The influence of intercalation rate and degree of substitution on the electrorheological activity of a novel ternary intercalated nanocomposite

Kaolinite/dimethylsulfoxide (DMSO)/carboxymethyl starch (CMS) ternary nanocomposites were prepared according to the combination of intercalation and solution reaction. The results show that the intercalation rate (IR) of kaolinite in the ternary composite is adjusted by changing the mass rate, and the basal spacing of kaolinite was swelled from 0.715 to 1.120 nm. At the suitable component ratio of ternary nanocomposite, the optimum electrorheological (ER) effect can be attained. It is apparent that the notable ER effect of ternary ER fluid was attributed to the prominent dielectric property of the ternary nanocomposite electrorheological fluids (ERF), which is closely associated with the IR. With the increase of degree of substitution, the ER effect of ternary composite ERF is enhanced.     

Comparison of the Temperature Effect on the π∗←n and π∗←π Electronic Transition Bands of NO<Subscript>3</Subscript><Superscript>−</Superscript>(aq)

The effect of temperature on the π∗←π transition band in the UV absorption spectrum of NO₃⁻(aq) centered at ≈200 nm was studied in the temperature range 10–70 ^∘C. The observed temperature independence of this band was in contrast to the significant influence of temperature on the nitrate π∗←n transition reported recently by us. However, taking into account the electronic states involved in both the transitions, it was concluded that this finding was in accordance with our previous assumption that interconversion between spectrally distinct (with respect to π∗←n band) nitrate species included the rupture/formation of hydrogen bond(s) in the hydration shell of the nitrate ion.     

Monodisperse chloromethyl-functionalized macroporous polymer particles by seeded polymerization in aqueous media

This study presents a method to produce monodisperse chloromethyl-functionalized macroporous poly(styrene-co-divinylbenzene) polymer particles by seeded polymerization in aqueous media. We observed that the molecular structure of polystyrene seed particles, the composition of the secondary monomer mixtures, and the type of solvents were very important factors that determine the morphology and porosity of the final particles. This study proposes that the molecular chemistry of polystyrene seed polymers, increasing molecular weight or crosslinking, is another factor that can control the porosity of the final particles. Also, the selection of a poor solvent was effective in forming the larger surface area. In this study, it was confirmed that the chloromethyl groups introduced on the surface of porous particles were quantified chemically and their effective incorporation had a close relationship with the surface area.     

Structural Changes of Cellulose Crystallites Induced by Mercerisation in Different Solvent Systems; Determined by Powder X-ray Diffraction Method

The completeness of mercerisation can be evaluated by investigating the changes in the crystalline regions of cellulose from cellulose I (C-I) to cellulose II (C-II) by the X-ray powder diffraction method. Mercerisation experiments in four different solution systems: ethanol/water, acetone, DMSO and xylene, are reported. Also the effect of some additives, external pressure, treatment time and alkalisation temperature were studied. In two-phase solvent systems, structural changes of cellulose crystallites depended primarily on the distribution and solubility of sodium hydroxide in the solvent phases. The sodium hydroxide concentration in the hydrophilic phase must exceed 7–8 w/w-% before complete crystal change from C-I to C-II can occur. The precipitation of sodium hydroxide due to high concentration prevents the successful use of one-phase ethanol/water system in slurry process. On the contrary, the 2-propanol/water/sodium hydroxide system separates into two layers; to the water-rich lower layer and the 2-propanol-rich upper layer, where the sodium hydroxide remains mainly in the water-rich lower layer. This prevents the precipitation of sodium hydroxide and promotes the alkalisation of cellulose. Ammonium chloride and ammonium hydroxide clearly had a positive effect by promoting the crystal changes, however, the urea concentration used in this study was obviously too small. In the advantageous two-phase 2-propanol/water systems, the alkalisation time was only 15 min when the treatment temperature was kept between 0 and 10 °C. Reduced external pressure was found to have a small but still detectable positive effect on cellulose alkalisation while over-pressure prevented crystal changes.     

Facile generation of platinum(IV) compounds with mixed labile moieties. Hydrogen peroxide oxidation of platinum(II) to platinum(IV) compounds

Hydrogen peroxide oxidation of platinum(II) compounds containing labile groups such as Cl, OH, and alkene moieties has been carried out and the products characterized. The reactions of [Pt^II (X)₂ (N–N)] (X = Cl, OH, X₂ = isopropylidenemalorate (ipm); N–N 2,2-dimethyl-1,3-propanediamine [(dmpda), N-isopropyl-1,3-propanediamine (ippda)] with hydrogen peroxide in an appropriate solvent at room temperature affords [Pt^IV (OH)(Y)(X)₂(N–N)] (Y = OH, OCH₃). The crystal structures of [Pt^IV(OH)(OCH₃)(Cl)₂(dmpda)]·2H₂O (P-1 bar, a = 6.339(2) Å , b = 9.861(1) Å, c = 11.561(1) Å, a = 92.078(9)°, β = 104.78(1)°, γ=100.54(1)°, V = 684.3(2) ų, Z = 2R = 0.0503) and [Pt^IV(OH)₂(ipm)(ippda)]·3H₂O (C 2/c, a = 27.275(6) Å, b=6.954(2) Å, c = 22.331(4) Å, β = 118.30(2)°, V = 3729(2) ų, Z = 8, R = 0.0345) have been solved and refined. The local geometry around the platinum(IV) atom approximates to a typical octahedral arrangement with two added groups (OH and OCH₃; OH and OH) in a transposition. The platinum(IV) compounds with potential labile moieties may be important intermediate species for further reactions.     

Core/shell nanocomposite based on the local polarization and its electrorheological behavior

Aimed at the increase of electrorheological effect, a novel core/shell material was prepared by the combination of mechanochemical activity and sol-gel technique. The structure analyses X-ray diffraction, Fourier transform infrared spectrometry, scanning electron microscopy, and energy-dispersive spectrometry showed that a modified kaolinite/titanium oxide nanocomposite consisted of the mechanochemically activated kaolinite/NaCl complex coated by titanium oxide. A distinct enhancement of the electrorheological activity was found by using such particles dispersed in silicone oil than those of kaolinite or titanium oxide alone under a direct current electric field. Modified kaolinite/titanium oxide electrorheological fluid has a larger dielectric constant enhancement deltaepsilon', and a strong interfacial polarization occurs with a clear dielectric loss peak around 2 kHz. Doping NaCl into the core (kaolinite) by the mechanochemical activation and limiting the transferring of the ions by the shell (titanium oxide) may increase the interfacial polarizability of particles and induce a high electrorheological effect.     

Highly enantioselective 1,4-conjugate addition of diethylzinc to acyclic enones with chiral phosphite–pyridine ligands derived from H8-NOBIN

A series of new phosphite–pyridine ligands, based on the H₈-binaphthyl backbone, were synthesized and employed in the copper-catalyzed enantioselective 1,4-conjugate addition of diethylzinc to acyclic enones. Ligands derived from (S)-H₈-NOBIN provided better results than their parent ligands in the reaction. Ligand L1 provided excellent ees for trans-4-aryl-3-buten-2-ones (up to 97.8% ee) as substrates. Ligand L2 was very efficient for various para-chalcones, and up to 97.2% ee was achieved.     

Method validation and qualification of instruments for atomic spectrometry

This work describes the analytical procedures for atomic absorption and inductively coupled plasma (ICP) techniques that have to be used in order to obtain a license to sell drugs in the USA. The qualification of atomic absorption spectrometers and ICP instruments is described. The method validation characteristics, e.g., accuracy, precision, linearity, range, detection limits, and quantification are discussed. The time involved and the quality of documentation are pointed out. The consequences for laboratory personnel and operating costs are also discussed.     

Solid-phase synthesis of amidines by the reduction of amidoximes

Amidines can be prepared on a solid support by reducing polymer-bound amidoximes with SnCl₂·2H₂O. The method has proved to be straightforward and highly efficient. Amidoximes attached to the solid support are readily available by treating resin-bound nitriles with hydroxylamine.     

Interface characteristics in diffusion bonding of Fe3Al with Cr18-Ni8 stainless steel

Fe3Al and Cr18-Ni8 stainless steel were diffusion-bonded in vacuum and a Fe3Al/Cr18-Ni8 interface with reaction layer was formed. Microstructure in the reaction layer at Fe3Al/Cr18-Ni8 interface was analyzed by means of scanning electron microscope (SEM) and electron probe micro-analyzer (EPMA). The growth of reaction layer with heating temperature (T) and holding time (t) was researched. The results indicate that FeAl, Fe3Al, Ni3Al, and alpha-Fe (Al) solid solution are formed in the reaction layer. These phases are favorable to promote the element diffusion and to accelerate the formation of the reaction layer at Fe3Al/Cr18-Ni8 interface. The growth of reaction layer obeys the parabolic law and its thickness (X) is expressed by X2 = 7.5 x 10(-4)exp(-83.59/RT)(t - t0).