Phase Systems and Post-Column Dithizone Reaction Detection for the Analysis of Organo-Mercurials by HPLC

Abstract

The suitability of HPLC (normal and reversed phase adsorption) with UV or post-column reaction detection for the analysis of organomercurials was investigated systematically. The separation of organomercurials is best carried out on a reversed phase system with a C-8 bonded phase material as the stationary phase and acetonitrile-aqueous sodium bromide mixtures as the mobile phase.

The precision and detection limit of the method and the efficiency of the extraction procedure were established. For the alkylmercury compounds the lowest limit of detection (80ppb) was obtained with the dithizone reaction detection and for the phenylmercury compounds with UV detection (60ppb). A chromatogram of a spiked fish (2ppmHg) and a river water sample (50ppbHg) is shown.     

Photochemically induced dynamic nuclear polarization in photosystem I of plants observed by 13C magic-angle spinning NMR

Photochemically induced dynamic nuclear polarization (photo-CIDNP) has been observed in photosystem I of spinach by (13)C magic angle spinning solid-state NMR under continuous illumination with white light. An almost complete set of chemical shifts of the aromatic ring carbons of a single Chl a molecule has been obtained which is assigned to the P2-cofactor of the primary electron donor P700. Since all light-induced (13)C NMR signals appear to be emissive, a predominance of the three-spin mixing mechanism over the differential decay mechanism is proposed. The origin of the strong contribution of the three-spin mixing mechanism and the differences with photosystem II are discussed.     

Investigation of lifetimes in dipole bands of 141Eu

Lifetimes have been measured for dipole bands in ¹⁴¹Eu using DSAM. The deduced B(M1) and B(E2) values as well as B(M1)/B(E2) ratios are compared with calculations in the framework of the TAC (Tilted Axis Cranking) and SPAC (Shears mechanism with Principal Axis Cranking) models. The dipole bands can be interpreted as magnetic rotational bands.Received: 6 April 2004, Revised: 14 May 2004, Published online: 13 July 2004PACS: 21.10.-k Properties of nuclei; nuclear energy levels - 21.10.Re Collective levels - 21.10.Tg Lifetimes - 27.60. + j      

Delayed crossing in the \pi h_{9/2} 1/2-[541] band of 173 Lu

High-spin states in the odd-proton nucleus ¹⁷³Lu have been populated in a ¹⁷⁰Er(⁷Li,4n) reaction and the emitted -radiation was detected with the GASP array. The favoured and unfavoured sequences of the band have been considerably extended. The favoured sequence does not show any indication of a band crossing up to a rotational frequency of 0.45 MeV. This is the largest crossing frequency ever observed for 1/2^- [541] bands of odd-proton nuclei with and . Previous Cranked Shell Model (CSM) calculations underestimate the crossing frequency by 100 keV.Received: 19 May 2003, Published online: 11 November 2003PACS: 21.10.-k Properties of nuclei; nuclear energy levels - 21.10.Re Collective levels - 23.20.Lv transitions and level energies - 27.70. + q      

Ringschlussreaktionen mit 2-(β-Styryl)benzylaminen 5-Phenyl-1H-2-benzazepine. 23. Mitteilung über siebengliedrige Heterocyclen

Cyclization reactions with 2-(β-styryl)benzylamines 5-Phenyl-1H-2-benzazepines Cyclization of the urea derivative 3 with POCl₃ to give 2-(4-methyl-1-piperazinyl)-4-phenylquinoline ( 4 ) was carried out in analogy to the quinoline synthesis of Foulds & Robinson. This reaction was used for the preparation of 2-benzazepines. The trisubstituted ureas 6 and 8 , derived from the 2-(β-styryl)-benzylamines 5 , were cyclized with POCl₃ to yield the 3-amino-5-phenyl-1H-2-benzazepines 7 and 9 , respectively. Similarly, cyclization of the corresponding acetyl-derivatives 10 gave the 3-methyl-5-phenyl-1H-2-benzazepines 12 . On the other hand, the disubstituted urea 15 , cyclized under the same conditions to the 1-methyl-1-phenylisoindoline derivative 16 , and 2-(β-styryl)benzylamine ( 5a ) on treatment with phosgene gave the isoindoline 17 in an analogous manner.     

Optimal pulse-width modulation for sinusoidal fringe generation with projector defocusing: comment

We comment on a recent Letter [Opt. Lett. 35, 4121 (2010)], in which the authors discuss an optimal pulse-width modulation (OPWM) method for sinusoidal fringe generation. We consider that the comparison of the squared binary method (SBM) and the sinusoidal pulse-width modulation (SPWM) method has considerable deficiencies.     

Synthesis and characterization of a new semi-interpenetrating polymer network hydrogel obtained by gamma radiations

A new polyacrylic acid/polyhydroxybutyrate semi-interpenetrating polymer network hydrogel, the s-IPN/PAA-PHB, was prepared by a gamma radiation-induced polymerization. Thermal behavior was studied by thermogravimetric analysis (TG) and Differential scanning calorimetry (DSC), while the s-IPNs composition, FTIR spectra, and swelling kinetics were also determined. It was found that the DSC curve showed a melting point which is attributed to polyhydroxybutyrate. The TG curves showed various stages of degradation which are in correspondence of the presence of crosslinked polyacrylic acid and confirmed the higher thermal stability of the polymer network. The s-IPN/PAA-PHB composition was 10% of PHB and 90% of PAA. Moreover, the network reached approximately 600% of swelling in water, so it behaves like a superabsorbent hydrogel.     

Determination of titanium content in pyrope by Raman spectroscopy

The titanium content of pyrope garnet can be quantified using the intensity of a Raman band at about 830 cm⁻¹ that is normalized to the 363 cm⁻¹ band using a spectrometer‐specific calibration using 10 to 15 chromian pyropes from Bohemia, Czech Republic. An accuracy of 0.025 wt% could be achieved for TiO₂ contents between 0.17 and 0.67 wt% TiO₂ with a Raman spectrometer with a spectral resolution of better than 3.9 cm⁻¹. The technique can be used in petrological and gemmological studies. Copyright © 2015 John Wiley & Sons, Ltd.     

Viskositätsmessung mit dem longitudinal schwingenden Band

A method for the detection of small masses with the aid of a longitudinally vibrating band is described and further applications, e.g. for viscosity and humidity measurement are discussed. The complex Young's modulus of the band can also be determined.