eu and Dy was satisfactory at 0.01, 0.003 and 0.002 mg kg^?1, respectively; as was the reproducibility for all rare earths added to thorium dioxide (1–4 μg/5 g). Limits of detection are adequate for certification of nuclear-grade material.     

Separation of rare earths by reverse phase partition chromatography

Journal of Radioanalytical and Nuclear Chemistry - Individual separation of rare earth isotopes from lanthanum to lutetium has been carried out using reverse phase partition chromatography and...     

Determination of rare earths and thorium in apatites by thermal and epithermal neutron-activation analysis

A procedure is described for the non-destructive determination of Na, Mn, La, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Yb, Lu and Th in apatites by thermal and epithermal neutron-activation of independent portions of the material. The method was applied to three apatites with different contents. The precision obtained was better than +/-5% for La, Ce, Sm, Eu, Gd, Tb and Dy and +/-20% for Yb, Nd, Ho, Er and Lu for an apatite with a total rare-earth oxide content of the order of 1%. Determination of Ce, Tb and Yb could only be carried out with thermal neutron-activation analysis, while Gd, Ho and Er could only be determined after irradiation with epithermal neutrons.     

Interference by neutron induced second order nuclear reaction in activation analysis of rare earths

In determining the trace impurities existing in high-purity rare earth samples by the neutron activation analysis, there are much interference due to nuclides induced from neutron induced second order nuclear reaction. This paper presents the degree of interference calculated over the ranges of irradiation time from 10⁵ to 10⁷ sec and of thermal-neutron flux from 1·10¹² to 1·10¹⁵ n·cm⁻²·sec⁻¹. According to the results of these calculations, degree of interference under the neutron irradiation condition for 288 hrs in the thermal-neutron flux of 3·10¹³n·cm⁻²·sec⁻¹ is concluded to be 6.4·10⁶ ppm Gd in Eu, 2.2·10⁴ ppm Sm in Eu, 1.9·10⁴ ppm Ho in Dy, 1.1·10³ ppm Eu in Sm, 1.1·10² ppm Ce in La and 1.1·10 ppm Tb in Gd, respectively. Especially, the Gd determination in the Eu target is extremely affected by¹⁵³Gd formed from the¹⁵¹Eu (n, γ) reaction. On the contrary, this reaction is effective in producing¹⁵³Gd activity.     

Separation of thorium from rare earths

Summary A method for separation of thorium from rare earths in monazite based on the difference of stability of EDTA complexes towards oxine is described.