1H-detected double-J-modulated INEPT-INADEQUATE for simultaneous determination of one-bond and long-range carbon-carbon connectivities and the measurement of all carbon-carbon coupling constants

We describe a new NMR experiment, (1)H-detected double-J-modulated (DJM)-INEPT-INADEQUATE, for tracing out the carbon skeleton of molecules. This experiment allows simultaneous correlation of directly bonded carbon atoms and those separated by multiple bonds, while at the same time also providing the values of all J(CC) coupling constants. This is achieved by replacing both fixed carbon-carbon coupling evolution intervals of the INEPT-INADEQUATE experiment by variable time intervals, which are incremented in concert with the DQ evolution period (t(1)). We show that the analysis of the fine structure of cross-peaks in DJM-INEPT-INADEQUATE spectra leads to accurate values of coupling constants and give guidelines for the proper usage of the method. The proposed experiment is two times less sensitive that the original INEPT-INADEQUATE experiment. We show that, using a 600-MHz cryoprobe and 20 mg of a monosaccharide, spectra that are suitable for the analysis of coupling constants as small as 2 Hz can be obtained within 24 h. Instead of performing multiple experiments, a single DJM-INEPT-INADEQUATE experiment can thus provide a wealth of information for the structural analysis of small molecules.     

Shifted products that are coprime pure powers

A set A of positive integers is called a coprime Diophantine powerset if the shifted product ab+1 of two different elements a and b of A is always a pure power, and the occurring pure powers are all coprime. We prove that each coprime Diophantine powerset A⊂{1,…,N} has for sufficiently large N. The proof combines results from extremal graph theory with number theory. Assuming the famous abc-conjecture, we are able to both drop the coprimality condition and reduce the upper bound to for a fixed constant c.     

Effects of starch types on the properties of baked starch foams

In order to determine how the physicochemical properties of starch foams depend on the type of the starch used in baking process, starch foams were prepared using native starch and selected starch derivatives. The morphology, the density, the water adsorption capacity, the impact strength, and the thermal properties were determined for foams made from native starch, pregelatinized starch, hydroxypropylated starch with different degrees of substitution (DS = 0.015–0.025 and DS = 0.1), low distarch phosphate, medium distarch phosphate, and two cationic starch types (DS = 0.027–0.029 and DS = 0.029–0.033). The modified starch foams exhibited a more expanded structure with thinner cell walls than the foam made from native starch. The density of the native starch was 0.21 g cm^?3 , while the density of the modified starch foams was lower, in the range of 0.14–0.17 g cm^?3 except for the starch foam made from medium distarch phosphate. The thermal and physicochemical properties of the foams made from the other starch derivatives were dependent on the functional groups and the degree of cross-linking. The foam made from medium distarch phosphate had a significantly higher density and impact strength that was accompanied by a somewhat lower water adsorptivity.     

Composition depth profile analysis of electrodeposited alloys and metal multilayers: the reverse approach

The reverse depth profile analysis is a recently developed method for the study of a deposit composition profile in the near-substrate zone. The sample preparation technique enables one to separate the deposit and a thin cover layer from its substrate, and the initial roughness of the sample is much smaller than in the conventional sputtering direction. This technique is particularly suitable to study the zones being formed in the early phase of the electrodeposition of alloys. It has been demonstrated with the reverse depth profile analysis that in many cases when one component of an alloy is preferentially deposited, an initial zone is formed that is rich in the preferentially deposited component. This phenomenon is demonstrated for Ni–Cd, Ni–Sn, Fe–Co–Ni, Co–Ni, and Co–Ni–Cu alloys. The composition change is confined to the initial 150-nm-thick deposit, and it is the result of the interplay of the deposition preference and the depletion of the electrolyte near the cathode with respect to the ion reduced preferentially. The reverse depth profile analysis made it possible to compare the measured and the calculated composition depth profile of electrodeposited multilayers. It has been shown that the decay in the composition oscillation intensity in Co/Cu multilayers with the increase of the sputtering depth can be derived from the roughness measured as a function of the deposit thickness.

     

A new electrode for acid-base titration based on poly(copper phthalocyanine)

Journal of Solid State Electrochemistry - A new electrode based on poly(copper phthalocyanine) (poly(CuPc)) microparticles attached to gold is characterized and introduced as a simple, robust, and...     

Visible light activated photo-catalytic effect and local structure of iron silicate glass prepared by sol-gel method

A relationship between methylene blue (MB) decomposition ability under visible light and local structure of xFe₂O₃·(100-x)SiO₂ glass abbreviated as xFS prepared by sol-gel method was investigated by ⁵⁷Fe-Mössbauer spectroscopy, X-ray diffractometry (XRD) and ultraviolet-visible light absorption spectroscopy (UV-Vis). Mössbauer spectra of xFS glass with x of 10, 30 and 50 annealed at 1000 °C for 3 h were mainly composed of a paramagnetic doublet due to fayalite (Fe₂SiO₄), and magnetic sextets due to magnetite (Fe₃O₄) or hematite (α-Fe₂O₃). The absorption area (A) of α-Fe₂O₃ gradually increased from 0.0 to 10.3 and 100 % with the increasing Fe₂O₃ content (x) of annealed xFS glass. A leaching test performed by 20 mL of MB aqueous solution and 40 mg of annealed 50FS glass showed that MB concentration decreased from 16.2 to 4.7 μmol L^?1 after 2 h with the first order rate constant of 1.8 × 10^?4 s^?1. These results prove that annealed iron silicate glass containing α-Fe₂O₃ can decompose MB effectively under visible light irradiation.     

Visible light activated catalytic effect of iron containing soda-lime silicate glass characterized by 57Fe-Mössbauer spectroscopy

A relationship between local structure and visible light activated catalytic effect of iron containing soda lime silicate glass with the composition of 15Na₂O·15CaO·xFe₂O₃·(70-x)SiO₂, x = 5–50 mass %, abbreviated as NCFSx was investigated by means of ⁵⁷Fe-Mössbauer spectroscopy, X-ray diffractometry (XRD), small angle X-ray scattering (SAXS), electrospray ionization mass spectrometry (ESI–MS) and ultraviolet–visible light absorption spectroscopy (UV–Vis). Mössbauer spectra of NCFSx glass with ‘x’ being equal to or larger than 30 after isothermal annealing at 1,000 °C for 100 min consisted of a paramagnetic doublet and a magnetic sextet. The former had isomer shift (δ) of 0.24 mm s^?1 and quadrupole splitting (Δ) of 0.99 mm s^?1 due to distorted Fe^IIIO₄ tetrahedra, and the latter had δ of 0.36 mm s^?1 and internal magnetic field (H _int) of 51.8 T due to hematite (α-Fe₂O₃). The absorption area (A) of α-Fe₂O₃ varied from 47.2 to 75.9, 93.1, 64.8 and 47.9 % with ‘x’ from 30 to 35, 40, 45 and 50, indicating that the amount of precipitated α-Fe₂O₃ varied with the Fe₂O₃ content of NCFSx glass. The precipitation of α-Fe₂O₃ was also confirmed by XRD study of annealed NCFS glass with ‘x’ larger than 30. A relaxed sexted with δ, H _int and Γ of 0.34 mm s^?1 and 37.9 T and 1.32 mm s^?1 was observed from the Mössbauer spectra of annealed NCFSx glass with ‘x’ of 45 and 50, implying that the precipitation of non-stoichiometric iron hydroxide oxide with the composition of Fe_1.833(OH)_0.5O_2.5 having the similar structure of α-Fe₂O₃ and α-FeOOH. A remarkable decrease in the concentration of methylene blue (MB) from 10 to 0.0 μmol L^?1 with the first-order rate constant (k) of 2.87 × 10^?2 h^?1 was observed for 10-day leaching test using annealed NCFS50 glass under visible light irradiation. ESI–MS study indicated that existence of fragments with m/z value of 129, 117 and 207 etc. originating from MB having m/z of 284. This result evidently showed that the MB concentration decreased due to visible light induced decomposition caused by the visible light activated catalytic effect of α-Fe₂O₃ and/or Fe_1.833(OH)_0.5O_2.5 precipitated in soda-lime silicate glass matrix.     

Small Interfering RNAs Are Highly Effective Inhibitors of Crimean-Congo Hemorrhagic Fever Virus Replication In Vitro

Crimean-Congo hemorrhagic fever virus (CCHFV) is one of the prioritized diseases of the World Health Organization, considering its potential to create a public health emergency and, more importantly, the absence of efficacious drugs and/or vaccines for treatment. The highly pathogenic characteristic of CCHFV restricts research to BSL-4 laboratories, which complicates effective research and developmental strategies. In consideration of antiviral therapies, RNA interference can be used to suppress viral replication by targeting viral genes. RNA interference uses small interfering RNAs (siRNAs) to silence genes. The aim of our study was to design and test siRNAs in vitro that inhibit CCHFV replication and can serve as a basis for further antiviral therapies. A549 cells were infected with CCHFV after transfection with the siRNAs. Following 72 h, nucleic acid from the supernatant was extracted for RT Droplet Digital PCR analysis. Among the investigated siRNAs we identified effective candidates against all three segments of the CCHF genome. Consequently, blocking any segment of CCHFV leads to changes in the virus copy number that indicates an antiviral effect of the siRNAs. In summary, we demonstrated the ability of specific siRNAs to inhibit CCHFV replication in vitro. This promising result can be integrated into future anti-CCHFV therapy developments.