Synthesis of poly(phenylene oxide) — aromatic polyester multiblock copolymers

Summary Poly(phenylene oxide) (PPO) — aromatic polyester multiblock copolymers were synthesized by polycondensation of bisphenol-A / isophthalic acid or m- and p-hydroxybenzoic acids in the presence of PPO having a carboxylic acid at one end and a phenolic hydroxy group at the other using triphenylphosphine / hexachloroethane as coupling agent. TG analysis showed that the multiblock copolymer showed relatively high thermal stability. Received: 5 January 1998/Accepted: 4 February 1998     

Dickey–Fuller, Lagrange Multiplier and Combined Tests for a Unit Root in Autoregressive Time Series

In this paper we investigate (augmented) Dickey–Fuller (DF) and Lagrange multiplier (LM) type unit root tests for autoregressive time series through comprehensive Monte Carlo simulations. We consider two sorts of null and alternative hypotheses: a unit root without drift versus level stationarity and a unit root with drift versus trend stationarity. The DF-type coef ficient tests are found to show the best overall performance in both cases, at least if the sample size is sufficiently large. How ever, it is also found that the DF and LM tests are roughly complementary with regard to their finite-sample power. We therefore consider combining these two types of unit root tests to obtain ( ad hoc 'but') 'robust' test procedures. Critical values for the proposed tests are provided     

A Novel Copolymer: Starch‐g‐Polyvinylpyrrolidone

In this study, graft copolymerization of N‐vinylpyrrolidone (N‐VP) onto starch was carried out in an aqueous medium using azobisisobutyronitrile (AIBN) as initiator. The variables affecting the graft copolymerization, such as monomer and initiator concentrations, reaction time and temperature, were thoroughly examined. In general, grafting of N‐vinylpyrrolidone onto starch increased with the increase in time and monomer concentration up to a certain value and then leveled off. Similarly, increase both in initiator concentration and temperature first favored and than impeded the grafting reaction. Optimum conditions established for grafting were as follows: N‐VP = 0.7 M, AIBN = 1.5×10^‐3 M, T = 70°C and t = 5 h. Structural changes of the grafted starch were followed by FTIR, intrinsic viscosity and water absorption capacity studies.     

Characterization of bacteriocins from two Lactococcus lactis subsp. lactis isolates

In this study, bacteriocins from two Lactococcus lactis subsp. lactis isolates from raw milk samples in Turkey designated OC1 and OC2, respectively, were characterized and identified. The activity spectra of the bacteriocins were determined by using different indicator bacteria including Listeria, Bacillus and Staphylococcus spp. Bacteriocins were tested for their sensitivity to different enzymes, heat treatments and pH values. Loss of bacteriocin activities after alpha-amylase treatment suggested that they form aggregates with carbohydrates. Molecular masses of the purified bacteriocins were determined by SDS-PAGE. PCR amplification was carried out with specific primers for the detection of their structural genes. As a result of these studies, the two bacteriocins were characterized as nisin and lacticin 481, respectively. Examination of plasmid contents of the isolates and the results of plasmid curing and conjugation experiments showed that in L. lactis subsp. lactis OC1 strain the 39.7-kb plasmid is responsible for nisin production, lactose fermentation and proteolytic activity, whereas the 16.0-kb plasmid is responsible for lacticin 481 production and lactose fermentation in L. lactis subsp. lactis OC2 strain.     

Hydrogen isotope permeation from cooling water through various metal piping

In order to investigate the behavior of hydrogen isotope on the water–metal boundary, deuterium permeation experiments from heavy water vessel through various metal piping, such as pure iron (Fe), nickel (Ni), stainless steel (SS304), and pure iron with 10 μm gold plating, were performed at 573 K and at 15 MPa. During the experiment, surfaces of metal piping except gold plating one were oxidized at the heavy water boundary and then deuterium would generate by the oxidation reactions. This deuterium could be detected by mass spectrometer, which monitored the inside gases of the piping under continuous evacuation. The result showed clearly that the deuterium permeated through Fe, Ni, and SS304 piping was detected as mainly deuterium gas (D₂) under continuous evacuation, though that through gold plating one could not be detected effectively. The D₂ permeation rate through Fe, Ni, and SS304 piping reached equilibrium conditions with oxide generation at D₂O–metal boundary, although concluding the transfer mechanism will require further testing and modeling activities.     

Numerical analysis of residual stress distribution generated by welding after surface machining based on hardness variation in surface machined layer due to welding thermal cycle

Recently, stress corrosion cracking (SCC) has been observed near the welded zone of the primary loop recirculation pipes made of low-carbon austenitic stainless steel type 316L in boiling water reactors. SCC is initiated by superposition effect of three factors. They are material, environmental and mechanical factors. For non-sensitized material such as type 316L, residual stress as a mechanical factor of SCC is comparatively important. In the joining processes of pipes, butt welding is conducted after surface machining. Surface machining is performed in order to match the inside diameter and smooth surface finish of pipes. Residual stress is generated by both processes. Moreover, residual stress distribution generated by surface machining is varied by subsequent welding processes, and it has the maximum residual stress around 900 MPa near the weld metal. The variation of metallographic structure, such as recovery and recrystallization, in the surface machined layer due to the welding thermal cycle is an important factor for this residual stress distribution. In this study, thermal ageing tests were performed in order to evaluate hardness variation due to the thermal cycle in the surface machined layer. Results of thermal ageing tests were applied to the finite-element method as the additivity rule of the hardness variation. Varied hardness was converted into equivalent plastic strain. Then, thermo-elastic-plastic analysis was performed under residual stress fields generated by surface machining. As a result, analytical results of surface residual stress distribution generated by bead-on-plate welding after surface machining show good agreement with measured results by the X-ray diffraction method. The maximum residual stress near the weld metal is generated by the same mechanism as in the both-ends-fixed bar model in the surface machined layer that has high yield stress.     

Influence of tungsten–carbon mixed layer and irradiation defects on deuterium retention behavior in tungsten

The D₂⁺ fluence dependence on deuterium (D) retention was studied to clarify the D retention mechanism in tungsten. The additional D desorption stage was observed around 660 K in the TDS spectrum for a sample implanted with D₂⁺ up to the fluence of 10²³ D⁺ m^?2, which desorption stage was not observed the D₂⁺ implanted sample with the fluence less than 10²² D⁺ m^?2. The TEM observation showed that the highly dense voids were formed in tungsten by D₂⁺ implantation with the fluence of 10²³ D⁺ m^?2, considering that the D would be trapped by voids. To understand the D trapping by voids in C⁺ implanted tungsten, C⁺–D₂⁺ sequential implantation experiments at various C⁺ implantation temperatures were performed. It was found that the amount of D desorbed around 560 K was increased by increasing the C⁺ implantation temperature. The formation of the voids was observed with increasing the C⁺ implantation temperature by TEM, indicating that the increase of D desorption around 560 K was caused by the formation of voids. However, the desorption temperature of D trapped by voids in C⁺ implanted sample was lower than that in D₂⁺ implanted one. TEM observation and XPS measurement indicated that this difference was caused by the increase of void size and/or the presence of implanted carbon.     

Preparation of gelatin fiber by gel spinning and its mechanical properties

A gel‐spinning process was used in an attempt to prepare a gelatin fiber with a high level of drawability. A gel fiber prepared by extrusion of 15 wt % gelatin in dimethyl sulfoxide into methanol at ?20°C was drawn to sixteen times the original length. After extraction of the dispersion medium, the mechanical strength of the fiber increased markedly with the draw ratio, and the fiber exhibited a tensile strength of 146 MPa and a Young's modulus of 2.3 GPa when drawn to the maximum. A gelatin fiber with greater mechanical strength was obtained when ethylene glycol was used as the spinning solvent. The X‐ray diffraction profile indicated the formation of triple‐helical structures and their lateral association, which is responsible for the mechanical strength of the fiber. Heat‐treatment improved the water‐resistance of the prepared fiber. γ‐Irradiation and treatment with glutaraldehyde improved the mechanical strength of the fiber. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

pH‐ and temperature‐sensitive in vitro release of salicylic acid through poly(vinyl alcohol‐g‐acrylamide) membranes

In this study, acrylamide (AAm) was grafted onto poly(vinyl alcohol) (PVA) in solution with UV radiation, and membranes were prepared from the graft copolymer (PVA‐g‐AAm) for transdermal release of salicylic acid (SA) at in vitro conditions. Permeation studies were carried out using a Franz‐type diffusion cell. Release characteristics of SA through PVA and PVA‐g‐AAm membranes were studied using 2.0 mg/mL SA solutions. Effects of the presence of AAm in the copolymer, pH of donor and acceptor solution, and concentration of SA and temperature on the release of SA were investigated. Permeation of SA through the membranes was found to be pH‐dependent, and increase in pH generally increased the release percentage of SA, and the presence of AAm in the membrane positively affected the permeation. The effect of concentrations of SA on the permeation was also searched using saturated solution of SA, and permeated amount of SA was found to be less than in the case of unsaturated SA solution. Studies showed that the release of SA from PVA‐g‐AAm membranes was temperature‐sensitive and increase in temperature increased the permeation rate. 82.76% (w/w) SA was released at the end of 24 h at (39 ± 1)°C, and the overall activation energy for the permeation of SA through PVA‐g‐AAm membranes was found to be 19.65 kJ/mol. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2008