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Abstract  

This work deals with the extraction behavior of neptunium in a high acid Purex Process. The composition of PWR fuel type with 3.2% enrichment, 500 MWd/t burn-up and 100 d cooling time was considered. Two consecutive cold runs were performed in a mock-up facility at IPEN-CNEN/SP with simulated feed solutions containing: 3M HNO3; 1M U; 455 g237Np labeled with239Np; 15 mg Zr l–1, 12 mg Ce l–1, 7 mg Ru l–1 and 13 mg Mo l–1 traced with active isotopes95Zr,141Ce,103Ru and99Mo as FP. A 30 vol% TBP/n-dodecane was used as solvent. Countercurrent experiments were carried out using two 16 stages plexiglass mixer-settlers, at 25°C, during 21 h continuous operation, with O/A ratio of 2 in the extraction section and 9 and 13 in the 1st and 2nd scrubbing sections, respectively. For a 65% organic loading, ca. 77% of neptunium remains in the waste stream, without any Np valence adjustment.

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Abstract  

A study of Pu recovery at trace level from U solutions by ion exchange technique is presented. Plutonium retention >99.5% onto strong anionic resin, AG-X8, from nitric acid solutions and a 92% recovery using 0.4M HNO3 at 60°C as eluent, were obtained. Uranium interference in Pu sorption from mixed U/Pu nitrate solutions with low U/Pu ratio (25) was not verified. However, for high U/Pu ratio solutions (10000), uranium interference in Pu retention on the resin, decreases to 59%. Selecting the loading conditions and using AG-X4 resin, 99% Pu retention was achieved. The Pu product is still contaminated with U and another purification cycle is recomended. A scheme for U/Pu first cycle separation is proposed.

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Abstract  

In the actinide separation process using TBP as extractant, hydrolytic and radiolytic reactions cause a gradual decomposition of the extractant, resulting in the formation of degradation products which can affect process performance adversely. The TBP diluent has to be cleaned from these degradation products before it is reused. This paper deals with a procedure for solvent cleanup, using a fourstage continuous contactor for increasing the scrubbing efficiency.

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Abstract  

Celeste-1 is a lab-scale hot cell intended for R&D work in reprocessing of low burn-up spent fuel elements. The studies are concerned with head-end, first separation cycle by Purex Process using mini mixer-settlers and development of analytical techniques. The analytical monitoring for process control purposes is based on several off-line techniques, such as X-ray fluorescence spectrometry, potentiometric titration, -and -spectroscopy, spectrophotometry, fluorimetry, density measurement and gas chromatography. The analytical treatment takes place in a shielded working place analytical hot cell, glove boxes and hoods and some final measurements are made in the associated analytical laboratory. A pneumatic system is used for transporting analytical samples. All analytical procedures are ready and in operation.

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Abstract  

The use of an electrochemical process for U/Pu partitioning has demonstrated a good performance and is a safe alternative for nuclear facilities. Its great advantages are the lack of introduction of foreign ions into the process and, especially, the minimization of the waste volume generated. For the introduction of electrochemical U/Pu partitioning in the 2nd Pu purification cycle, preliminary studies were carried out with a single mixer-settler unit. Based on the results, an 8-stage electrolytic mixer-settler (M-S MIRELE) was designed. Titanium was MIRELE's housing material (cathode) and platinum the anode, insulated with PTFE. The Pu recovery was higher than 99%, indicating the efficiency of this equipment.

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Abstract

The synthesis of pigments from the system Ce1−x O2–M x O (M = Cu, Co) was achieved via a polymeric precursors method, Pechini method. Differential scanning calorimetry (DSC) and thermogravimetry (TG) techniques were used to accurately characterize the distinct thermal events occurring during synthesis. The TG and DSC results revealed a series of decomposition temperatures due to different exothermal events, which were identified as H2O elimination, organic compounds degradation, and phase formation. X-Ray diffraction patterns show the presence of pure cubic CeO2 phase for the samples with low Cu and Co loading. A decrease of the specific surface area with increasing copper and cobalt content was observed. The UV–visible diffuse reflectance technique was employed to study the optical properties in the 200–800 nm range. Colorimetric coordinates L*, a*, b* were calculated for the pigment powders. The powders presented a variety of colors from yellow for pure CeO2, to brown for the ones loaded with copper and gray for the ones with cobalt.

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Journal of Thermal Analysis and Calorimetry
Authors:
Ana C. R. Melo
,
Edjane F. B. Silva
,
Larissa C. L. F. Araujo
,
Mirna F. Farias
, and
Antonio S. Araujo

Abstract

In this study, were studied the degradation of pure sunflower oil and mixed with H-Beta zeolite. This zeolite was synthesized by the hydrothermal method, followed by calcination and ion exchanged. The characterization of the zeolite was performed by X-ray diffraction and nitrogen adsorption/desorption by the method of BET. The analysis showed that H-Beta zeolite presented a good crystallinity and the template was completely removed from the catalyst. The thermal and catalytic degradation study was carried out using the TG/DTG method in multiple heating rates of 5, 10, and 20 °C min−1. The isoconversion method proposed by Vyazovkin was applied to determine the kinetic parameters for degradation of the sunflower oil. The activation energy for the degradation process of pure sunflower oil was 193 kJ mol−1, while for sunflower oil mixed with 20% of H-Beta zeolite was equivalent to 88 kJ mol−1. It was verified that for the degradation of 90% of the sunflower oil mixed with H-Beta, for a period of 1 h, a temperature of 356 °C was required, whereas for the pure vegetable oil, this value was of 387 °C, at the same time period, showing that the catalyst was effective for the degradation process of sunflower oil.

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Abstract

The thermo-programmed reduction study of Pt/WOx–ZrO2 materials prepared with different tungsten loading were performed by thermogravimetry. The samples were synthesized by impregnation method and calcined at 600, 700 and 800°C. The characterizations of both un-calcined and calcined materials were carried out using different techniques: thermal analysis (TG and DTA), X-ray diffraction (XRD) and thermo-programmed reduction (TPR). TG and DTA analysis of un-calcined were used to determination of calcination temperatures of the samples. XRD diffractograms were useful to help us in the determination of phase presents. TPR profiles showed between three and four events at different temperatures attributed to platinum reduction and the different stages of tungsten specie reduction.

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Abstract

Zinc oxide is a widely used white inorganic pigment. Transition metal ions are used as chromophores and originate the ceramic pigments group. In this context, ZnO particles doped with Co, Fe, and V were synthesized by the polymeric precursors method, Pechini method. Differential scanning calorimetry (DSC) and thermogravimetry (TG) techniques were used to accurately characterize the distinct thermal events occurring during synthesis. The TG and DSC results revealed a series of decomposition temperatures due to different exothermal events, which were identified as H2O elimination, organic compounds degradation and phase formation. The samples were structurally characterized by X-Ray diffractometry revealing the formation of single phase, corresponding to the crystalline matrix of ZnO. The samples were optically characterized by diffuse reflectance measurements and colorimetric coordinates L*, a*, b* were calculated for the pigment powders. The pigment powders presented a variety of colors ranging from white (ZnO), green (Zn0.97Co0.03O), yellow (Zn0.97Fe0.03O), and beige (Zn0.97V0.03O).

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