Structure and properties of the mesophase of syndiotactic polystyrene. II. Effect of stepwise extraction on the preparation of the mesophase

In this study, a novel stepwise extraction method has been examined. The guest molecules housed between the helices of the clathrate δ form of syndiotactic polystyrene can be removed completely with this method. A systematic study of the preparation of a solvent‐free mesophase (emptied clathrate) membrane, its helical and residual solvent contents, and its structural transformations has been performed. In this first attempt, an enhancement in the TTGG helical content has been observed in the extracted membrane, and a conceptual mechanism is proposed. © 2002 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 41: 269–273, 2003     

Structure and properties of the mesophase of syndiotactic polystyrene. VIII. Solvent sorption behavior of syndiotactic polystyrene/p‐chlorotoluene mesophase membranes

A crystalline δ form of a syndiotactic polystyrene (sPS) membrane was prepared from a solution of sPS (1 wt %) and p‐chlorotoluene (p‐CT) by a solution‐casting method. The mesophase (δ empty form) of sPS was obtained by the extraction of the guest solvent from the δ form of sPS by a stepwise solvent‐extraction method. The sPS/p‐CT mesophase membrane [p‐CT (A‐M)] was used for the sorption of 1 mol % p‐CT for different times and for the sorption of different concentrations of p‐CT, chlorobenzene (CB), p‐xylene (p‐X), toluene, and chloroform for 48 h. The presence of solvents in the sPS membrane was confirmed by IR analysis. A thermal study revealed that the sorption amount of 1 mol % p‐CT increased with increasing immersion time, and the sorption amounts of different solvents increased with increasing solvent concentration. Differential scanning calorimetry results showed that the desorption peak temperature increased as the amount of the solvent increased in the clathrated sPS membrane. Wide‐angle X‐ray diffraction results showed that 2θ at 8.25° was slightly shifted toward 8°, and there was no change in the peak position at 10° for p‐CT (A‐M), which was immersed in different solvents (1 mol %); however, the intensity of 2θ at 10° was not similar for all the samples. Among the solvents used for the sorption studies at 1 mol %, p‐CT (A‐M) could sorb more p‐CT and CB than p‐X, toluene, and chloroform. The solvent sorption isotherm was the Langmuir sorption mechanism. © 2004 Wiley Periodicals, Inc. J Polym Sci Part B: Polym Phys 42: 3439–3446, 2004     

Laser writing techniques for photomask fabrication using a femtosecond laser

Photomasks are the backbone of microfabrication industries. Currently they are fabricated by a lithographic process, which is very expensive and time consuming since it is a multi-step process. These issues can be addressed by fabricating photomasks by direct femtosecond laser writing, which is a single-step process and comparatively cheaper and faster than lithography. In this paper we discuss our investigations on the effect of two types of laser writing techniques, namely front- and rear-side laser writing, with regard to the feature size and the edge quality of a feature. It is proved conclusively that for the patterning of masks, front-side laser writing is a better technique than rear-side laser writing with regard to smaller feature size and better edge quality. Moreover the energy required for front-side laser writing is considerably lower than that for rear-side laser writing. Received: 22 May 2001 / Accepted: 14 September 2001 / Published online: 17 October 2001     

Novel simulated moving-bed adsorber for the fractionation of gas mixtures

The separation of propylene-propane mixture is an energy intensive operation commercially practiced using cryogenic distillation. The separation by pressure swing adsorption has been studied as an alternative. A fixed-bed pressure swing adsorption yields the heavy component as a pure product. The product recovery and the productivity are not high. In a moving-bed process, because of the counter-current solid-gas contact, the separation achieved is similar to that of the fractionation by distillation. Although the moving-bed operation offers the upper limit for the performance of a cyclic adsorptive process, due to mechanical complexities in the handling of solids the 'simulated' moving-bed is preferred. By moving the inlet and outlet ports of streams located along the length of the bed, a moving-bed process can be realized in a fixed bed. We describe here a 'moving-port' system which permits injection or withdrawal of the fluid along the axial direction in a fixed bed. A fixed bed embedded with the moving-port systems emulates a simulated moving-bed adsorber. The proposed adsorber can fractionate a binary gas mixture into two product streams with high purities. It is similar to the Sorbex process of UOP but does not have the eluent as an additional separating agent. A parametric study indicates that high purity products and a higher productivity by an order of magnitude can be achieved with simulated moving-beds compared to the fixed beds.     

Determination of Natural Vitamin E from Italian Hazelnut Leaves

A new potential source of natural vitamin E from thirteen samples of Corylus avellana L. leaves was screened: the major Italian cultivar — Tonda romana (collected from Latium and Sardinia localities); ten local genotypes from Sardinia — Moro seme, Suconcale, Moro, Sarda grossa, Sarda grossa seme, Sarda schiacciata, Coccoredda, Sarda lunga, Sarda piccola and Sarda tardiva; wild genotype — Selvatico from Latium. The determination was performed after optimizing the high-efficiency pressurized liquid extraction (PLE) conditions of α-tocopherol from Italian hazelnut tree green leaves. Moro from Sardinia showed the highest content of α-tocopherol (237.4±0.3 μg/g d.w). Leaves of this genotype may be considered as a potential new source for natural α-tocopherol. __________ Published in Khimiya Prirodnykh Soedinenii, No. 6, pp. 538–540, November–December, 2005.