CS2 extraction and FTIR & GC/MS analysis of a Chinese brown coal

The abundance of low-rank coals in China, such as bituminous and brown coals, makes studies of their composition and structure of great significance to both coal chemistry research and for efficient utilization of the coal. We describe how a Chinese brown coal was ultrasonically extracted with carbon disulfide (CS2) and the raw and extracted coals were characterized by Fourier Transform Infrared Spectroscopy (FTIR). The corresponding extract was analyzed with a coupled gas chromatograph mass spectrometer (GC/MS). The FTIR analysis shows a great abundance of amidocyanogen, carbonyl, aromatic and hetero aromatic rings and single carbon-heteroatom bonds. This suggests the possible occurrence of compounds like alcohols, phenols, amines, esters, carboxylic acids, ethers, aromatics or heteroaromatics. The GC/MS analysis of the CS2 extract detected 62 compounds, among which the non-polar ones were of lower abundance while the polar ones were in higher abundance and were structurally diverse. This demonstrates the compositional and structural complexity of Shengli coal.     

介质阻挡放电对RTV涂料憎水性的影响

室温硫化硅橡胶（RTV）材料的憎水性消失与恢复性能是表征该材料特性的重要指标,传统方法是利用长时间水浸泡或电晕放电使RTV材料的憎水性消失,此试验利用介质阻挡放电设备,分析了介质阻挡放电对RTV材料性能的影响。傅氏转换红外线（FTIR）图谱等分析结果表明：介质阻挡放电使RTV憎水性消失的本质是放电破坏涂料内部的有机官能团,产生亲水性基团。试验研究表明：放电处理时间越长,放电输出电压越大,放电输出频率越高,涂料憎水性消失越快。在此基础上,使用介质阻挡放电处理不同配方的RTV试品,然后观测其憎水性恢复过程,测量结果表明RTV涂料配方中生胶的分子基团越小,甲基硅油的质量分数越大,其憎水恢复性越好。     

ARMOS纤维的紫外老化

通过氙灯辐照试验对ARMOS纤维进行了紫外老化试验,采用单丝拉伸、FTIR、SEM和XRD研究了紫外光辐照对ARMOS纤维的影响。结果表明,短时间的紫外光辐照引起ARMOS纤维的拉伸强度在辐照6h后上升了13.7%,36h后又下降了2.1%。利用FTIR、SEM和XRD发现,经过紫外光辐照后,ARMOS纤维中酰胺基团的C—N键发生了断裂,同时氢键缔合能力增强,纤维结晶度增加,从而导致纤维表面出现沟槽,断口方式由微纤劈裂转向脆性断裂,说明短时间的紫外辐照对ARMOS纤维有削弱和强化2种相互矛盾的影响作用。     

Vinyl ester/clay based nanocomposites: a complementary study of vinyl ester polymerization by hyphenated rheo‐Fourier transform infrared and separate rheology/Fourier transform infrared measurements

This work is focused on the complementary information obtained from advanced in situ Fourier transform infrared (FTIR) spectroscopy and rheological measurements to correlate the structural changes with rheological properties upon polymerization of different organically modified montmorillonite clay/vinyl ester composites prepared by in situ polymerization. The microstructure and morphology of the nanocomposites were examined by X‐ray diffraction and transmission electron microscopy. The effect exerted by the presence of organic clay on the polymerization reaction of a vinyl ester based polymer matrix was evaluated. In situ and ex situ rheo‐FTIR measurements were compared to demonstrate the accuracy of this technique. © 2013 Society of Chemical Industry     

Ethyl group as matrix modifier and inducer of ordered domains in hybrid xerogels synthesised in acidic media using ethyltriethoxysilane (ETEOS) and tetraethoxysilane (TEOS) as precursors

Hybrid silica xerogels favourably combine the properties of organic and inorganic components in one material; consequently these materials are useful for multiple applications. The versatility and mild synthetic conditions provided by the sol-gel process are ideal for the synthesis of hybrid materials. The specific aims of this study were to synthesise hybrid xerogels in acidic media using tetraethoxysilane (TEOS) and ethyltriethoxysilane (ETEOS) as silica precursors, and to assess the role of the ethyl group as a matrix modifier and inducer of ordered domains in xerogels. All xerogels were synthesised at pH 4.5, at 60 °C, with 1:4.75:5.5 TEOS:EtOH:H₂O molar ratio. Gelation time exponentially increased with the ETEOS molar ratio. Incorporation of the ethyl groups into the structure of xerogels reduced cross-linking, increased the average siloxane bond length, and promoted the formation of ordered domains. As a result, a transition from Qⁿ to Tⁿ signals detected in the ²⁹Si NMR spectra, the Si–O structural band in the FTIR spectra shifted to lower wavelength, and a new peak in the XRD pattern at 2θ < 10° appeared in the XRD patterns. Mass spectroscopy detected fragments with high numbers of silicon atoms and a polymeric distribution.     

Experimental investigation and numerical modelling of the fire performance for epoxy resin carbon fibre composites of variable thicknesses

This paper applies a unique integrated approach to determine the flammability properties of a composite material (epoxy with carbon fibre) and compares its fire behaviour at two different thicknesses (2.1 and 4.2 mm) by performing small scale (thermo‐gravimetric analysis (TGA)/Fourier transform infrared radiation) and meso‐scale tests (cone calorimeter). For small‐scale tests, experiments were conducted in nitrogen using TGA coupled to gas analysis by Fourier transform infrared radiation. These results allow the determination of thermal stability, main degradation temperature and main gaseous emissions released during the thermal degradation. For meso‐scale tests, experiments were carried out using a cone calorimeter with sample dimensions of 100 × 100 mm at five heat fluxes (30, 40, 50, 60 and 70 kW/m²). The results show that the ignition time increases with an increase in the thickness of the material. Relative hazard classification of the fire performance of the current composites has also been compared with other materials using parameters obtained elsewhere. In addition, the effective ignition, thermal and pyrolysis properties obtained from the ignition and mass loss rate experiments for the 4.2‐mm thick samples were used in a numerical model for pyrolysis to predict well ignition times, back‐surface temperatures and mass pyrolysis rates for all heat fluxes as well as for the 2.1‐mm thick samples. Note that the ignition temperature obtained in the cone agrees with the main degradation temperature in the TGA. The flammability properties deduced here can be used to predict the heat release rate for real fire situations using CFD modelling. Copyright © 2016 John Wiley & Sons, Ltd.     

Physicochemical Characterization of Interaction of Ibuprofen by Solid-State Milling with Aluminum Hydroxide

This present study is a preliminary exploration of the affinity between a carboxylic model drug ibuprofen and aluminum hydroxide. Ibuprofen was comilled with aluminum hydroxide in different weight ratios in the solid state and was characterized by scanning electron microscopy (SEM), X-ray powder diffractometry (XRD), Fourier transform infrared spectroscopy (FTIR), and in vitro dissolution studies. XRD and SEM studies indicated complete interaction of ibuprofen with aluminum hydroxide and complete amorphization of aluminum hydroxide–ibuprofen complexed salt as well, on comilling with aluminum hydroxide at 1:2 ratio. FTIR data showed the disappearance of acid carbonyl peak with the appearance and the corresponding increase in absorbance of new signal at 1,682 cm^?1 in the 1:1 and 1:2 ibuprofen–aluminum hydroxide-comilled powder. The accompanied increase in the absorbance of carboxylate peak in the ibuprofen–aluminum hydroxide physical mixture, and 1:0.1, 1:0.5, 1:1, and 1:2 (IBA_pm, and IB₁A_0.1, IB₁A_0.5, IB₁A₁, and IB₁A₂, respectively) comilled powder indicated an acid–base reaction between ibuprofen and aluminum hydroxide. On storage at 40°C and 75% relative humidity (RH) for 10 weeks, XRD study showed the absence of reversion to the crystalline state and FTIR data revealed continued increase of new signal at 1,682 cm^?1 relative to carboxylic acid peak and no reappearance of carboxylic acid peak. In vitro dissolution studies revealed that the percent release of ibuprofen from the aluminum hydroxide-comilled powder is in the following order: IB₁A₂ < IB₁A₁ < ibuprofen crystal < ibuprofen milled alone < IB₁A_0.1 < IB₁A_0.5. Aluminum metal cation might have interacted to form a complex through the carboxyl and carbonyl groups of ibuprofen. Improved dissolution of drug associated with IB₁A_0.1 and IB₁A_0.5 is because of the absence of a new signal at 1,682 cm^?1 and improved amorphization of the drug to some extent. Dissolution of drug affected in IB₁A₂ and IB₁A₁ may be because of the insoluble stable complex formation.     

Functional properties of sonicated and non-sonicated extracted leaf protein concentrate from Diplazium esculentum

Leaf protein concentrate of edible fern Diplazium esculentum was extracted using sonication and non-sonication methods and its functional properties were evaluated. The leaf protein concentrate contained 34.28 and 9.89% protein for sonicated and non-sonicated extractions, respectively. Sonication yielded (36.36%) better emulsion activity over non-sonication (31.10%). Foaming capacity was also found better in sonication (7.27%) over non-sonication (6.99%), and oil absorption capacity also improved in sonication (7.55 g of oil/g) over its counterpart (7.41 g of oil/g). Contact angle experiments with the leaf protein concentrate evidenced the enhancement of more hydrophilicity of the sonicated sample. Thermal properties of the leaf protein concentrate with sonication evidenced more stability (55.58 and 95.95°C) over the non-sonicated (46.75 and 75.60°C). Fourier transform infrared spectral analysis with the leaf protein concentrate of Diplazium esculentum was used to assess the secondary structural data such as α-helix and β-sheets. The various percentages of secondary structures of protein in sonicated and non-sonicated samples were 49.06 and 69.16% for α-helix, 33.59% and 17.02% for β-sheet and 42.02 and 35.68% for turn, respectively. The results of the present investigation showed credible evidence to support that sonication method of extraction of leaf protein concentrate was better in terms of protein yield and functional properties as compared to the non-sonication. The sonicated extracted leaf protein concentrate has the potential for developing value added products.     

Influence of Al2O3 on the electrical conductivity and structure of calcium-silicate-based melts

Electrical conductivity and structure of the CaO-SiO₂-based mold flux melts with various Al₂O₃ contents were investigated. The results show that the electrical conductivity increases with the addition of Al₂O₃ from 2 wt% to 4 wt%, but decreases with the further increase of Al₂O₃ from 4 wt% to 8 wt%. Correspondingly, the apparent activation energy reduces firstly from 55.12 ± 1.20 kJ mol to 41.09± 0.38 kJ mol, and then increases from 41.09 ± 0.38 kJ mol to 98.99 ± 1.42 kJ mol. The structure analyses suggest that complex structural units, such as Si-O-Al, Al-O⁰, Si-O-Si and Q³(Si), reduce first, but increase with the further addition of Al₂O₃. Conversely, these simple structural units, such as Al-O^-, Q⁰(Si), Q¹(Si) and Q²(Si) vary in the opposite way with the change of Al₂O₃ content. From the variations of electrical conductivity, activation energy and structural units, it can be found that when Al₂O₃ works as network breaker to simplify the melt structure, the energy barrier for transportation of conducting ions/ionic reduce, which results in the increase of electrical conductivity; while when Al₂O₃ becomes into network former, the conductivity increases, correspondingly.