Experimental study of Pd hydrolysis in aqueous solutions at 25–70°C

Koroleva, L. A.; Shikina, N. D.; Kolodina, P. G.; Зотов, А. В.; Тагиров, Б. Р.; Shvarov, Yu. V.; Volchenkova, V. A.; Shazzo, Yu. K.

doi:10.1134/s0016702912080034

Cited by 13 publications

(6 citation statements)

References 10 publications

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“…Thus, the hydrolysis of Pd complexes is a general issue in the synthesis of Pd-NPs that needs to be considered if the precursor solution cannot be used within a few seconds. This applies in particular to large-scale syntheses, seedmediated growth procedures, synthetic procedures at elevated temperatures (which accelerate the hydrolysis 44 ) and syntheses using mild reducing agents.…”

Section: Precursor Stabilization and Upscalingmentioning

confidence: 99%

Reliable palladium nanoparticle syntheses in aqueous solution: the importance of understanding precursor chemistry and growth mechanism

et al. 2015

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Reliable protocols for the synthesis of palladium nanoparticles (Pd-NPs) in aqueous solution are rarely found and the corresponding growth mechanisms often remain unknown. Furthermore, syntheses of Pd-NPs always demand the use of stabilizing agents which are often unfavorable for catalytic applications. In this contribution, the importance of the palladium precursor chemistry as a prerequisite for any reliable Pd-NP synthesis in aqueous solution is shown. This includes a detailed study of the influence of the precursor chemistry on the nanoparticle growth mechanism. The findings enable the controlled modification of a common synthetic protocol (i.e. the reduction of a palladium precursor with NaBH4) to obtain sub-5 nm Pd-NPs without the use of any stabilizing agent. In addition, it is also shown that such mechanistic studies are not only of great importance to the development of novel synthetic procedures. Exemplarily, the successful transfer of the synthesis from lab-to large-scale is demonstrated.BMBF, 03EK3009, Design hocheffizienter Elektrolysekatalysatore

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Section: Precursor Stabilization and Upscalingmentioning

confidence: 99%

Reliable palladium nanoparticle syntheses in aqueous solution: the importance of understanding precursor chemistry and growth mechanism

et al. 2015

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“…Binodal curves and tie-lines in the (1) PEG1500–Na 2 SO 4 –0.1 M HCl (red line), pH from 1.74 to 2.1 and (2) PEG1500–Na 2 SO 4 –(0.05 M H 2 SO 4 + 0.1 M NaCl) (blue line), pH from 1.84 to 2.22 in comparison (3) with published data (pH = 2).…”

Section: Resultsmentioning

confidence: 58%

“…28 To prevent hydrolysis of palladium(II), the pH should be less than 4. 29 High values of acidity and concentration of chloride ions needed for extraction will definitely affect the phase equilibria in ATPS.…”

Section: Introductionmentioning

confidence: 99%

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Effect of Sodium Chloride and pH on the Composition of the Equilibrium Phases and the Partition of Palladium(II) in the Aqueous Two-Phase System PEG1500–Na₂SO₄–Water

et al. 2021

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Binodal curves for aqueous two-phase systems (ATPS) polyethylene glycol 1500 (PEG1500)−sodium sulfate− water with additions of sodium chloride and hydrochloric or sulfuric acids were determined by turbidimetric titration and analysis of coexisting phases. The results are compared with published data for the ATPS PEG1500−sodium sulfate−water without additions, and the influence of additions on the width of the two-phase field, tielines length, and slopes was traced. The influence of initial concentration of palladium, time of phase contact, pH, concentration of sodium chloride and sodium sulfate on the extraction of palladium(II) was studied. The coefficients of distribution of palladium(II) between the phases of ATPS were measured as a function of the concentrations of sodium chloride (0.1, 1.0, and 2.0 mol•L −1 ) and pH values. At lower concentrations of Cl − ions Pd(II) is extracted as a mixture of ions [Pd(H 2 O)Cl 3 ] − and [PdCl 4 ] 2− , whereas the growth of C(Cl − ) leads to prevalence of the latter, which has poorer extraction properties. Maximal values of the distribution coefficient D Pd of about 9.5 ± 0.75 were achieved in the ATPS PEG1500−Na 2 SO 4 −0.1 M HCl and PEG1500− Na 2 SO 4 −(0.05 M H 2 SO 4 + 0.1 M NaCl).

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“…However, the presence of a higher oxidation state is very unlikely, requiring an oxidizing potential upward of 1 V . The additional species may therefore be associated with hydrolysis products of Pd in the acidic media, most probably Pd(OH) 2 . , Hydrolysis in acidic conditions has also been seen for other species that would be present in reprocessing liquors, including U and Pu, forming colloidal species at pH values as low as 0. , …”

Section: Surface Contamination Speciationmentioning

confidence: 99%

Development of a Multi-technique Characterization Portfolio for Stainless Steels Exposed to Magnox Reprocessing Liquors

Barton,

Denman,

Grebennikova

et al. 2023

ACS Omega

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AISI Type 304 stainless steel coupons have been exposed to a simulant aqueous environment representative of the Magnox Reprocessing Plant (MRP) at Sellafield, UK. The experiments were performed for extended time periods (up to 420 days) at elevated temperatures to develop a comprehensive understanding of the extent, nature, and depth of contamination for pipework and vessels in Magnox spent nuclear fuel reprocessing environments. This will inform upcoming decommissioning work which represents a major post-operational challenge. Previous relevant literature has focused on developing fundamental understanding of contamination mechanisms of stainless steels in simplistic, single-element systems, which lack elements of industrial relevance. Contamination behavior is expected to be drastically different in these more complex environments. A characterization portfolio has been developed to enable detailed assessment of corrosion and contamination behavior in acidic reprocessing environments. Solution, surface, and depth analysis determined that uptake was dominated by the elements present in highest concentrations within the environment, namely, Mg, Nd, and Cs. Most contaminants were incorporated into a relatively thin surface oxide layer (<100 nm) in metal oxide form, although there were some exceptions (Cs and Sr). Grain boundary etching was present despite very low corrosion rates (3 μm year −1 ). As a result of this lack of corrosion, diffusion of contaminants beyond the immediate surface (10− 20 nm) did not occur, evidenced through depth profiling. As a result of these findings, surface-based decontamination techniques minimizing excess secondary waste generation can be further developed in order to reduce the environmental and economic burden associated with decommissioning activities.

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Experimental study of Pd hydrolysis in aqueous solutions at 25–70°C

Cited by 13 publications

References 10 publications

Reliable palladium nanoparticle syntheses in aqueous solution: the importance of understanding precursor chemistry and growth mechanism

Reliable palladium nanoparticle syntheses in aqueous solution: the importance of understanding precursor chemistry and growth mechanism

Effect of Sodium Chloride and pH on the Composition of the Equilibrium Phases and the Partition of Palladium(II) in the Aqueous Two-Phase System PEG1500–Na₂SO₄–Water

Development of a Multi-technique Characterization Portfolio for Stainless Steels Exposed to Magnox Reprocessing Liquors

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Experimental study of Pd hydrolysis in aqueous solutions at 25–70°C

Cited by 13 publications

References 10 publications

Reliable palladium nanoparticle syntheses in aqueous solution: the importance of understanding precursor chemistry and growth mechanism

Reliable palladium nanoparticle syntheses in aqueous solution: the importance of understanding precursor chemistry and growth mechanism

Effect of Sodium Chloride and pH on the Composition of the Equilibrium Phases and the Partition of Palladium(II) in the Aqueous Two-Phase System PEG1500–Na2SO4–Water

Development of a Multi-technique Characterization Portfolio for Stainless Steels Exposed to Magnox Reprocessing Liquors

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Effect of Sodium Chloride and pH on the Composition of the Equilibrium Phases and the Partition of Palladium(II) in the Aqueous Two-Phase System PEG1500–Na₂SO₄–Water