Effect of preparation conditions on the thermal stability of an epoxy-functional inorganic-organic hybrid material system doped with Zr

An inorganic-organic hybrid material system consisting of (3-glycidyloxypropyl)trimethoxysilane, dimethyldimethoxysilane and zirconium(IV) n-propoxide was prepared by the sol-gel method. The influence of processing parameters including Zr content, UV irradiation and sol ageing on the thermal stability of the resultant thin films was characterised by thermogravimetry. It was demonstrated that the crosslinking of epoxy groups in the structure was the primary reason for variation in the thermal stability of the system. As Zr and/or UV irradiation may be employed to crosslink the epoxy groups in the structure, the thermal stability of the system can be tuned by the optimal combination of these two crosslinking methods.     

Effect of preparation conditions on the thermal stability of an epoxy-functional inorganic-organic hybrid material system with phenyl side group

A hybrid material system consisting of (3-glycidyloxypropyl)trimethoxysilane and dimethyldimethoxysilane as matrix materials and diphenyldimethoxysilane (DPDMS) as both a matrix material and a potential thermal stabiliser by the sol-gel method. A detailed thermogravimetric analysis study of the influence of processing parameters, including DPDMS content, UV irradiation and sol ageing, on the thermal stability of the resultant thin films was presented. FT-IR spectroscopy was used to monitor the changes in the relative amount of epoxy rings in the system during processing. It was demonstrated that the crosslinking of epoxy groups in the structure is the primary reason for changes in the thermal stability of the system. It was also shown that the thermal stability, in terms of 10% mass loss, of the material system could be improved up to 280 °C, by adjusting the preparation conditions, compatible with several subsequent high temperature optoelectronic integration processes.     

Studies on the atom transfer radical polymerization of a maleimide AB* monomer and modification of the halogen end groups

The atom transfer radical polymerization (ATRP) of an AB* monomer, N-(4-α-bromobutyryloxy phenyl)maleimide (BBPMI), was conducted using the complex of CuBr/2,2′-bipyridine as catalyst. The study of kinetics of polymerization and the growth behavior of macromolecules show that the polymerization proceeds rapidly in first 1 h and then slows down. The decrease in the rate of polymerization is ascribed to the poor reactivity of maleimide radicals from A* to initiate the polymerization of maleimide double bonds. The molecular weight of the resulting polymer also increases with the dosage of catalyst. The coincidence of molecular weight determined by hydrogen proton nuclear magnetic resonance spectroscopy (¹H NMR) and gel permeation chromatography (GPC) proves that the resulting polymer is of linear structure, which is further verified by ¹³C NMR measurement and high performance liquid chromatography (HPLC) analysis of the hydrolysate of the resulting polymer. The stabilization modification of the halogen end groups of the resulting polymer by free-radical chain transfer reaction was attempted under ATRP condition. Isopropyl benzene was employed as the chain transfer agent. Indeed, the modified polymer with carbon-bromine bonds conversion of 40.7% shows enhanced thermal stability. The initial weight loss temperature has been increased from 193 to 243 °C. On the other hand, the atom transfer radical copolymerization of BBPMI with styrene resulted in the formation of hyperbranched polymer.     

The effect of phosphorus content on the thermal and the burning properties of cotton fabric coated with an ultrathin film of a phosphorus-containing polymer

The effect of phosphorus content on thermal degradation and burning behavior of poly(acryloyloxyethyl diethyl phosphate) or PADEP-coated cotton was studied. The results showed that PADEP-coated cotton prepared by admicellar polymerization using hexadecyltrimethylammonium bromide (HTAB) as a surfactant has higher amounts of phosphorus than that prepared using dodecyltrimethylammonium bromide (DTAB). Higher phosphorus content led to lower decomposition temperatures and greater amounts of char formation after thermal degradation. The effectiveness of the amount of phosphorus on the burning behavior of the treated cotton was investigated by an ASTM flammabilty test. In the case of PADEP-coated cotton prepared with DTAB, the flame spread slowly and extinguished with char formation on the fabric. For untreated cotton however, the flame spread quickly and burned the fabric entirely without char formation. Cotton coated with PADEP using HTAB exhibited self-extinguishing behavior after removing the ignition source. Decrease in decomposition temperature, increase in char formation and the burning behavior of PADEP-coated cotton are all consistent with phosphorus content on the treated fabric.     

Fructose determination using immobilized enzymes in a flow system with special emphasis on the effect of isomerism

A flow injection method for the determination of fructose has been developed using immobilized hexokinase, glucose phosphate isomerase and glucose-6-phosphate dehydrogenase. The produced NADH was monitored amperometrically with a graphite electrode modified by an adsorbed Nile-blue derivative. The response was linear from the detection limit, 1M to 3 mMD-fructose for a sample volume of 25l. Glucose, the only interfering substrate, was eliminated with a reactor containing immobilized glucose oxidase, mutarotase and catalase. The experiments indicate that hexokinase is selective for the-fructo-furanose isomer. The other isomers will spontaneously isomerize to-fructo-furanose with time, if the latter is consumed. The fructose response factor of an enzyme reactor or biosensor will therefore depend on the isomer distribution in the original sample solution. The effect of pH and temperature can be controlled, but complexing ligands like borate interfere in a complex way and should be absent.     

A simple strategy for determining ethanol in all types of alcoholic beverages based on its on-line liquid-liquid extraction with chloroform, using a flow injection system and Fourier transform infrared spectrometric detection in the mid-IR

In this work, a simple strategy for the determination of ethanol in all types of alcoholic beverages using Fourier transform infrared spectrometric detection has been developed. The methodological proposal includes the quantitative on-line liquid-liquid extraction of ethanol with chloroform, through a sandwich type cell equipped with a PTFE membrane, using a two-channel manifold; and direct measurement of the analyte in the organic phase, by means of Fourier transform infrared spectrometry. The quantification was carried out measuring the ethanol absorbance at 877 cm⁻¹_, corrected by means of a baseline established between 844 and 929 cm⁻¹. The procedure, which does not require any sample pretreatment (except for the simple degassing of beer and gassy wine samples, and a simple dilution of spirits with water), was applied to determine ethanol in different alcoholic beverages such as beers, wines and spirits. The results obtained highly agree with those obtained by a derivative FTIR spectrometric procedure, and by head space-gas chromatography with FID detection. The proposed method is simple, fast, precise and accurate. Moreover, it can be easily adapted to any infrared spectrometer equipped with a standard transmission IR cell, and provides attractive analytical features, which are comparable to, or better than those offered by other published methods. In consequence, it represents a valid alternative for the determination of ethanol in alcoholic beverages, and could be suitable for the routine control analysis.     

Ultra‐high performance liquid chromatography with linear ion trap‐Orbitrap hybrid mass spectrometry combined with a systematic strategy based on fragment ions for the rapid separation and characterization of components in Stellera chamaejasme extracts

Stellera chamaejasme, a famous toxic herb, has been used in traditional Chinese medicine to treat various diseases. For decades, increasing attention in modern pharmacological studies has been drawn to S. chamaejasme because of its potential anti‐tumor, anti‐virus, and anti‐fungus activities. However, due to the intrinsic complexity of chemical constitutes, hardly any investigations formed an overall recognition for the chemical profiles of this herb. In this study, a rapid and sensitive ultra‐high performance liquid chromatography coupled with linear ion trap‐Orbitrap mass spectrometry method was developed to characterize the chemical components of S. chamaejasme extracts. Based on optimized ultra‐high performance liquid chromatography and mass spectrometry conditions and systematic fragment ions‐based strategy, a total of 47 components including flavones, diterpenes, coumarins, and lignans were simultaneously detected and identified or tentatively identified for the first time. The MSⁿ fragmentation patterns of all the characterized compounds in positive or negative electrospray ionization modes were also explored and summarized. These results provided essential data for further pharmacological research on S. chamaejasme. Moreover, the method was demonstrated to be an efficient tool for rapid qualitative analysis of secondary metabolites from natural resources.