A Metatitanic Acid Particulate Xerogel: Green Synthesis, Structure Determination, and Detailed Characterization.

The manuscript focuses on an original method of preparation of metatitanic acid when only environmentally safe base substances are used in the synthesis process. The synthesis is based on the reaction of solid titanyl sulfate in an aqueous solution of sodium hydroxide. This method allows for (i) a full preservation of the morphology of the starting titanyl sulfate and (ii) a preparation of metatitanic acid substances with specific parameters. This can be achieved via a precise control of the alkali metal/titanyl sulfate ratio resulting in substances with varying contents of alkali metals or even sulfate anions. The prepared metatitanic acid then also contains very small weakly crystalline particles (2-3 nm) and forms pseudomorphic aggregates whose shape and dimensions correspond to those of the starting titanyl sulfate. These aggregates exhibit regular nanoporosity with a high surface area of up to 500 m2·g-1, have no tendency to form colloids, and are mechanically highly resistant even by high-energy ultrasound. The characterization of the resulting products is done via their chemical composition and methods of structural analysis, as well as by electron microscopy and local analysis. The mechanism of product formation is discussed based on the structure of the precursor, including the so far unknown structure of metatitanic acid.

Persistent Homology Approach for Human Presence Detection from 60 GHz OTFS Transmissions.

Orthogonal Time Frequency Space (OTFS) is a new, promising modulation waveform candidate for the next-generation integrated sensing and communication (ISaC) systems, providing environment-awareness capabilities together with high-speed wireless data communications. This paper presents the original results of OTFS-based person monitoring measurements in the 60 GHz millimeter-wave frequency band under realistic conditions, without the assumption of an integer ratio between the actual delays and Doppler shifts of the reflected components and the corresponding resolution of the OTFS grid. As the main contribution of the paper, we propose the use of the persistent homology technique as a method for processing gathered delay-Doppler responses. We highlight the advantages of the persistent homology approach over the standard constant false alarm rate target detector for selected scenarios.

Tuning the C/N Ratio of C-Rich Graphitic Carbon Nitride (g-C3 N4 ) Materials by the Melamine/Carboxylic Acid Adduct Route.

C-rich graphitic carbonitride materials (CNx ) with a large range of compositions have been prepared thanks to the self-assembly, in different ratios, of melamine (M) and a panel of polycarboxylic acids (A) such as oxalic, tartaric and citric acid. The thermal conversion of the formed adducts (MAy ), led to CNx phases, with x ranging from 0.66 to 1.4 (x=1.33 for g-C3 N4 for comparison). The properties of these materials were examined by different techniques (XRD, Raman spectroscopy, TEM, TGA, XPS and DRIFT). It appears that the increase in the C content is associated with the disappearance of the long-range order of heptazine units and an increase in the sub-nanometer carbon-rich cluster size within the graphitic g-C3 N4 structure. This trend is followed by a significant increase in the interlayer spacing and a lower proportion of N=C-N bonds compared to C=C bonds. The thermal stability under an inert atmosphere of these phases and their UV-Visible absorbance properties were also investigated.

Digitally-Compensated Wideband 60 GHz Test-Bed for Power Amplifier Predistortion Experiments.

Millimeter waves will play an important role in communication systems in the near future. On the one hand, the bandwidths available at millimeter-wave frequencies allow for elevated data rates, but on the other hand, the wide bandwidth accentuates the effects of wireless front-end impairments on transmitted waveforms and makes their compensation more difficult. Research into front-end impairment compensation in millimeter-wave frequency bands is currently being carried out, mainly using expensive laboratory setups consisting of universal signal generators, spectral analyzers and high-speed oscilloscopes. This paper presents a detailed description of an in-house built MATLAB-controlled 60 GHz measurement test-bed developed using relatively inexpensive hardware components that are available on the market and equipped with digital compensation for the most critical front-end impairments, including the digital predistortion of the power amplifier. It also demonstrates the potential of digital predistortion linearization on two distinct 60 GHz power amplifiers: one integrated in a direct-conversion transceiver and an external one with 24 dBm output power.

Kinetics of Resorcinol-Formaldehyde Condensation-Comparison of Common Experimental Techniques.

Porous carbons, originated from resorcinol-formaldehyde (RF) gels, show high application potential. However, the kinetics and mechanism of RF condensation are still not well described. In this work, different methods (dynamic light scattering-DLS, Fourier transform infrared spectroscopy-FTIR, low field 1H nuclear magnetic resonance relaxometry-1H-NMR, and differential scanning calorimetry-DSC) were used to follow the isothermal RF condensation of mixtures varying in catalyst content (Na2CO3) and reactant concentration. The applicability and results obtained by the methods used differ significantly. The changes in functional groups can be followed by FTIR only at very early stages of the reaction. DLS enables the estimate of the growth of particles in reaction solution, but only before the solution becomes more viscous. Following the relaxation of 1H nuclei in water during RF condensation brings a different view on the system-this technique follows the properties of the present water that is gradually captured in polymeric gel. From this side, the process behaves similarly to the nucleation reaction, which is in contradiction to the n-order mechanism confirmed by other techniques. The widest range of applicability was found for DSC measurement of the freezing/melting behavior of the reaction mixture, which is possible to use without any limitations until full solidification. Furthermore, this approach enables us to follow the gradual formation and development of the gel through the intermediate undergoing glass transition.

Interaction among clays and bovine serum albumin.

Interactions between bovine serum albumin and various clays including pure clay minerals and bentonite were studied with the aim to describe the interaction process. The adsorption of albumin on the clays is strongly affected by the behavior of clays in the aquatic environment (hydrolysis and release of cations). A sufficient amount of albumin was adsorbed on the acid-activated montmorillonite K10 (0.067 mg mg-1) and on the illite-smectite (0.086 mg mg-1). These clay minerals do not strongly affect the sorption solution parameters such as pH value and content of cations. Practically no adsorption was observed on the bentonite and vermiculite. Bentonite and vermiculite are subject to stronger interactions with water which cause the increase of pH value of the sorption solution and release of cations to the solution and thus they cause conformational changes of albumin, which was confirmed by circular dichroism measurements. Obtained results were confirmed by infrared spectroscopy and thermal analysis as well. Interaction of studied materials with bovine serum albumin causes the reduction of particle size in the case of all studied clays except vermiculite. Albumin probably attacks the clay structure during the adsorption, which causes the decrease of particle size. The presented work contributes to the knowledge about interaction of bovine serum albumin with clays in the field of influence of physico-chemical behaviour of clays in the solution on the interaction with albumin.

The role of the oxygen functional groups in adsorption of copper (II) on carbon surface.

The effect of carbon surface oxidation on the adsorption of Cu(II) ions from aqueous solution was studied in order to explain the role of the oxygen functional groups in the binding of copper ions. Pristine carbonaceous adsorbent was oxidized to a various extent of oxygen uptake (Fenton-like oxidation < persulphate in H2SO4 < H2O2 in HNO3). Equilibrium adsorption tests were performed in acetate buffer at pH ≈ 5. The results show that the adsorption capacity of pristine adsorbent is expectable low (~0.1 mmol g-1). The oxidized samples adsorb Cu(II) at a considerably higher level of ~1.4 mmol g-1 despite the degree of surface oxidation. Analysis of the surface groups (FTIR, TPD) and surface charge (zeta potential) of used adsorbents and their Cu(II) saturated counterpart lead to the finding that Cu(II) ions are mostly bonded by complexation with the dissociated carboxylic groups (partly formed by anhydrides hydrolysis) probably in the form of Cu(Ac)+ formed in the acetate buffer. The extent of dissociation is given by equilibrium pH during the adsorption and does not depend on the total amount of the surface groups. Thus, the content of active sites and consequently adsorption capacity is independent on the degree of oxidation when pH is kept constant. The results indicate that even moderate oxidation treatment of carbonaceous materials can produce highly effective adsorbents for Cu(II) immobilization.