X‐Ray Tomography Imaging of Porous Polyolefin Particles in an Electron Microscope

Advanced models of penetrant transport and reaction in spatially 3D porous polyolefin particles reconstructed from X‐ray µCT images require proper determination of particle morphology. Moreover, polyolefins exhibit a relatively low absorptivity for X‐rays, therefore their investigation using µCT can be difficult. In this paper, a low‐resolution µCT built into an SEM is used to examine how the µCT resolution and several user‐selected parameters associated with the scanning/reconstruction affect the resulting particle morphology. Using samples with known morphology and independent imaging techniques, the performance of the µCT device is critically assessed. Finally, a method suitable for the reliable reconstruction of polyolefin particles using low‐resolution µCT is proposed.

     

Self-assembled sensor based on boron-doped diamond and its application in voltammetric analysis of picloram

A self-assembled sensor based on a boron-doped diamond was investigated as a sensitive tool for voltammetric analysis of a member of a pyridine herbicide family - picloram. A cyclic voltammetry and a differential pulse voltammetry were applied for investigation of the voltammetric behaviour and quantification of this herbicide. Picloram yielded one well-developed irreversible oxidation signal at a very positive potential about +1.5 V vs. Ag/AgCl/3 mol L^?1 KCl electrode in an acidic medium and 1 mol L^?1 H₂SO₄ was chosen as a suitable supporting electrolyte. Operating parameters of differential pulse voltammetry were optimized and the proposed voltammetric method provided a high repeatability (a relative standard deviation of 20 repeated measurements at a concentration level of picloram of 50 µmol L^?1 equaled to 2.58%), a linear concentration range from 2.5 to 90.9 µmol L^?1 and a low limit of detection (LD = 1.64 µmol L^?1). Practical usefulness of the ‘environmentally-green’ electrochemical sensor was verified by an analysis of spiked water samples with satisfactory recoveries.     

Structure equations and constraint manifolds on Lorentz plane

Calculating the structure equation of a chain is important to represent the position of the end link on the chain. Furthermore, the structure equation helps to determine the constraint manifold of the chain. The constraint manifold satisfies to make geometric interpretations about the form that is obtained. What is more, the constraint forced on the positions of the end link by the rest of the chain is represented by the manifold. In Lorentz space, the structure equations change according to the causal characters of the first link. In this paper, we attain the structure equations of a planar open chain in terms of the causal character of the first link in this space. Later, the constraint manifolds of the chain by using these equations are given. Some geometric comments about these manifolds are explained.     

铈基模型催化剂的纳米结构:有序CeO2(111)薄膜上的Pt-Co纳米颗粒

制备并表征了原子分散的模型体系:氧化铈负载的Pt-Co核壳催化剂.采用超高真空物理气相沉积法制备了有序CeO2(111)膜上的Pt@Co和Co@Pt核壳纳米结构,并用同步辐射光电子能谱和共振光发射光谱对其进行了研究.在低Co覆盖率(0.5 ML)下Co在CeO2(111)上沉积生成Co-CeO2(111)固溶体,然后在更高Co覆盖率下生长为金属Co纳米粒子.Pt@Co和Co@Pt两种模型结构在300-500 K温度范围内都能稳定地抗烧结.在500 K退火后, Pt@Co纳米结构含有接近纯的钴壳,而Co@Pt中的铂壳部分被金属钴覆盖.在550 K以上,在Pt@Co和Co@Pt纳米结构中近表面区域的重新排序中产生了次表层的Pt Co合金和富铂外壳.对于Co@Pt纳米粒子,近表面区域的化学有序性取决于沉积铂壳的初始厚度.无论初始铂壳的厚度如何,在有氧存在下对Co@Pt纳米结构进行退火,都会导致Pt-Co合金的分解以及Co的氧化.Co的逐步氧化与吸附质诱导的Co偏析共同导致在负载的Co@Pt纳米结构表面形成厚的Co O层.这一过程伴随着CeO2(111)薄膜的裂解,以及在550K以上氧气中退火后CeO2包裹氧化的Co@Pt纳米结构.很明显,于不同温度下在氧气和氢气的氧化-还原循环过程中,无论铂的初始厚度是多少,负载的Co@Pt纳米颗粒的结构和化学成分的变化主要是由氧化所致,而还原处理的影响则很小.     

Enhancing Magnetic Cooperativity in Fe(II) Triazole‐based Spin‐crossover Nanoparticles by Pluronic Matrix Confinement

Polymeric one‐dimensional (1D) triazole‐based Fe^II spin crossover nanoparticles have been entrapped in pluronic P123 matrix, forming nanorods in which the interaction between host (P123) and guest (Fe^II complex) promoted high reproducibility of the spin crossover process, significant shifts of the transition temperatures (T↑=370 K, T↓=338 K for the P123 entrapped material vs the literature values of T↑=358 K, T↓=341 K for the neat/polymer free system) and larger magnetic hysteresis width.     

Click synthesis of triazole-linked calix[4]arene ionophores. Potentiometric and ESI-MS screening of ion-selectivity

A series of 1,2,3-triazole-linked calix[4]arene ionophores comprised of different O-donor groups (OH, COOEt, CONEt₂) attached either to the lower rim of calix or to the triazole moieties were synthesized to explore their ion-selectivity for the first time in potentiometric transduction. Plasticized PVC membrane electrodes (ISEs) were fabricated, and their potentiometric selectivities were measured toward a series of mono- and divalent metal ions. Structure-ion-selectivity relationship and the structural requirements of the coordination sphere for selective binding were established. ISEs made of calix[4]arene-bis-triazoles were found generally to exhibit distinct Ag⁺ selectivity in the order 3 ≈ 4 > 2 > 1, indicating the beneficial effect of the carboxamide or ester groups in the complexing site. In contrast, calix[4]arene-tetratriazole 5 comprised only sp ² N-donor atoms displayed excellent Cu²⁺ selectivity over a series of alkali-, alkaline earth- and transition metal ions. A unique feature of the outstanding Ag⁺ selective electrodes made of 3 and 4 was recognized and suggested their potential application as Na⁺ ISEs in systems not containing silver ions. Further, the potential use of competitive ESI-MS experiments for screening the binding affinities of ionophores 3–6 to different metal ions was also demonstrated.     

Concentrations of 137Cs and 40K radionuclides and some heavy metals in soil samples from the eastern part of the Main Ridge of the Flysch Carpathians

The aim of the study is to present the results of determination of radioactivity of artificial ¹³⁷Cs and natural ⁴⁰K and certain heavy metals in soil samples collected from the eastern part of the Main Ridge of Carpathians, including the Beskid Niski Mts and the Bieszczady Mts. The evaluation of level of radionuclides was based on the bulk density analysis of the soil. A valuable finding of the study was a good linear correlation between the level of ¹³⁷Cs concentration and bulk density of the soil as well as an inverse correlation between radioactivity of natural ⁴⁰K and tested soil density. This might indicate though a high competitiveness of these elements between each other. Moreover, a good correlation between the concentrations of artificial element ¹³⁷Cs and Pb has been also observed in soil samples collected from the Beskid Niski Mts. In most cases, the level of artificial ¹³⁷Cs was lower comparing to an average ¹³⁷Cs concentration established for soils in Poland.     

Photocatalytic performance of silver-modified TiO2 embedded in poly(ethyl-acrylate-co-methyl metacrylate) matrix

The plasmonic Ag-TiO₂ (with 0.5 wt% Ag) photocatalyst was prepared on P25 TiO₂ surface. The presence of AgNPs on the titania was indicated by the UV–vis spectrum, which showed a plasmonic absorbance band in the visible range (λ _max?=?455 nm). XPS measurements suggested that Ag was in metallic (Ag) and in oxide forms on TiO₂. Ag-TiO₂ photocatalyst and TiO₂ were embedded in [poly(ethyl acrylate-co-methyl methacrylate; p(EA-co-MMA)] copolymer to attain mechanically stable, photocatalytically active nanocomposite films. The photooxidation of ethanol was slower on the photocatalyst/polymer nanocomposites, but it could be significantly improved by irradiating them with UV light. The photoaging was applied as a post-preparation treatment to improve the photocatalytic activity of the nanocomposite films. Changed surface morphology and the partial destruction of the polymer were supported by AFM and FTIR results. Contact angle measurements were used to determine the surface free energies of the prepared and the photoaged nanocomposite films.     

Synthesis of E- and Z-o-Methoxy-Substituted 2,3-Diphenyl Propenoic Acids and Its Methyl Esters

A series of stereoisomeric o-methoxy-substituted 2,3-diphenyl propenoic acids and their methyl esters have been synthesized. The E isomers were prepared by a modified Perkin condensation (substituted benzaldehyde, phenylacetic acid, Et₃N/acetic anhydride). The difficult to access Z isomers were obtained conveniently in good yields when the appropriate coumarin derivatives were allowed to react with KOH and CH₃I in DMSO.