Synthesis of Carbon–Nitrogen–Phosphorous Materials with an Unprecedented High Amount of Phosphorous toward an Efficient Fire‐Retardant Material

Phosphorus incorporation into carbon can greatly modify its chemical, electronic, and thermal stability properties. To date this has been limited to low levels of phosphorus. Now a simple, large‐scale synthesis of carbon–nitrogen–phosphorus (CNP) materials is reported with tunable elemental composition, leading to excellent thermal stability to oxidation and fire‐retardant properties. The synthesis consists of using monomers that are liquid at high temperatures as the reaction precursors. The molten‐state stage leads to good monomer miscibility and enhanced reactivity at high temperatures and formation of CNP materials with up to 32 wt % phosphorus incorporation. The CNP composition and fire‐retardant properties can be tuned by modifying the starting monomers ratio and the final calcination temperature. The CNP materials demonstrate great resistance to oxidation and excellent fire‐retardant properties, with up to 90 % of the materials preserved upon heating to 800 °C in air.     

The nanostructure of non-oriented electrical steel sheets

Nanostructures of two non-oriented electrical steels were investigated in order to elucidate the influence of nanostructure and its components on magnetic properties. The main difference between the two samples was related to the mean grain size and level of core loss. Surprisingly, the sample with coarser ferrite grains exhibited higher core loss. For this reason (HR)TEM imaging was carried out. Precipitation reactions were monitored using differential scanning calorimetry (DSC). Light microscopy, FE-SEM/EDX and EBSD analyses were also performed to analyse the microstructures and crystallographic textures. The results were compared and related to the magnetic properties. It was shown that besides the microstructural components, the nanostructure and nanoprecipitates also have a crucial impact on the magnetic properties.     

Retention of Some Metal Ions and Their Separation on Silica Gel Modified with Acid Red 88

 Acid Red 88 is strongly extracted by chloroform solutions of Aliquat 336 by an ion exchange mechanism and for its reextraction from the ion pair formed, relatively high concentrations of mineral acids are required. By impregnation of silica with the ion pairs between the cation of Aliquat 336 and the anion of the dye a chelating sorbent for metal ions can be obtained. The sorbent prepared may be successfully used for separation of mixtures of various metal ions by the column extraction chromatography technique, additional purification of sodium and potassium salts from ions of heavy metals and for concentration of trace amounts of ions of various metals from aqueous solutions followed by their quantitative determination. The sorbent can be used repeatedly in the process of sorption and desorption of metal ions (especially those forming less stable complexes with the reagent) after regeneration with solutions of perchloric acid. Received January 28, 1998. Revision March 1, 1999.     

The impact of ambient gas on the magnetic properties of Ti40Zr40Ni20 powders during mechanical alloying

Ti₄₀Zr₄₀Ni₂₀ in the form of elemental powders was mechanically alloyed in a planetary ball-mill under argon and hydrogen atmospheres at an acceleration of 55 m s^?2 for different time intervals. The samples were analyzed by X-ray diffraction (XRD), vibrating-sample magnetometry (VSM) and scanning electron microscopy (SEM), which revealed the large impact of the ambient gas, i.e. argon and hydrogen, on the magnetic properties, morphology and structure. Namely, during mechanical alloying in argon the saturation magnetization decreased due to the modification of the Ni d-states upon alloying with paramagnetic Ti and Zr, whereas in hydrogen the Ni d-states remained largely unmodified, since the formation of TiH₂ and ZrH₂ was faster than the alloying with the ferromagnetic nickel. However, after 40 h we obtained a mixture of nanocrystalline Ni and ZrH₂/TiH₂ hydrides, which in equilibrium contained 1.55 mass% of hydrogen. In the case of argon we determined welding of the Ti₄₀Zr₄₀Ni₂₀ amorphous particles, whereas in hydrogen such a process was suppressed by the brittle ZrH₂/TiH₂ hydrides. In addition, we revealed that the mechanical alloying of pure Ni powder for 100 h in argon does not affect its magnetic properties.     

Global intercompany assessment of ICIEF platform comparability for the characterization of therapeutic proteins

An international team spanning 19 sites across 18 biopharmaceutical and in vitro diagnostics companies in the United States, Europe, and China, along with one regulatory agency, was formed to compare the precision and robustness of imaged CIEF (ICIEF) for the charge heterogeneity analysis of the National Institute of Standards and Technology (NIST) mAb and a rhPD-L1-Fc fusion protein on the iCE3 and the Maurice instruments. This information has been requested to help companies better understand how these instruments compare and how to transition ICIEF methods from iCE3 to the Maurice instrument. The different laboratories performed ICIEF on the NIST mAb and rhPD-L1-Fc with both the iCE3 and Maurice using analytical methods specifically developed for each of the molecules. After processing the electropherograms, statistical evaluation of the data was performed to determine consistencies within and between laboratory and outlying information. The apparent isoelectric point (pI) data generated, based on two-point calibration, for the main isoform of the NIST mAb showed high precision between laboratories, with RSD values of less than 0.3% on both instruments. The SDs for the NIST mAb and the rhPD-L1-Fc charged variants percent peak area values for both instruments are less than 1.02% across different laboratories. These results validate the appropriate use of both the iCE3 and Maurice for ICIEF in the biopharmaceutical industry in support of process development and regulatory submissions of biotherapeutic molecules. Further, the data comparability between the iCE3 and Maurice illustrates that the Maurice platform is a next-generation replacement for the iCE3 that provides comparable data.     

Entropic trapping binding mechanism: its likely role in receptor-ligand and other biochemical systems

Entropy-driven binding continues to be discovered in receptor-ligand systems as well as in other important biochemical systems. In receptor-ligand systems the "thermodynamic agonist-antagonist discrimination" is often found: in some such receptor types the binding of antagonists is entropy-driven, in others this is a characteristic of the agonist binding. The interpretation of the entropy-driven binding mechanism in the systems in question is still rather elusive. Experimental findings clearly indicate that the entropic binding mechanisms which are usually considered cannot provide a consistent interpretation in these cases. Entropic trapping was therefore proposed in our earlier papers as a possible binding model which does not contradict the experimental facts. It is pointed out here that through the work which has appeared subsequently the existence of such a mechanism has been firmly established and that its role is strongly corroborated by the more recent data from several biochemical systems.     

Osmotic and volume properties of stereoregular poly(methacrylic acids) in aqueous solution: role of intermolecular association

Osmotic coefficients, phi, and apparent molar volumes, PhiV, of aqueous solutions of isotactic, syndiotactic, and atactic poly(methacrylic acid), i-PMA, s-PMA, and a-PMA, respectively, were measured at 298 K in dependence on polymer concentration and on degree of neutralization, alphaN, of carboxyl groups. The solutions of i-PMA have lower phi values than those of a-PMA and s-PMA in the whole region of alphaN. Molecular dynamics simulation studies of the isotactic and the syndiotactic PMA 101-mer have shown that lower phi is a consequence of a shorter distance between charges, which leads to a greater charge density of the isotactic polymer and thus to stronger binding of counterions. The experimental phi data were analyzed using a cylindrical cell model. Good agreement between theory and experiment was achieved when charges on the polyion were distributed periodically along the z-axis of the polyion in accordance with the simulation results. The alphaN dependence of the PhiV data pointed out that all PMA isomers bind an appreciable amount of water in the elementary dissociation process (electrostriction). For a- and s-PMA, the PhiV values decrease linearly with increasing alphaN, whereas they show a marked nonlinear dependence in the case of i-PMA for alphaN < 0.6. The latter finding was ascribed to a very high intermolecular association tendency of the isotactic polymer. This association tendency of PMA chains was confirmed by light scattering measurements. It is present in both i- and a-PMA solutions but is much more pronounced in the i-PMA case.