Zinc Coated Steel/Epoxy Adhesive Systems: Investigation of the Interfacial Zone by FTIR Spectroscopy

The present study takes advantage of the ability of Fourier Transform Infrared Spectroscopy (FTIR) for the analysis of ultrathin organic films on metals. FTIR in the reflection mode (IRRAS) is used in order to study the interaction of ultrathin films of dicyandiamide (hardener of most one-pack epoxy resins) with various substrates, model ones such as gold or zinc and industrial ones such as steel and zinc-coated steels.

Pure zinc surfaces and, to a lesser extent, zinc-coated steels are shown to react with dicyandiamide after heating at 180°C, as evidenced by the frequency shift of the absorption band (at about 2200 cm^-1) characteristic for nitrile groups. As real systems consist of thick layers of a fully formulated adhesive cured onto a metallic substrate, the direct investigation of such a buried interphase is no longer possible by FTIR and by most of the known spectroscopies. Some mechanically tested specimens are then analysed, after failure, by FTIR microspectrometry. The spectra obtained, corresponding to the fracture initiation zone which is about 100 μm in diameter, advocate for the presence of an ultrathin layer of modified polymer still covering the substrate.     

固相萃取净化-气相色谱-质谱法测定染料中7种指示性多氯联苯

本文建立了以固相萃取(SPE)前处理净化、结合气相色谱-质谱(GC-MS)测定染料中7种指示性多氯联苯的分析方法。该法将染料样品经溶剂萃取后,通过固相萃取(SPE)净化、浓缩,气相色谱-质谱采用选择离子监测模式(SIM)测定,以保留时间和特征离子定性,外标法定量。     

Analysis of solvent extracts of bituminous coal macerals by chromatography, 1H n.m.r. and field-desorption mass spectrometry

Analysis of the carbon disulphide extracts of nine samples of UK coal-maceral concentrates by ¹H highresolution n.m.r. spectroscopy, gas-liquid chromatography and field-desorption mass spectrometry indicates the presence of components with a wide molecular weight range extending up to 1200 amu; these are attributed to n-alkanes up to ≈C₅₀ and highly condensed polynuclear aromatic compounds.     

Quantitation of volatile compounds in heated triolein by static headspace capillary gas chromatography/infrared spectroscopy-mass spectrometry

Static headspace and capillary gas chromatography/infrared spectroscopy-mass spectrometry were used to collect, separate, identify and quantitate the oxidative and thermal decomposition products in heated triolein. Approximately 4 L of triolein was heated in a deep-fat fryer at 190°C for 12 h each day for a total of 60 h, until it contained>-20% polymeric material. The concentration of heptane and octane increased after 12 h heating, then decreased upon further heating, while the concentration of volatile aldehydes decreased gradually during heating. After 12 h of heating, the concentrations of the major volatiles changed as follows: heptane (16.36 to 30.17 ppm), octane (24.48 to 40.77 ppm), heptanal (21.68 ppm to 9.11 ppm), octanal (35.53 to 36.64 ppm), nonanal (68.95 to 43.16 ppm), (E)-2-decenal (135.00 to 89.00 ppm) and (E)-2-undecenal (88.50 to 61.00 ppm). After 60 h of heating, when the oil contained over 20% polymeric material, the concentrations of heptane, octane, heptanal, octanol, nonanal, (E)-2-decenal and (E)-2-undecenal were 5.16, 4.39, 5.45, 7.02, 18.07, 12.50 and 6.00 ppm, respectively.     

日光照射对荧光增白剂VBL顺-反异构现象影响的研究

用紫外光谱和荧光光谱法对日光照射荧光增白剂VBL溶液进行了研究。结果表明、随日光照射时间的延长，VBL溶液在432nm处荧光强度下降；而在267nm处有所增强，低浓度溶液对日光照射更加敏感。1mg／1在避光时测得吸光度为0.449，而在日光照射15分钟后，其吸光度下降至0.141，证明日光照射使VBL溶液中的顺式异构体增加。     

应用质谱扫描测定胸腺肽相对分子质量

目的 精确测定胸腺肽相对分子质量分布。方法 采用质谱扫描法。结果 3批胸腺肽相对分子质量均在2000～4000,无10 000以上的大分子蛋白。结论 本方法灵敏度高,可直观地测定胸腺肽相对分子质量分布状况,为控制胸腺肽质量提供了新的检测方法。     

4-(α-吡啶甲酰基)-PMP的合成与谱学特性研究

合成了新吡唑啉酮类试剂1-苯基-3-甲基-4-(α-吡啶甲酰基)-吡唑啉-5-酮(简称4-(α-吡啶甲酰基)-PMP,下同)。在表征分子结构的同时,对其红外、紫外吸收光谱,核磁共振氢谱、碳谱,质谱等谱学特性和质谱裂解规律进行了分析与研究。     

Method for characterization of triacylglycerols and fat-soluble vitamins in edible oils and fats by supercritical fluid chromatography

This study demonstrates the usefulness of capillary supercritical fluid chromatography (SFC) for the characterization of triacylglycerols of edible oils and fats. Triacylglycerols were separated according to the acyl carbon number and the degree of unsaturation on a 25% cyanopropyl/25% phenyl/50% methylpolysiloxane stationary phase. Valuable information concerning the triacylglycerol composition of berry oils was obtained, despite the overlapping of certain triacylglycerol peaks. Simultaneous analysis of fat-soluble vitamins and triacylglycerols is not practical by capillary SFC with flame-ionization detection because of the low concentration of naturally-occurring fat-soluble vitamins in edible oils. Therefore, higher loading of the sample, which led to overloading of triacylglycerols, was required to get reasonable peaks for fat-soluble vitamins. The method was applied to the characterization of triacylglycerols and tocopherols in sea buckthorn pulp and seed oil, and cloudberry seed oil without any sample purification prior to SFC. In addition, the stationary phase proved useful for separating the more complex mixtures of triacylglycerols found in milk fat and in fish oil.