Time dependent crystal-smectic transformation in perylene-containing polyimides

The crystalline conformations of perylene polyimides (PPIs), with alkyl spacers varying in length from C₃ to C₁₂ are discussed. Although modeling of single chains would suggest the possibility that those with odd number of CH₂ groups adopt a flat helical shape, X-ray diffraction suggests that the chains with odd and even spacers have the same conformation, due to the necessity to pack the perylene units. Upon annealing, the UV-vis absorption maximum red-shifts by about 10 nm, indicating enhanced π-stacking between the perylenes. Several changes in the spectra are seen with an increase in annealing time, at a given temperature. With an increase in annealing time, X-ray diffraction patterns show changes in the number of reflections, indicative of a crystal to mesogenic transition. The time required for this transition increases with a decrease in the spacer length, and annealing temperature, suggesting that the dynamics of this transition is very slow.     

Life cycle of hydroprocessing catalysts and total catalyst management

Hydroprocessing catalysts based on Ni, Co, Mo and W are used in various refinery processing applications where several deactivation mechanisms become of importance (coke formation, active phase sintering, metals deposition, poisoning) in the catalyst's life cycle. The life cycle of commercial hydroprocessing catalysts is very complex and includes the catalyst production, sulfidation, use, oxidative regeneration followed by re-sulfidation and reuse or, if reuse is not possible, recycling or disposal. To understand the changes in catalyst properties taking place during a life cycle, the catalyst quality in the different stages can be best monitored by using advanced analytical techniques. The catalyst's life cycle is further complicated by numerous technical, environmental and organizational issues involved. In principle, different companies can be involved in each of the life cycle steps. Leading catalyst manufacturers, together with specialized firms, offer refineries a total catalyst management concept, starting with the purchase of the fresh catalyst and ending with its final recycling or disposal. Total catalyst management includes a broad range of services, ensuring optimal timing during the change-out process, reliable, smooth and safe operations, minimal downtime and maximum catalyst and unit performance.     

A small-angle X-ray scattering study of powder compaction

This work demonstrated a novel and potentially important application of two-dimensional small-angle X-ray scattering (2D-SAXS) to investigate powder compaction. SAXS from powder compacts of three materials commonly used for pharmaceutical tabletting exhibited azimuthal variations, with stronger intensity in the direction of the applied compaction force, relative to the transverse direction. This implied that compaction of a (macroscopic) powder could also produce changes on the molecular (nanometre) scale, which can be probed by 2D-SAXS. Two possible explanations for this effect were suggested. A combination of anisometric (i.e. elongated or flattened) granules with anisotropic morphologies could result in azimuthal variation in X-ray scattering due to granule orientation. It is expected that this mechanism would require relatively low packing density, so may operate during die filling. Granule re-orientation appeared less likely at higher packing densities and compaction pressures, however. Under these conditions, the changes in the 2D-SAXS patterns would be consistent with the powder granules becoming relatively flattened in the compression direction, with corresponding changes in their nano-scale morphology. The magnitude of this effect was found to vary between the materials used and increased with compaction pressure. This suggested that 2D-SAXS studies could provide useful information on force-transmission within a compressed powder. Further analysis of the data also suggested differences in the compaction mechanisms (i.e. granule re-orientation, deformation or fragmentation) between the materials studied.     

An investigation into physicochemical characteristics of ash produced from combustion of oil palm biomass wastein a boiler

Ash derived from combustion of Malaysian oil palm biomass (empty fruit bunches consisting of fibers) was physically and chemically characterized in order to provide a comprehensive understanding of its specific properties in terms of toxicity, compositions and reusability. Principal analyses conducted include particle size distribution, scanning electron microscopy, elemental dispersive X-ray, elemental analysis, toxicity characteristic leaching procedure (TCLP) as well as thermogravimetric, X-ray diffractometry and Fourier-transform infrared analyses. TCLP result indicated that the oil palm ash (OPA) should not be classified as toxic wastes in terms of heavy metal leachability since leachable copper, cadmium, lead and nickel concentrations were detected below the stipulated leachability limits. It was determined that the OPA contained high amount of potassium as well as presence of silica which implied its suitability to be reused as crude fertilizer or cement replacement material.     

Structural properties of phosphorous-doped polycrystalline silicon

The structural properties and hydrogen bonding of undoped and phosphorous doped polycrystalline silicon produced by step-by-step laser dehydrogenation and crystallization technique were investigated using Raman spectroscopy and hydrogen effusion measurements. At low laser fluences, E_L, a two-layer system is created. This is accompanied by the change in hydrogen bonding. The intensity of the Si–H vibration mode at 2000 decreases faster than the one at 2100 cm⁻¹. This is even more pronounced in phosphorous-doped specimens. The laser crystallization results in an increase of the hydrogen binding energy by approximately 0.2–0.3 eV compared to the amorphous starting materials.     

Formation and electronic structure of interface

In the present work the formation of the interface between polycrystalline silver and thin films of titanium oxide was studied with photoelectron spectroscopy (XPS, UPS) and time-of-flight secondary ion mass spectrometry (TOF-SIMS). Titanium oxide was deposited stepwise on 100 nm thick silver films by reactive magnetron sputtering allowing to study the evolution of the interface formation process. The process involves two steps: formation of thin layer of silver oxide and subsequent growth of the TiO₂ film. For better understanding of the silver oxidation process, pure silver films were exposed to a low temperature Ar/O plasma for different time intervals providing a possibility to investigate early stages of the oxide film growth.     

基于复数主成分分析的磁共振波谱信号衰减系数的自动校正

衰减系数的校正是磁共振波谱信号处理和分析过程中的一个关键难题。本文基于复数主成分分析，提出了一种自动的磁共振波谱衰减系数的校正方法，较成功地解决了这个难点问题。文中的模拟数据及其实现结果充分验证了该方法的有效性。     

The effect of aluminium coating on elemental standards in X-ray microanalysis

The standardisation of frozen hydrated bulk biological specimens using gelatin standards is described. The relationship between corrected elemental X-ray counts and ionic concentration was found to be linear, and minimum detectable limits for each element are stated. Variations in uncorrected standard curves were found to be due to changes in aluminium coating thickness. There was an inverse relationship between coating thickness and elemental X-ray counts. The factors causing this are discussed. To avoid errors arising from inconsistent aluminium thickness, experimental material should only be compared with standards of similar aluminium net counts. This can be achieved most easily by mounting and analysing specimen and standard together.     

Synthesis of selenium nanoparticles in the presence of silk fibroin

This paper describes a solution-phase approach to the synthesis of selenium nanoparticles by reducing selenious acid solution with ascorbic acid in the presence of silk fibroin. The monodispersed spherical selenium colloid particles obtained were very stable in silk fibroin solution and characterized by Atomic force microscopy and X-ray techniques. The influences of temperature and ultrasonication on the morphology of selenium nanoparticles were also discussed. The experiments showed that the selenium nanoparticles with various morphologies could be obtained under different temperatures and the appropriate ultrasonication time was 60 min. This result indicated that the silk fibroin molecules intimately associated with the surface of the selenium particles and controlled the growth particles.     

A novel method for determination of polyester end-groups by NMR spectroscopy

An efficient, convenient and quantitative method for characterising polyester end-groups is described. We have found that trichloroacetyl isocyanate (TAI) reacts rapidly and quantitatively with both carboxyl [C(O)OH] and hydroxyl (OH) chain ends to form derivatives that can be readily determined by ¹H NMR spectroscopy. The TAI capped end-groups give rise to characteristic imidic NH resonances in a normally clear region of the ¹H NMR spectrum [δ∼10-11.5 for C(O)-O-C(O)-NH-C(O)CCl₃ from C(O)OH, δ∼8-9 for O-C(O)-NH-C(O)CCl₃ from OH]. The method has been successfully applied to quantitative determination of the end-groups of a wide variety of oligomeric polyesters. It has also been applied to higher molecular weight polyesters including commercial, bottle grade, poly(ethylene terephthalate) (PET) and PET based copolyesters (e.g. PETG).