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- Author or Editor: D. Joseph x
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Abstract
The first experimental evidence of the existence of the rigid amorphous fraction (RAF) was reported by Menczel and Wunderlich for several semicrystalline polymers. It was observed that the hysteresis peak at the glass transition was absent when these polymers were heated much faster than they had previously been cooled. In the glass transition behavior of poly(ethylene terephthalate) (PET), the hysteresis peak gradually disappeared as the crystallinity increased. At the same time, it was noted that the ΔC p of higher crystallinity PET samples was much smaller than could be expected on the basis of the crystallinity calculated from the heat of fusion. It was also observed that this behavior was not unique to PET only, but is characteristic of most semicrystalline polymers: the sum of the crystallinity calculated from the heat of fusion and the amorphous content calculated from the ΔC p at the glass transition is much less than 100% (a typical difference is ~20–30%). This 20–30% difference was attributed to the existence of the “RAF”. The presence of the RAF also affected the unfreezing behavior of the “mobile (or traditional) amorphous fraction.” As a consequence, the phenomenon of the enthalpy relaxation diminished with increasing rigid amorphous content. It was suggested that the disappearance of the enthalpy relaxation was caused by the disappearance or drastic decrease of the time dependence of the glass transition. To check the validity of this suggestion, the glass transition had to be also measured on cooling in order to overlay it on the DSC curves measured on heating. However, before this overlaying work could be accomplished, the exact temperatures on cooling had to be determined since the temperature of the DSC instruments that time could not be calibrated on cooling using the usual low molecular weight standards due to the common phenomenon of supercooling. Therefore, a temperature calibration method needed to be developed for cooling DSC experiments utilizing high purity liquid crystals using the isotropic → nematic, the isotropic → cholesteric, and other liquid crystal → liquid crystal transitions. After the cooling calibration was accomplished, the cooling glass transition experiments indicated that the glass transition in semicrystalline polymers is not completely time independent, because its width depends on the ramp rate. However, it was shown that the time dependence is drastically reduced, and the midpoint of the glass transition seems to be constant which can explain the absence of the enthalpy relaxation. The work presented here has led to a number of studies showing the universality of the rigid amorphous phase for semicrystalline polymers as well as an ASTM standard for DSC cooling calibration.
Abstract
A simple technique using a combination of cation exchange and solid phase extraction chromatographic resins has been developed for the separation of99Tc from other radionuclides present in nuclear fuel leachates. Quantification of the isolated99Tc is accomplished using liquid scintillation counting. The method provides consistently high recoveries (>96%), generates small amounts of waste compared to classical methods, and requires less analysis time.
Abstract
Energy dispersive X-ray fluorescence spectroscopy (EDXRF) has been used for elemental analysis of Cu−Ni alloy, neodymium aluminide, and iron and nickel powder. The preparation of Cu−Ni alloy and neodymium aluminide has been carried out by aluminothermic reduction of mixed oxides of copper and nickel and neodymium oxide respectively. Aqueous electrorefining technique has been followed for the preparation of iron and nickel powder using Fe−Ni alloy as anode. The determination of major and trace elements present in the Cu−Ni and, electrolytically refined nickel and iron has been accomplished by EDXRF using Cd109 radioisotope source. In the case of Nd−Al alloy Am241 radioisotope source has been used. The rapid and multielement analysis of the thermit product by EDXRF has aided in the appropriate variation of the charge constituents during the standardization of the optimum charge composition for Cu−Ni alloy. EDXRF analysis of electrolytically refined nickel and iron revealed heavy contamination of iron in nickel as compared to that of nickel in iron. Neodymium content has been found to be 67.68% in Nd−Al alloy.
Kinetic studies on the effect of metal oxide catalysts, (25% w/w) such as Cr2O3, CuO, MnO2, Al2O3 and TiO2, on the thermal decomposition of KBrO3 have been carried out. The kinetic parameters of the catalysed and uncatalysed decompositions were calculated by the Freeman-Carroll, Coats-Redfern and Horowitz-Metzger methods. It has been found that Al2O3 is almost as good a catalyst as any other oxide used unlike in the thermal decomposition of KClO3. In the case of TiO2 there was an increase in the activation energy of decomposition. Of the other oxides Cr2O3 underwent reaction and was converted to dichromate and so the parameters of the reaction were not calculated. The effect of varying amounts of Al2O3 on the thermal decomposition was also studied.
This paper reviews the use of thin-layer chromatography (TLC) for the analysis of neutral lipids and phospholipids in medically and economically important snails (gastropod molluscs). It updates and fills in unintentionally neglected papers from earlier reviews on this topic published in 1990 and 2006 in this journal, and extends coverage to lipophilic pigments for the first time. The review discusses all steps of the TLC procedure, including sample preparation, sample and standard application, layers and mobile phases, detection of zones, and quantification. Significant findings on the effects of temperature, larval parasitism, diet, and environmental changes on the lipid and lipophilic pigment content in the snails as determined by TLC as well as the results of other miscellaneous studies and advantages and future prospects are presented.
Abstract
Analysis by Energy Dispersive X-ray Fluorescence spectroscopy of monazite ores from Kerala /Chavara and Manavalakurichi/, Orissa /Chattrapur/ and Tamil Nadu /Tirunelveli/ has been carried out for the determination of their elemental composition using109Cd /annular/ and241Am /disc/ radioisotope sources. The elements Y, Zr, Mo, Pb, Th and U were analyzed using a109Cd source, and the elements La, Ce, Pr, Nd, Sm, Gd and Dy were analyzed using the241Am source in side source geometry. Quntitative results on these 13 elements present in these ores were obtained by the EDXRF technique. It was seen that despite the diverse geological settings, there is remarkable similarity in the elemental composition of these ores, although some trace elements do show certain variations from sample to sample. These results are presented and discussed in this paper.
