Small Angle X-ray Scattering Studies of Polymeric Zirconium Species in Aqueous Solution

ABSTRACTSmall angle X-ray scattering techniques have been used to investigate the shape and size distribution of Zr(IV) species in aqueous solution. This study has shown that when zirconyl chloride solutions, containing the zirconyl tetramer, are subjected to various treatments polymerisation occurs. While ageing and addition of base produces an increase in particle size the shape remains globular. Refluxing the solutions produces “rod” like particles of varying length but constant cross sectional radius.

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Synthesis and Advanced Characterization of Polymer-Protein Core-Shell Nanoparticles

Catalysts ◽

10.3390/catal11060730 ◽

2021 ◽

Vol 11 (6) ◽

pp. 730

Author(s):

Erik Sarnello ◽

Tao Li

Keyword(s):

Particle Size ◽

Small Angle ◽

Core Shell ◽

Assembly Process ◽

Shell Nanoparticles ◽

X Ray ◽

X Ray Scattering ◽

Wide Range ◽

Core Shell Nanoparticles ◽

Ray Scattering

Enzyme immobilization techniques are widely researched due to their wide range of applications. Polymer–protein core–shell nanoparticles (CSNPs) have emerged as a promising technique for enzyme/protein immobilization via a self-assembly process. Based on the desired application, different sizes and distribution of the polymer–protein CSNPs may be required. This work systematically studies the assembly process of poly(4-vinyl pyridine) and bovine serum albumin CSNPs. Average particle size was controlled by varying the concentrations of each reagent. Particle size and size distributions were monitored by dynamic light scattering, ultra-small-angle X-ray scattering, small-angle X-ray scattering and transmission electron microscopy. Results showed a wide range of CSNPs could be assembled ranging from an average radius as small as 52.3 nm, to particles above 1 µm by adjusting reagent concentrations. In situ X-ray scattering techniques monitored particle assembly as a function of time showing the initial particle growth followed by a decrease in particle size as they reach equilibrium. The results outline a general strategy that can be applied to other CSNP systems to better control particle size and distribution for various applications.

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A Small-Angle X-Ray Scattering Study on Pre-Irradiated Malate Synthase. The Influence of Formate, Superoxide Dismutase, and Catalase on the X-Ray Induced Aggregation of the Enzyme

Zeitschrift für Naturforschung C ◽

10.1515/znc-1985-5-614 ◽

1985 ◽

Vol 40 (5-6) ◽

pp. 364-372 ◽

Cited By ~ 7

Author(s):

P. Zipper ◽

R. Wilfing ◽

M. Kriechbaum ◽

H. Durchschlag

Keyword(s):

Aqueous Solution ◽

Superoxide Dismutase ◽

Small Angle ◽

Malate Synthase ◽

X Ray ◽

X Ray Scattering ◽

X Irradiation ◽

The Mean ◽

Induced Aggregation ◽

Ray Scattering

Abstract The sulfhydryl enzyme malate synthase from baker’s yeast was X-irradiated with 6 kGy in air-saturated aqueous solution (enzyme concentration: ≃ 10 mg/ml; volume: 120 μl), in the absence or presence of the specific scavengers formate, superoxide dismutase, and catalase. After X-irradiation, a small aliquot of the irradiated solutions was tested for enzymic activity while the main portion was investigated by means of small-angle X-ray scattering. Additionally, an unirradiated sample without additives was investigated as a reference. Experiments yielded the following results: 1. X-irradiation in the absence of the mentioned scavengers caused considerable aggregation, fragmentation, and inactivation of the enzyme. The dose Dt37 for total (= repairable + non-repayable) inactivation resulted as 4.4 kGy. The mean radius of gyration was found to be about 13 nm. The mean degree of aggregation was obtained as 5.7, without correction for fragmentation. An estimation based on the thickness factor revealed that about 19% of material might be strongly fragmented. When this amount of fragments was accordingly taken into account, a value of 7.1 was obtained as an upper limit for the mean degree of aggregation. The observed retention of the thickness factor and the finding of two different cross-section factors are in full accord with the two-dimensional aggregation model established previously (Zipper and Durchschlag, Radiat. Environ. Biophys. 18, 99 - 121 (1980)). 2. The presence of catalytic amounts of superoxide dismutase and/or catalase, in the absence of formate, during X-irradiation reduced both aggregation and inactivation significantly. 3. The presence of formate (10 or 100 mᴍ) during X-irradiation led to a strong decrease of aggregation and inactivation. This effect was more pronounced with the higher formate concentration or when superoxide dismutase and/or catalase were simultaneously present during X-irradiation. The presence of formate also reduced the amount of fragments significantly. 4. The results clearly show that the aggregation and inactivation of malate synthase upon X-irradiation in aqueous solution are mainly caused by OH·; to a minor extent O·̄2 and H2O2 are additionally involved in the damaging processes.

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