Solubility of Natural Gas in Diesel Fuel

The solubility of commercially available natural gas in commercially available diesel fuel at room temperature and defined pressure is investigated experimentally. The gas phase is considered to be pure methane. The use of Henry's law to model the solubility is discussed. Solubility is given in terms of the mole fraction and the volumetric mass concentration of dissolved gas and the corresponding Henry's coefficients. The solubility is compared to that of pure methane in pure hexadecane, which is similar to diesel fuel with respect to the mean carbon number.     

Determination of nano-roughness of carbon fibers by atomic force microscopy

We present a novel approach to determine the surface roughness on varying scales using atomic force microscopy data. The key factor is to find a suitable background correction for the desired scale. Using the example of the surface of sized and unsized high-tenacity carbon fibers, we present an easy method to find backgrounds for widely varying scales and to evaluate respective topography and surface roughness with the same lateral resolution as the microscope itself. The analysis is done by subtracting a tunable background from the respective height data. By choosing an appropriate background to investigate the surface topography of a carbon fiber on a nm-scale, only small nano-structures with a width of around 20 nm remain after the background subtraction. Evaluating the mean roughness R _a of these nano-structures, sized carbon fibers show an overall value of around 0.1 nm while unsized carbon fibers a value of around 0.4 nm. Total background corrected height analysis shows an even distribution of these nano-structures along the fibrils of the unsized fibers, whereas for the sized fibers the nano-structures are not present. The presented method allows analysis and visualization of the distribution of nano-structures on a carbon fiber surface for the first time. This feature is used to visualize the distribution of the sizing and can further be used to investigate the influence of different production parameters on the fiber topography or to evaluate the contribution of mechanical interlocking to the interfacial strength.     

Solvent diffusion in silica/poly[styrene‐co‐(acrylic acid)] core‐shell microspheres by pulsed field gradient NMR techniques

Polymer‐coated SiO₂ particles are prepared by precipitation of poly[styrene‐co‐(acrylic acid)] on SiO₂ microspheres through an improved phase inversion method. The diffusion resistance of the polymer membrane was considered to be the critical reason for producing tailor‐made polyethylene by catalysts supported on these polymer‐coated particles. This paper employs pulsed field gradient NMR (PFG‐NMR) to distinguish diffusion of n‐hexane in different regimes, i.e., in the space between each particle, the pores in SiO₂ and the polymer shell, by their respective diffusion coefficients. By varying the observation time, the time scale of the molecular exchange is discussed. A three‐region ansatz was used to interpret the exchange and diffusion in polymer‐coated SiO₂ system, and was compared with results acquired with noncoated particles. At long diffusion times, the mean‐squared displacement, and thus the averaged self‐diffusion coefficient, of hexane in the system of polymer‐coated SiO₂ particles is significantly reduced. The PSA membrane is identified as an efficient barrier against molecular exchange between the pores in SiO₂ and the intraparticle space. Consistently, the relaxation measurements indicated that the mobility of n‐hexane molecules, especially the rotation of n‐hexane, was limited by the PSA membrane. © 2013 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 40160.     

4-Acyl-2-acylamino-4,5-dihydro-1,3,4-thiadiazole durch Acylierung von Thiosemicarbazonen

4-Acyl-2-acylamino-4,5-dihydro-1,3,4-thiadiazoles by Acylation of Thiosemicarbazones Thiosemicarbazones and acid anhydrides or halides react to 4-acyl-2-acylamino-4,5-dihydro-1,3,4-thiadiazoles ( 2a – 2v ) in high yields. 3-Acyl-2-amino-4,5-dihydro-1,3,4-thiadiazoles 5 are proved as intermediates in this conversion. In special cases they can be isolated or submitted to further acylation with an other acylating agent. ¹H-n.m.r., ¹³C-n.m.r. and mass spectroscopic data of compounds 2a – 2v and 5a – 5e are given. The preparation of the compounds 2 can also be carried out starting with a carbonyl compound and thiosemicarbazide without isolation of the thiosemicarbazone.     

N-Aminierung von Isochinolinbasen

N-Amination of Isoquinoline Bases 3, 3-Pentamethylene oxaziridine 1 forms an N N-bond with secondary isoquinoline bases 2a – f to give the cyclohexylidene hydrazines 3a – f . In some cases nitrogen elimination yielding indane derivatives 13b, 13e competes with hydrazone formation. The cyclic Schiff'base 14 and the β-carboline derivative 16 can also be aminated.