The fluorimetric determination of cerium and terbium

1989 ◽  
Vol 54 (3) ◽  
pp. 616-621 ◽  
Author(s):  
Záviš Holzbecher

It has been found that phosphoric acid decreases the first excitation maximum of Ce(III) at 256 nm, increases the second excitation maximum at 297 nm and shifts the fluorescence maximum from 350 to 346 nm. Under optimum conditions, with λexc = 297 nm and λem = 346 nm, Ce(III) can be determined fluorimetrically with a detection limit of 1.2 ng ml-1 in 12M-H3PO4 medium. No interference was observed from a 20-200 fold excess of HCl, H2SO4, Na, K, NH4+, Al and the rare earth elements. HNO3 interferes and Ce(IV) and Fe(III) interfere strongly. It follows from the stereofluorograms of Ce and Tb that the spectra of the two elements are practically independent. The detection limit for Tb(III) in 0.02-2.5M-H2SO4 medium for λexc = 222 nm and λem = 494 nm is 33 ng ml-1. No interference was observed from a 5-20 fold excess of Al3+ and the other rare earth elements. The determination is slightly less sensitive in H3PO4 or HCl medium. The relative standard deviation of the measurement for 10 ng ml-1 Ce(III) or 50 ng ml-1 Tb(III) is about 3%.

2021 ◽  
Vol 17 (1) ◽  
pp. 96-102
Author(s):  
Олександр Пономаренко ◽  
Анатолій Самчук ◽  
Катерина Вовк ◽  
Ольга Заяць ◽  
Ірина Кураєва

Introduction. To date, rare earth elements (REE) are used to manufacture most high-tech goods and are crucial in defense technologies (lasers, radars, and electromagnetic weapons), nuclear engineering, metallurgy, and others. All this determines the relevance of their study to assess the rare earth mineral resource base of Ukraine. Problem Statement. The determination of REE in rocks and minerals is a fundamental problem in geochemistry and petrology for understanding the processes of rock formation. However, it is a complex analytical task related to the similar chemical properties of these elements, which are caused by the "lanthanide compression effect". Purpose. The purpose is to develop analytical technologies for determining REE content by the ICP-MS method, to evaluate their content and distribution in granitoids of the Ukrainian Shield. Materials and Methods. The hybrid method of ICP-MS analysis and microwave decomposition of rocks and minerals has been used to measure the REE content. This technique has been tested and used to estimate the content and distribution of REE in fluorites and rare-metal granitoids of the Rusko-Polyanskyi massif of the Korsun-Novomirgorod pluton of the Ukrainian Shield. Results. Analytical technologies for determination of REE in granites and minerals have been developed. The method for determining REE in fluorites and granites without their prior concentration in the range from 0.01 to 1000 ppm with a relative standard deviation of 0.01–0.10 has been described. The content of rare earth elements in the Rusko-Polianskyi granites increases (218–797 g/t), the main concentrator of these elements is fluorite (692–26933 g/t REE). An inverse relationship has been observed between the REE content in fluorites and granites. Conclusions. The developed analytical technologies are the basis for establishing quality assessment criteria and developing principles for the rational use of rare-earth granitoids to create a rare-earth mineral resource base in Ukraine.


2019 ◽  
Author(s):  
Chem Int

A method is described for the inductively coupled plasma optical emission spectrometric (ICP-OES) determination of rare earth elements (REE), yttrium (Y), thorium (Th) and phosphorus (P) in monazite samples. Sample preparation was carried out by fuming with sulphuric acid followed by fluoride fusion of the remaining residue. The method was validated using the single laboratory approach by assessment of analytical performance characteristics like specificity, linearity, range, accuracy and precision. Spectral interferences were observed in the case of some heavy REE (Ho,Er,Tm) by light REE (Nd) and correction factors were deduced and applied. The limit of quantification, instrument linearity and the method range were evaluated. Relative standard deviation (RSD) values ranging from 2.6 to 10.2 % were obtained for repeatability studies and RSD values ranging from 1.7 to 11.1% for intra-lab reproducibility studies. Accuracy was established by application to a monazite certified reference material (CRM) and also through comparison of results obtained by present method with those obtained by an alternate method. The validation results were compliant with the acceptance criteria for the various parameters assessed. A simple procedure has been described for the estimation of associated measurement uncertainty using the GUM “bottom-up” modelling approach and results presented in this paper. The validated method was applied to the determination of REE, Y, Th and P in some monazite samples from India.


2021 ◽  
Vol 14 (4) ◽  
pp. 515-526
Author(s):  
Anna A. Kravchenko ◽  
◽  
Irina V. Nikolaeva ◽  
Stanislav V. Palesskiy

Method of microwave digestion using HNO3, HCl and HF in MARS‑5 system followed by ICP-MS analysis is proposed for determination of rare earth elements (REE) in plant materials. Limits of detection are 0.0001–0.001 ppm and allow for determination of all REE in certified reference materials Tr‑1, LB‑1 and EK‑1 and new reference material NSP‑1, relative standard deviations are lower than 13 %.Influence of HF addition during microwave digestion in UltraWAVE system on the ICP-MS analysis of REE in plant materials depending on silica content is studied. Necessity of HF addition during microwave digestion for better REE recoveries is shown for plant materials with Si contents exceeding 0.1 %


Environments ◽  
2018 ◽  
Vol 5 (10) ◽  
pp. 112 ◽  
Author(s):  
Martin Makombe ◽  
Charlton van der Horst ◽  
Bongiwe Silwana ◽  
Emmanuel Iwuoha ◽  
Vernon Somerset

The increasing demand for rare earth elements in green technology, electronic components, petroleum refining, and agricultural activities has resulted in their scattering and accumulation in the environment. This study determined cerium, lanthanum and praseodymium in environmental water samples with the help of adsorptive differential pulse stripping voltammetry (AdDPSV) and inductive coupled plasma-optical emission spectroscopy (ICP-OES). A comparison of the results of these two analytical techniques was also made. The accuracy and precision of the methods were evaluated by spiking water samples with a known amount of REEs. The detection limit obtained for the stripping analysis was 0.10 μg/L for Ce(III), and 2.10 μg/L for combined La(III) and Pr(III). The spectroscopic method of determination by ICP-OES was applied to the same samples to evaluate the effectiveness of the voltammetry procedure. The ICP-OES detection limit obtained was 2.45, 3.12 and 3.90 μg/L for Ce(III), La(III) and Pr(III), respectively. The results obtained from the two techniques showed low detection limits in voltammetry; the ICP-OES method achieved better simultaneous analysis. This sensor has been successfully applied for the determination of cerium, lanthanum, and praseodymium in environmental water samples, offering good results.


1966 ◽  
Vol 20 (4) ◽  
pp. 236-240 ◽  
Author(s):  
B. Strzyzewska ◽  
Z. Radwan ◽  
J. Minczewski

A carrier distillation method has been applied for quantitative determination of trace amounts of rare earths in hydrochloric acid solution evaporated on graphite matrix. The method can be applied to the analysis of all rare earth elements. The detection limit obtained for individual elements was from 0.02 to 0.16 μg per sample (except for Yb it was 0.0008 μg per sample). The deviations of the position of the analytical curves for the individual rare earth elements have been investigated as they are affected by addition of all other rare earth elements in concentrations at the upper limit of the procedure. It was established that the influence of additional elements is different for the various elements and for the different lines of the same element. The interpolation error for maximal difference in composition between the sample and spectrographic standards has been calculated.


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