The analysis of organic matter in oil-shales

The organic matter in five oil shales (three from the Kimmeridge Clay sequence, one from the Oxford Clay sequence and one from the Julia Creek deposits in Australia) has been isolated by acid demineralisation, separated into kerogens and bitumens by solvent extraction and then characterised in some detail by chromatographic, spectroscopic and degradative techniques. Kerogens cannot be characterised as easily as bitumens because of their insolubility, and hence before any detailed molecular information can be obtained from them they must be degraded into lower molecular weight, more soluble components. Unfortunately, the determination of kerogen structures has all too often involved degradations that were far too harsh and which lead to destruction of much of the structural information. For this reason a number of milder more selective degradative procedures have been tested and used to probe the structure of kerogens. These are: 1. Lithium aluminium hydride reduction. - This procedure is commonly used to remove pyrite from kerogens and it may also increase their solubility by reduction of labile functional groups. Although reduction of the kerogens was confirmed, increases in solubility were correlated with pyrite content and not kerogen reduction. 2. O-methylation in the presence of a phase transfer catalyst. - By the removal of hydrogen bond interactions via O-methylation, it was possible to determine the contribution of such secondary interactions to the insolubility of the kerogens. Problems were encountered with the use of the phase transfer catalyst. 3. Stepwise alkaline potassium permanganate oxidation. - Significant kerogen dissolution was achieved using this procedure but uncontrolled oxidation of initial oxidation products proved to be a problem. A comparison with the peroxytrifluoroaceticacid oxidation of these kerogens was made. 4. Peroxytrifluoroacetic acid oxidation. - This was used because it preferentially degrades aromatic rings whilst leaving any benzylic positions intact. Considerable conversion of the kerogens into soluble products was achieved with this procedure. At all stages of degradation the products were fully characterised where possible using a variety of techniques including elemental analysis, solution state 1H and 13C nuclear magnetic resonance, solid state 13C nuclear magnetic resonance, gel-permeationchromatography, gas chromatography-mass spectroscopy, fourier transform infra-red spectroscopy and some ultra violet-visible spectroscopy.

Detection of organic aromatic compounds in paraffin by a long-period fiber grating optical sensor with optimized sensitivity

A long-period grating (LPG) sensor is used to detect small variations in the concentration of an organic aromatic compound (xylene) in a paraffin (heptane) solution. A new design procedure is adopted and demonstrated to maximize the sensitivity of LPG (wavelength shift for a change in the surrounding refractive index, (dλ/dn3)) for a given application. The detection method adopted is comparable to the standard technique used in industry (high performance liquid chromatograph and UV spectroscopy) which has a relative accuracy between ∼±0.5% and 5%. The minimum detectable change in volumetric concentration is 0.04% in a binary fluid with the detection system presented. This change of concentration relates to a change in refractive index of Δn ∼ 6 × 10-5. © 2001 Elsevier Science B.V.

A general one-pot strategy for the synthesis of high-performance transparent-conducting-oxide nanocrystal inks for all-solution-processed devices

For all-solution-processed (ASP) devices, transparent conducting oxide (TCO) nanocrystal (NC) inks are anticipated as the next-generation electrodes to replace both those synthesized by sputtering techniques and those consisting of rare metals, but a universal and one-pot method to prepare these inks is still lacking. A universal one-pot strategy is now described; through simply heating a mixture of metal-organic precursors a wide range of TCO NC inks, which can be assembled into high-performance electrodes for use in ASP optoelectronics, were synthesized. This method can be used for various oxide NC inks with yields as high as 10 g. The formed NCs are of high crystallinity, uniform morphology, monodispersity, and high ink stability and feature effective doping. Therefore, the inks can be readily assembled into films with a surface roughness of 1.6 nm. Typically, a sheet resistance of 110 Ω sq-1 can be achieved with a transmittance of 88%, which is the best performance for TCO NC ink-based electrodes described to date. These electrodes can thus drive a polymer light-emitting diode (PLED) with a luminance of 2200 cdm-2 at 100 mA cm-2.