A test for the reliability of the controlled potential coulometric method to determine plutonium in uranium-plutonium mixtures

1976 ◽  
Vol 279 (1) ◽  
pp. 29-32 ◽  
Author(s):  
Y. Duigou ◽  
W. Leidert

1959 ◽  
Vol 31 (1) ◽  
pp. 10-16 ◽  
Author(s):  
G. L. Booman ◽  
W. B. Holbrook




2020 ◽  
Vol 86 (12) ◽  
pp. 15-22
Author(s):  
N. A. Bulayev ◽  
E. V. Chukhlantseva ◽  
O. V. Starovoytova ◽  
A. A. Tarasenko

The content of uranium and plutonium is the main characteristic of mixed uranium-plutonium oxide fuel, which is strictly controlled and has a very narrow range of the permissible values. We focused on developing a technique for measuring mass fractions of uranium and plutonium by controlled potential coulometry using a coulometric unit UPK-19 in set with a R-40Kh potentiostat-galvanostat. Under conditions of sealed enclosures, a special design of the support stand which minimized the effect of fluctuations in ambient conditions on the signal stability was developed. Optimal conditions for coulometric determination of plutonium and uranium mass fractions were specified. The sulfuric acid solution with a molar concentration of 0.5 mol/dm3 was used as a medium. Lead ions were introduced into the background electrolyte to decrease the minimum voltage of hydrogen reduction to –190 mV. The addition of aluminum nitride reduced the effect of fluoride ions participating as a catalyst in dissolving MOX fuel samples, and the interfering effect of nitrite ions was eliminated by introducing a sulfamic acid solution into the cell. The total content of uranium and plutonium was determined by evaluation of the amount of electricity consumed at the stage of uranium and plutonium co-oxidation. Plutonium content was measured at the potentials, at which uranium remains in the stable state, which makes it possible to subtract the contribution of plutonium oxidation current from the total oxidation current. The error characteristics of the developed measurement technique were evaluated using the standard sample method and the real MOX fuel pellets. The error limits match the requirements set out in the specifications for MOX fuel. The technique for measuring mass fractions of uranium and plutonium in uranium-plutonium oxide nuclear fuel was certified. The relative measurement error of the mass fraction of plutonium and uranium was ±0.0070 and ±0.0095, respectively. The relative error of the ratio of the plutonium mass fraction to the sum of mass fractions of uranium and plutonium was ±0.0085.



2018 ◽  
Vol 68 (12) ◽  
pp. 2799-2803
Author(s):  
Maria Daniela Pop ◽  
Oana Brincoveanu ◽  
Mihaela Cristea ◽  
George Octavian Buica ◽  
Marius Enachescu ◽  
...  

Preparation and microscopy characterization of polymer modified glassy carbon electrodes based on (5-[(azulen-1-yl) methylene]-2-thioxothiazolidin-4-one (L) were reported. Atomic Force Microscopy was used to investigate the morphological and mechanical properties of the deposited polyL films onto glassy carbon. The topography images of the analyzed samples exhibited the presence of some columnar shape features onto the layer surfaces. The surface roughness of the layers deposited at constant charge calculated from topography images, increased with the more positive applied potential for controlled potential electrolysis. At different charges, the roughness parameter showed the same behavior for the layers obtained applying a constant potential without having a noticeable influence on the adhesion properties on the substrate. Analysis using scanning electron microscopy shows a relatively uniform surface arrangement of the polymer and the presence of some clusters which are disturbing the planarity. PolyL chemically modified electrodes have been used for heavy metal ions detection with best results for lead.



1985 ◽  
Vol 50 (1) ◽  
pp. 33-41 ◽  
Author(s):  
Jaromír Hlavatý

The o-nitrobenzyl thiocyanate (I) behaves differently on the DME and on a large mercury pool electrode. Polarography did not give a sufficiently clear explanation of the reaction mechanism, only the preparative experiments yielded useful results. Whereas polarographic curves in solutions of Britton-Robinson buffer system with 50% by vol. ethanol exhibit two cathodic waves within the pH region 1-12, corresponding according to their height ratio to an uptake of 4 e and 2 e respectively, the controlled potential preparation electrolysis (CPE) and coulometry results indicate a more complicated reaction path. In the CPE carried out at the concentration of I 1 . 10 -2 mol/l the electroreductive splitting of CH2-SCN occurs as the first step. Nitrobenzyl radicals so formed react in the follow-up dimerization resulting in dibenzyl or toluene structures. Simultaneously or at a later stage the completion of the electrolytic reduction of the nitro group proceeds to the hydroxylamino group. In solution of 9 > pH > 1 the CPE of nitro compound I takes place by an ECEC mechanism yielding dibenzodiazocine III, its N-oxide IV and 2,2'-dimethylazoxybenzene (V). In course of preparative electrolysis in strongly acidic medium 2-amino-benzo(l,3)-thiazine-l-oxide (II) is formed by an EC mechanism.



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