Inter-laboratory exercise with an aim to compare methods for 90Sr and 239,240Pu determination in environmental soil samples

In order to deliver reliable results for a multitude of different scenarios, e.g. emergency preparedness, environmental monitoring, nuclear decommissioning and waste management, there is a constant process of method development in the field of radioanalytical chemistry. This work presents the results of a method comparison exercise aimed at quantifying ⁹⁰Sr and ^239,240Pu in environmental soil samples, with the intention of evaluating the performance and applicability of different methods. From the methods examined in this work, recommendations are given in order to find a radioanalytical measurement procedure, for ⁹⁰Sr and ^239,240Pu analysis, which is fit-for-purpose for a particular scenario.

     

Degradation effects in the extraction of antioxidants from birch bark using water at elevated temperature and pressure

Experiments with birch bark samples have been carried to enable a distinction between extraction and degradation effects during pressurised hot water extraction. Two samples, E80 and E180, contained birch bark extracts obtained after extraction at 80 and 180 °C for up to 45 min, respectively. Two other samples, P80 and P180, were only extracted for 5 min at the two temperatures and were thereafter filtered and hydrothermally treated at 80 and 180 °C, respectively. During the latter treatment, samples were collected at different times to assess the stability of the extracted compounds. An offline DPPH (2,2-diphenyl-1-picrylhydrazyl) assay, as well as a high performance liquid chromatographic separation coupled to an electrochemical detector, were used to determine the antioxidant capacity of the processed samples. The results obtained with the different techniques were compared to assess the yield of the extraction and degradation processes. In addition, an online hyphenated system comprising high performance liquid chromatography coupled to diode-array; electrochemical; and tandem mass spectrometric detection (HPLC-DAD-ECD-MS/MS) was used to study the compositions of the extracts in more detail. The results for the samples processed at 80 °C showed that the extraction reached a steady-state already after 5 min, and that the extracted compounds were stable throughout the entire extraction process. Processing at 180 °C, on the other hand, gave rise to partly degraded extracts with a multitude of peaks in both the diode array and electrochemical detectors, and a higher antioxidant capacity compared to for the extracts obtained at 80 °C. It is concluded that HPLC-DAD-ECD is a more appropriate technique for the determination of antioxidants than the DPPH assay. The mass spectrometric results indicate that one of the extracted antioxidants, catechin, was isomerised to its diastereoisomers; (+)-catechin, (−)-catechin, (+)-epicatechin, and (−)-epicatechin.     

Unexpected Isolation of 4‐Isothiocyanatomethylene‐4H‐pyridine‐1‐carboxylic Acid Ethyl Ester as Potential Template in Organic Synthesis

The synthesis of 4‐isothiocyanatomethyl‐pyridine 4 in 36% yield by Hasegawa and Kotani (Japanese patent 49088878, 1974) has spurred us to investigate this preparation in detail. In addition to this compound, 4‐isothiocyanatomethylene‐4H‐pyridine‐1‐carboxylic acid ethyl ester 3 can be isolated. The synthesis of both compounds 3 and 4 were optimized to 75% and 50% yield respectively. Reaction of compound 3 with methylamine gave thiourea derivatives 5, the same product obtained on reacting 4‐isothiocyanatomethyl‐pyridine 4 with methylamine. We succeed in adjusting the reaction conditions to obtain high yield either from compound 3 or isothiocyanate derivatives 4.     

INTERACTIONS BETWEEN POLY(ETHYLENE OXIDE) COATED SURFACES AND BETWEEN SUCH SURFACES AND PROTEINS

Surfaces coated with poly(ethylene oxide) containing nonionic polymers are of interest in medical applications due to, among other things, the low adsorption of proteins on such surfaces. In this paper we have studied the interfacial properties of surfaces coated with PEO by measuring the forces acting between two such surfaces in water and across a protein solution as well as between one such surface and a surface carrying adsorbed proteins. One type of surface coating was a graft copolymer of poly(ethylene imine) and poly(ethylene oxide) where the cationic poly(ethylene imine) group anchored the polymer to negatively charged mica surfaces. Three different ways to prepare this coating was used and compared. It was found that this coating was not stable in the presence of lysozyme, a small positively charged protein, when the PEO graft density was low. The other type of coating was obtained by adsorbing ethyl(hydroxyethyl)-cellulose onto hydrophobised mica surfaces. The driving force for adsorption is in this case the hydrophobic interaction between nonpolar segments of the polymer and the surface. The EHEC coating was stable in the presence of lysozyme and the interactions between adsorbed layers of lysozyme and EHEC coated surfaces are purely repulsive due to long-range steric forces.     

Orthoconic antiferroelectric liquid crystals

The ubiquitous liquid crystal display (LCD) is based on nematic liquid crystals (LCs) and has during 40 years developed from simple few digit displays into high-resolution flat-panel displays. A last and very important step towards the present TVs was the combination with thin film transistors that also led to the introduction of several new switching modes. Despite the enormous success of this technology, there is presently a renewed interest in LCs with faster electrooptic response, especially for future 3D vision display systems and possibly for field-sequential-colour (FSC) generation displays. Here, I focus on the so-called orthoconic antiferroelectric LCs (OAFLCs), which can provide the fast switching of conventional antiferroelectric LCs, but combined with a potentially much higher optical contrast. The reason is that the dark state of orthconic materials has a homeotropic optic axis, which makes the extinction ideally complete between crossed polarisers and independent of in-plane alignment fluctuations characteristic of all antiferroelectric LCs. The basic features and device physics issues of orthoconic LCs are reviewed and the most important remaining challenges to be met in terms of materials development are discussed in this article. Furthermore, a few examples of new applications made possible with the use of present and future orthoconic materials are given.     

An Unusual Cyclic System: Derivatives of N-Acetyl [2-Deoxy-β-D-Mannopyranosid]Urono-6,2-Lactam

ABSTRACT

Syntheses are described of a new ring system, namely derivatives of N-acetyl [2-deoxy-β-D-mannopyranosid]urono-6,2-lactam. These were formed by participation of a 2-acetamido-2-deoxy group in the oxidation using pyridinium dichromate of a 6-hydroxyl group in a mannopyranosidic system The structures of the new compounds were determined mainly by NMR experiments inter alia by HMBC techniques.