Nonisothermal crystallization kinetics of PEO in ethylene terephthalate-ethylene oxide segmented copolymers

The nonisothermal crystallization behavior of Ethylene Terephthalate-Ethylene Oxide (ET-EO) segmented copolymers has been studied with the use of differential scanning calorimetry (DSC). The kinetics of PEO in ET-EO segmented copolymer under nonisothermal crystallization conditions has been analyzed with the Ozawa equation. The results show that there is no agreement with Ozawa's theoretical predictions in the whole crystallization process owing to the constraint of ET segments imposed on the EO segments. A distinct two-crystallization process has been investigated by using the Avrami equation modified by Jeziorny to deal with the nonisothermal crystallization data. The value of the Avrami exponent n is independent of the length of soft segments. However, the crystallization rate is sensitive to the length of soft segments. The longer the soft segments, the faster the crystallization will be.

Self-organization of interlaced network lamellar crystals of trans-1,4-polybutadiene (TPBD) on an amorphous surface

A novel morphology of TPBD crystals consisting of a three-dimensional interlaced network was obtained by casting the self-seeded 0.1% benzene solution onto carbon-boated mica. Both the transmission electron microscopy (TEM) and electron diffraction (ED) analyses showed that the network was composed of well-developed lamellae. It is imagined this interesting morphology is the results of asymmetrical growth of the original TPBD lamellae on the amorphous interface, and that their preferred orientation changed when they encountered each other.

Lamellar single crystals of nylon-10,10 crown from a dimethylformamide solution

A new solvent, dimethylformamide (DMF), and the traditional solvent, 1,4-butanediol, were used to prepare single crystals of nylon-10,10 from a dilute solution. The lamellae grown from DMF inhabited a more perfect structure and regular shape than those crystals crystallized from traditional solvents such as 1,4-butanediol and glycerin. These thin and perfect lamellar crystals demonstrated patterns of variation in spacing different from those of melt-crystallized spherulites on heating. Specifically, the two main spacings slightly separated rather than continuously approaching each other when the temperature was greater than 180 degreesC. This is a novel phenomenon observed in nylons. Nevertheless, the usual pattern of change in spacing was observed during the cooling process. These lamellar crystals showed more compact spacing of the (002) and (010/100) planes than spherulites at room temperature. (C) 2001 John Wiley & Sons, Inc.

Morphology and structure of micro-fibrillar crystal of nylon 10 10

The nanoscale and microscale fibrillar crystals of nylon 10 10 were obtained by atomizing the very dilute formic acid solution. The length-diameter ratio of these fibrillar crystals increases as the concentration of the atomizing solution increases. Electron diffraction (ED) analysis showed that the hydrogen-bonded sheet in these solution-grown fibrillar crystals was imperfect and had a lower order. Both electron diffraction and characteristic morphology show that melt-crystallized fibrillar crystals always possess perfect packing order and stable structure. A rather perfect ED pattern of the triclinic form of nylon 10 10 along the [001] zone was obtained by tilting the specimen 41 degrees along the elongated direction of the crystal. Fibrillar crystals from bulk have a great tendency to aggregate with parallel packing to form crystal clusters, which look like shish kebabs in morphology. Spherulite is observed occasionally in the domains with very rich sample. (C) 2001 Elsevier Science Ltd. All rights reserved.

Electrostatic-field-induced chain alignment of liquid crystalline copolyether TPP thin films

A liquid crystalline (LC) copolyether has been synthesized from 1-(4-hydroxy-4'-biphenyl)-2-(4-hydroxyphenyl)propane with 1,7-dibromoheptane and 1,11-dibromoundecane with a 50/50 (both in %) equal composition of the 7- and 11-methylene monomers [coTPP-7/11(5/5)]. A mono-domain with a homeotropic alignment can be induced by a thin film surface in the LC phase. When an electrostatic field is applied to the surface-induced mono-domains parallel to the thin film surface normal, the molecular alignment undergoes a change from the homeotropic to uniaxial homogeneous arrangement. However, when the field is applied to a direction perpendicular to the thin film surface normal. the molecular alignment is about 10 degrees -tilt with respect to the homeotropic alignment toward the a*-axis. This is because the permanent dipole moment of the copolyether is not right vertical to the molecular direction. The calculation of molecular dipoles indicates that the permanent dipole moment of this copolyether is about 70 degrees away from the molecular axis, which leads to a negative dielectric anisotropy. It is speculated that the 10 degrees- rather than 20 degrees -tilt is due to a balance between the alignment induced by the electrostatic field and the surface. In the electrostatic field, molecules are subjected to a torque tau, which is determined by the permanent dipole moment P and the electrostatic field E: tau = P x E. The molecular realignment in both parallel and perpendicular directions to the thin film surface normal is determined by satisfying the condition of tau = P x E = 0. (C) 2001 Elsevier Science Ltd. All rights reserved.

Size-affected crystallization of trans-1,4-polybutadiene

By using different catalyst systems, two trans-1,4-polybutadiene (TPBD) samples with different tr trans-content and molecular weight were synthesized. The phase transition of two samples from monoclinic form to hexagonal phase was revealed by differential calorimeter scanning and X-ray, respectively. The small-angle X-ray scattering measurements showed the remarkable discrepancy of phase transition and melting point between the two samples was attributed to the different lamellar thickness of crystals: The crystals with different crystalline morphology and lamellar thickness were developed by casting different concentration TPBD solutions. Transmission electron microscopy morphology observations proved that annealing the specimen at the temperature above the phase transition point for different times resulted in the different lamellae thickening of monoclinic form. It means that annealing the TPBD in its hexagonal phase will also slightly favor the increase of both the phase transition temperature and melting point of hexagonal phase. (C) 2001 Elsevier Science Ltd. All rights reserved.

Effect of electron radiation on crystal structure transition of trans-1, 4-polybutadiene

trans-1,4-Polybutadiene (PTBD) was synthesized by rare earth catalyst system, The effect of electron radiation on phase transition from monoclinic phase to hexagonal phase was observed by TEM, Electron diffraction patterns of monoclinic phase, hexagonal phase and two coexistent phases were recorded, The mechanism of phase transition was also discussed in this paper.

Separation of phenothiazines using aqueous and nonaqueous capillary electrophoresis

Separations of phenothiazines, promethazine(PZ), dioxypromethazine (OZ), chlorpromazine(CZ), trifluoperazine(TfZ) and thioridazine(TZ) by capillary electrophoresis in water and FA media were carried out and compared. Thus different selectivity and resolution were observed as media varying from water to FA. Migration order was PZ, OZ, CZ and TZ in water but (TZ+PZ), CZ and OZ in FA, when the same buffer, 25 mmol/L Tris and 25 mmol/L citric acid, was used. It also has been observed that pH has great effect on selectivity both in water and FA and a possible explanation was given. Separation efficiency was higher in FA media than in water because of the permission of high voltage applied. For all separations in FA 30 kV was applied, and when 25 mmol/L Tris was used as buffer, current was only 20 mu A and complete separation of TZ, CZ, PZ and OZ was achieved with effencicy higher than 3.5 x 10(5) theoretical plates for all analytes. The high performance of capillary electrophoresis in FA suggests that FA is an excellent media separation.

Chiral separation of binaphthol enantiomers in capillary electrophoresis

Binaphthol enantiomers could be baseline separated using cholic acid as chiral selector at the concentration of 20 mmol/L. The effects of cholic acid concentration and pH of the buffer on separation were studied. The influence of methanol, acetonitrile, iso-propyl alcohol were also studied.

Separation of promethazine and thioridazine using capillary electrophoresis with end-column amperometric detection

Promethazine and thioridazine were separated and detected by capillary electrophoresis with end-column amperometric detection. The influence of pH Value on oxidation potential, the peak current and the resolution were studied and the following conditions was selected: 0.03 M Na2HPO4 and 0.015 M citric acid at pH 3.0, detection potential at 1.10 V. The detection limits of these two substances were in the range of 10(-8) mol/l. The linear range spanned two to three orders of magnitude. This method was applied to the detection of promethazine and thioridazine spiked in urine. (C) 1999 Elsevier Science B.V. All rights reserved.

聚苯乙烯-聚丁二烯-聚苯乙烯三嵌段共聚物和聚苯乙烯共混体系的微相分离结构

嵌段共聚物的微相分离结构研究表明,改变某一组分的体积分数 f、聚合度 N、两组分间的相互作用参数 x 都可以改变其微相分离结构.当 xN>>10时,嵌段共聚物处于强相分离区;xN≤10时,体系处于弱相分离区.

Comparison of effectiveness of different ashing auxiliaries for determination of phosphorus in natural waters, aquatic organisms and sediments by ignition method

An improved method for the determination of phosphorus in natural waters, aquatic organisms and sediments by ignition method is proposed. The recoveries of phosphorus (P) from selected inorganic and organic P-containing compound standards after ignition with different auxiliaries, such as MgSO4, Mg(NO3)(2), MgO2, Mg(Ac-2) and CaCl2, were compared. We found that the phosphorus from most compound standards could not be completely recovered when these compounds were ignited (450-500degreesC) with the MgSO4 as auxiliary and the baked residue was extracted with 0.2 mol l(-1) HCl for 30min at 80degreesC or at room temperature. P recoveries, for example, were poor, less than 85%, if pyrophosphate and metaphosphate were ignited with the addition Of MgSO4 prior to the extraction of the baked residue with 0.2 mol l(-1) HCl at 80degreesC for 30 min. In contrast, MgO2, Mg(Ac)(2) and CaCl2, as well as Mg(NO3)(2), could all yield complete P recoveries at routine ashing temperatures (450-500degreesC). The results demonstrate that MgC12 is a more effective auxiliary agent for the determination of phosphorus in natural waters, aquatic organisms and sediments by ignition method than MgSO4 which is commonly used. (C) 2003 Elsevier Science Ltd. All rights reserved.

Extraction of phosphorus in natural waters and sediments by ignition method

Phosphorus recoveries from selected inorganic and organic P-containing compounds after ignition with auxiliaries, such as MgSO4, Mg (NO3)(2), MgCl2, Mg (Ac)(2) and CaCl2 were studied. It was found that the phosphorus could not be completely recovered when most P-containing compounds were ignited with MgSO4 at temperature not higher than 500degreesC if the baked residue was extracted with 0.2 mol/L HCl for 30 min at 80degreesC or at room temperature. In contrast, MgCl2, Mg(Ac)(2) and CaCl2, as well as Mg(NO3)(2), could all yield complete P recoveries. We suggest that MgCl2 rather than MgSO4, which is usually used, should be utilized as ashing auxiliary agent in the P extraction by ignition method. Although Mg (NO3)(2) is a highly effective auxiliary agent, yet interference from MgSO4, danger of explosion, toxicity of nitrogen dioxide and more manipulation steps may limit its widespread utilization. It is suggested that if sediment is ignited with MgCl2, the extraction of residue with 0.2 mol/L HCl for 30 min at 80degreesC could give good result.