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991.
Jin-Woong?Kim Jin-Gyu?Park Jee-Hyun?Ryu Ih-Seop?Chang Kyung-Do?SuhEmail author 《Colloid and polymer science》2005,283(11):1233-1240
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. 相似文献
992.
Paavo?Mansikkam?ki Manu?Lahtinen Kari?RissanenEmail author 《Cellulose (London, England)》2005,12(3):233-242
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. 相似文献
993.
Tae?Shin?Chung Young?Mee?Na Shin?Won?Kang Ok-Sang?JungEmail author Young-A?Lee 《Transition Metal Chemistry》2005,30(5):541-545
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 [PtII (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 [PtIV (OH)(Y)(X)2(N–N)] (Y = OH, OCH3). The crystal structures of [PtIV(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) Å3, Z = 2R = 0.0503) and [PtIV(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) Å3, 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. 相似文献
994.
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. 相似文献
995.
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. 相似文献
996.
Thermodynamics and crystallization kinetics of the hydrothermal synthesis of Na4Ti4Si3O10 (NaTS) were systemically studied by both experiments and model simulation. Experimental results showed that the curve of
crystallinity with time was a characteristic signmoid in the shape that indicated the crystallization of Na4Ti4Si3O10 was a typical spontaneous nucleation process on the laboratory scale. Crystallization of NaTS belongs to the liquid-liquid
transformation mechanism and the reaction is endothermic (ΔH = 15.3 kJ/mol). A mathematic model of crystallization kinetics was developed to simulate the synthesis of NaTS. Runge-Kutta
and simplex methods were adopted to solve the partial differential equations. Model results fitted well with the experimental
data and showed that the synthesis process belongs to spontaneous nucleation and crystal growth. Moreover, the very small
crystal growth constant (5.6·10−7) and gel dissolution constant (7.0·10−7) indicate they are the rate-limiting steps of the whole synthesis process. 相似文献
997.
Complex systems of paramagnetic centres existing in demineralised flame coal (71.4 wt% C), medium-rank coal (85.6 wt% C) and
anthracite (94.9 wt% C) were analysed by electron paramagnetic resonance spectroscopy (EPR). Different groups of paramagnetic
centres were searched in macerals (exinite, vitrinite, inertinite) of coals with carbon contents of 73.8 wt% C and 85.6 wt%
C. Experimental EPR spectra were fitted by different superposition of theoretical lines. Total concentration of paramagnetic
centres both in coal and macerals increases with carbon content in the sample. Total concentration of paramagnetic centres
in macerals increases from exinite to inertinite. Four groups of paramagnetic centres were found in medium-rank coal, and
only two groups exist in flame coal and anthracite. The EPR spectrum of medium-rank coal is a superposition of two broad and
two narrow lines. Both broad and narrow, and two narrow lines were measured in EPR spectra of flame coal and anthracite, respectively.
Two types of paramagnetic centres with broad lines and one group with narrow lines exist in exinite and vitrinite from medium-rank
coal. Two narrow components were observed in EPR spectra of its inertinite. Two different broad electron paramagnetic resonance
signals were detected for macerals from low-coalificated coal. Paramagnetic centres systems of medium-rank coal samples reveal
the most complex character. Broad EPR lines were not observed for the higher coalificated samples, i.e., anthracite and inertinite
from medium-rank coal. Narrow lines do not occur in EPR spectra of low-coalificated macerals. Strong dipolar interactions
and fast spin-lattice relaxation processes are characteristic for paramagnetic centres with broad lines. Strong exchange interactions
and short spin-lattice relaxation time were measured for paramagnetic centres with the narrowest EPR signals. 相似文献
998.
The kinetics of the oxidation of five catecholamines viz., dopamine (A), L-dopa (B), methyldopa (C), epinephrine (D) and norepinephrine
(E) by sodium N-chloro-p-toluenesulfonamide or chloramine-T (CAT) in presence of HClO4 was studied at 30±0.1 °C. The five reactions followed identical kinetics with a first-order dependence on [CAT]
o
, fractional-order in [substrate]
o
, and inverse fractional-order in [H+]. Under comparable experimental conditions, the rate of oxidation of catecholamines increases in the order D>E>A>B>C. The
variation of ionic strength of the medium and the addition of p-toluenesulfonamide or halide ions had no significant effect
on the reaction rate. The rate increased with decreasing dielectric constant of the medium. The solvent isotope effect was
studied using D2O. A Michaelis-Menten type mechanism has been suggested to explain the results. Equilibrium and decomposition constants for
CAT-catecholamine complexes have been evaluated. CH3C6H4SO2NHCl of the oxidant has been postulated as the reactive oxidizing species and oxidation products were identified. An isokinetic
relationship is observed with β=361 K, indicating that enthalpy factors control the reaction rate. The mechanism proposed
and the derived rate law are consistent with the observed kinetics. 相似文献
999.
Both single-molecule detection (SMD) methods and miniaturization technologies have developed very rapidly over the last ten years. By merging these two techniques, it may be possible to achieve the optimal requirements for the analysis and manipulation of samples on a single molecule scale. While miniaturized structures and channels provide the interface required to handle small particles and molecules, SMD permits the discovery, localization, counting and identification of compounds. Widespread applications, across various bioscience/analytical science fields, such as DNA-analysis, cytometry and drug screening, are envisaged. In this review, the unique benefits of single fluorescent molecule detection in microfluidic channels are presented. Recent and possible future applications are discussed.Dedicated to the memory of Wilhelm Fresenius 相似文献
1000.
Gytis-Kazimieras Kupetis Gintautas ?aduikis Ona Nivinskien? Olegas Eicher-Lorka 《Monatshefte für Chemie / Chemical Monthly》2002,71(11):313-321
A series of 1-alkyl-4-dialkylaminopyridinium halides derived from 4-dimethylamino- and 4-morpholinopyridines were synthesized and tested as phase-transfer catalysts in three typical reactions of dichlorocarbene: dehydration of benzamide, N-formylation of diphenylamine, and dichlorocyclopropanation of styrene. The catalytic performance of the above compounds was found comparable or higher than that of conventional quaternary ammonium catalysts. The influence of catalyst structure on the reactivity was evaluated. 相似文献