Progress in near-field photothermal infra-red microspectroscopy

Near‐field photothermal Fourier transform infra‐red microspectroscopy, which utilizes atomic force microscopy (AFM)‐type temperature sensors, is being developed with the aim of achieving a spatial resolution higher than the diffraction limit. Here we report on a new implementation of the technique. Sensitivity of the technique is assessed by recording infra‐red spectra from small quantities of analytes and thin films. A photothermomechanical approach, which utilizes conventional AFM probes as temperature sensors, is also discussed based on preliminary results. Early indication suggests that the photothermal approach is more sensitive than the thermomechanical one.     

两种在用发动机油氧化衰变情况监控方法对比分析

分析了两种常用监控在用发动机油氧化衰变情况的试验方法，并通过监控试验数据，探讨酸值和红外两种监测方法的各自特点，提出高档发动机油酸值变化极限值应区别于中低档发动机油的观点，为今后监控在用发动机油选用合适的试验方法和标准提供了参考。     

Electrochemical,FTIR and morphological study of polypyrrole—Polystyrenesulphonate conducting films

The electrochemical behaviour, FTIR spectrum and the morphology of polypyrrole-polystyrenesulphonate (PPy-PSS) films obtained potentiostatically at 0.6 V in a 0.05m Py + 1.7 × 10^?2m NaPSS medium have been analysed. Different electrochemical parameters have been modified in order to establish the first polaron formation, the reversibility of the redox process and the doping mechanism. The FTIR spectrum confirms the existence of C?O groups in the film structure and two possible explanations are suggested. SEM reveals a higher homogeneity in these films than in PPy films doped with smaller counterions.     

Microplastic and other anthropogenic microparticles in water and sediments of Lake Simcoe

Microplastics (plastic particles <5 mm in size) have been reported in ecosystems worldwide and have been shown to cause adverse negative impacts on organisms. This study provides the first report of microplastics and other anthropogenic microparticles in the surface waters and sediments of Lake Simcoe in Ontario, Canada, a popular recreational and fishing lake. Surface waters (low volume grabs and manta trawls) and sediments were sampled from eight sites to determine microparticle abundances and character (size, morphology, material identity). Concentrations ranged from 0 to 0.7 particles/L in surface water grab samples, 0.4–1.3 particles/m³ in manta trawl samples, and 8.3–1070 particles/kg in sediment samples. Spectroscopic analysis confirmed that 72% of particles were anthropogenic, with 64% unambiguously identified as microplastics. However, confirmed microplastic concentrations were approximately 6–7 times lower than unadjusted counts in sediments, demonstrating the importance of verifying and adjusting reported values. Fibers were only quantified and characterized in surface water grab samples and sediments, and were the most common morphology, accounting for 82% and 89% of anthropogenic particles, respectively. Fragments were most common in manta trawl samples (75%, excluding fibers) and consisted predominantly of polyethylene (41%) and polypropylene (22%). The influence of proximity to urban centers and prevailing winds on the distribution of microplastics was apparent in surface water manta trawls. Microplastics and other anthropogenic microparticles are present in Lake Simcoe but at lower abundances than at locations impacted by larger population centers in other large freshwater lakes such as Lakes Ontario and Erie of the Great Lakes.     

"牺牲"阳极法合成乙醇钽研究

研究了“牺牲“阳极法电化学合成乙醇钽过程中,添加剂种类与浓度、电解液温度、阴阳极极距和电流密度的影响.选取最佳合成条件为:四甲基氯化铵0.04 mol/L,温度为电解液的沸腾温度,极距约2 cm,电流密度220 A/m2.电合成的混合液经常压蒸馏和减压蒸馏,得到产品用红外光谱、拉曼光谱和元素分析进行表征,确定了产品为乙醇钽.电合成的电流效率大于95%,产品蒸馏时钽的直收率82.8%.     

Effect of laser fluences on the structure of carbon nitride films deposited by direct current plasma assisted pulsed laser ablation

Carbon nitride films were deposited by direct current plasma assisted pulsed laser ablation of a graphite target under a nitrogen atmosphere at room temperature. The surface morphology, composition and bonding structure of the deposited films were characterized by atomic force microscopy (AFM), Fourier transform infrared (FTIR) spectroscopy, Raman, and X-ray photoelectron spectroscopy (XPS). The effect of laser fluences in the range 0.5–3 J/cm² on the surface morphology, composition and bonding structure of the carbon nitride films were systematically studied. As laser fluence is increased, AFM results show a great decrease in the surface roughness of carbon nitride films. FTIR and XPS results indicate an increase in the N/C ratio and the content of N atoms bonded to sp³ C, as well as a decrease in the content of H atoms and the content of N atoms boned to sp² C in the deposited films, and Raman spectra indicate an increase in the content of disordered sp² C atoms and the sp² cluster size. The increase in the film density and the decrease in the particle fraction contribute to the decrease of surface roughness with increasing laser fluence.     

FTIR estimation of free fatty acid content in crude oils extracted from damaged soybeans

A user-interactive computer-assisted Fourier transform infrared (FTIR) method has been developed for estimation of free fatty acids (FFA) in vegetable oil samples by deconvolution of the infrared (IR) absorbances corresponding to the triglyceride ester and FFA carbonyl bonds. Peak areas were used to determine FFA as a percentage of the total carbonyl areas in weighed standards of refined, bleached, deodorized soybean oil containing from 0 to 5% added oleic acid. These data for percent FFA by FTIR were compared to corresponding FFA data obtained by two titration methods-the AOCS Official Method Ca 5a-40 and the Official Method with a slight modification. Correlation coefficients were 0.999 for the Ca 5a-40, 0.999 for the modified and 0.989 for the FTIR methods. FFA in samples of crude soybean oils extracted from damaged beans (0.5 to 2.1% FFA) were measured by FTIR and compared to data obtained by titration of the same samples (correlation coefficient, 0.869). To whom correspondence should be addressed at National Center for Agricultural Utilization Research, Agriculture Research Service, U.S. Department of Agriculture, 1815 North University Street, Peoria, IL 61604. ¹The mention of firm names or trade products does not imply that they are endorsed or recommended by the U.S. Department of Agriculture over other firms or similar products not mentioned.     

Hydroxyls nests in defective silicalites and strained structures derived upon dehydroxylation: vibrational properties and theoretical modelling

Defective silicalite, an efficient and selective catalyst in the gas phase Beckmann rearrangement reaction, has been characterised by infrared spectroscopy and by molecular modelling techniques. We report a detailed IR study on the effect of outgassing treatments at increasing temperature on silanols bands and on framework modes. The effect of a temperature decrease up to 100 K (during the IR measurement) on the H-bonding interactions has also been investigated. The interaction of silanols with mesitylene, a probe molecule which cannot penetrate the channels, has been studied in order to distinguish between internal and external OH groups. Molecular mechanics and ab initio methods have also been used to model the structure and the vibrational features of a properly designed nest in order to support the assignments of the IR spectrum.     

Coloring effect of the organic hybrid of polyamide 6 and N,N′‐ethylene‐bis(tetrabromophthalimide)

Coloring study in organic hybrid of polyamide (PA6) and N,N′‐ethylene‐bis(tetrabromophthalimide) (EPT), where the chromophore was self‐assembled by hydrogen bonding formed between PA6 molecular chains and EPT compound, have been characterized by several techniques. CS930 double wavelength lamella scanner was employed to measure the change of color. The existence of hydrogen bonding in PA6/N‐N′‐ethylene‐bis (tetrabromophthalimide) (PA6EPT) was investigated with Fourier transform infrared (FTIR), the results of which were compared with that of PA6 with the same thermal history. FTIR spectra at room temperature revealed that there is essentially hydrogen bonding between PA6 and EPT. The crystallization behavior of PA6EPT affected by hydrogen bonding was studied by using FTIR. The temperature‐dependent behavior of both PA6 and PA6EPT was studied by temperature‐FTIR spectroscopy and differential scanning calorimetry (DSC). With temperature increasing, changes in sensitive, high‐resolution absorbance spectra are observed as dissolve‐volatilizing thin film. Temperature‐FTIR results showed that the hydrogen bonding in PA6EPT attenuated and dissociated considerably at a smaller rate than PA6, that is to say, hydrogen bonding in PA6EPT is more stable than that in PA6. DSC showed that the melting temperature of PA6EPT and PA6 are similar. However, the crystalline degree and crystalline temperature and melting enthalpy of PA6 and PA6EPT are different. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 104: 594–600, 2007     

Structural changes and mechanical performance of recycled poly(vinyl chloride) bottles exposed to ultraviolet light at 313 nm

The structural changes and mechanical performance of virgin poly(vinyl chloride) (PVC) bottle (VB) compounds blended with postconsumer PVC bottles collected from a specified factory (RB‐F) and houses (RB‐H), were examined before and after UV irradiation at 313‐nm UV wavelength for different periods of time up to 28 days. The results indicated that, when exposed to UV light, the RB‐F/VB blends containing greater conjugated double bonds with higher yellowness index appeared to exhibit better mechanical performance than that of the RB‐H/VB blends. It was found that the amount of conjugated double bonds was not a linear function of the discoloration level of PVC compounds. Tensile strength of the VB compounds was not affected when incorporated with RB‐F recyclate, but progressively decreased with increasing RB‐H recyclate. An optimum concentration for RB recyclates to be added into the virgin compound was recommended for obtaining a maximum impact strength. Both tensile and impact strengths decreased with increasing UV exposure time, a severe degradation being obvious after a UV exposure time of 21 days. Hardness was not affected significantly by the addition of PVC recyclate, but increased with increasing UV exposure time. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 92: 84–94, 2004