Influence of deuteration on lithium acetate dihydrate studied by inelastic X-ray scattering, density functional theory, thermal expansion, elastic and thermodynamic measurements.

The influence of deuteration on the properties of lithium acetate dihydrate has been investigated by thermal expansion measurements, ultrasound spectroscopy and calorimetry. Inelastic X-ray scattering has been employed to investigate if the low temperature structural phase transition can be detected by a change in the vibrational spectrum. Density functional theory, DFT, calculations have been employed to complement the experimental investigations. The thermal expansion coefficients and the specific heat of the deuterated compound differ significantly from the protonated form. The differences in the elastic stiffness coefficients are just above the detection limit of the technique employed here. Temperature dependent inelastic X-ray spectroscopic measurements show no significant change of the vibrational spectrum when crossing the transition temperature. The DFT calculations show that the methyl group dynamics are best described in the framework of coupled rotators of opposing methyl groups. One of the coupled rotational modes corresponds to a hindered rotator with a barrier of 15 meV, while the other is a free rotator.

Quantum impurities and the neutron resonance peak in YBa2Cu3O7: Ni versus Zn.

The influence of magnetic (S=1) and nonmagnetic (S=0) impurities on the spin dynamics of an optimally doped high temperature superconductor is compared in YBa2(Cu0.97Ni0.03)3O7 (Tc=80 K) and YBa2(Cu0.99Zn0.01)3O7 (Tc=78 K). In the Ni-substituted system, the magnetic resonance peak (which is observed at Er approximately 40 meV in the pure system) shifts to lower energy with a preserved Er/Tc ratio while the shift is much smaller upon Zn substitution. By contrast Zn, but not Ni, restores significant spin fluctuations around 40 meV in the normal state. These observations are discussed in the light of models proposed for the magnetic resonance peak.

Solid-phase microextraction coupled with high performance liquid chromatography: a complementary technique to solid-phase microextraction-gas chromatography for the analysis of pesticide residues in strawberries.

Solid-phase microextraction coupled with high performance liquid chromatography has been studied for the analysis of methiocarb, napropamide, fenoxycarb and bupirimate in strawberries. The strawberries were blended and centrifuged. Then, an aliquot of the resulting extracting solution was subjected to solid-phase microextraction (SPME) on a 60 microns polydimethylsiloxane/divinylbenzene (PDMS/DVB) fibre for 45 min at room temperature. The extracted pesticides on the SPME fibre were desorbed into SPME/high performance liquid chromatography (HPLC) interface for HPLC analysis with diode-array detection (DAD). The method is organic solvent-free for the whole extraction process and is simple and easy to manipulate. The detection limits were shown to be at low microgram kg-1 level and the linear response covered the range from 0.05 to 2 mg kg-1 of pesticides in strawberries with a regression coefficient larger than 0.99. A good repeatability with RSDs between 2.92 and 9.25% was obtained, depending on compounds.

Solid phase microextraction of pesticide residues from strawberries.

A new solid phase microextraction method for the determination of pesticide residues in strawberries for 16 commonly used compounds was described. The strawberries were crushed and centrifuged. An aliquot of the well agitated aqueous supernatant (4 ml) was extracted with a fibre coated with polydimethylsiloxane (PDMS, 100 microns) for 45 min at room temperature. Identification and quantification were achieved using a gas chromatography-mass spectrometry (GC-MS) system and selective ion monitoring (SIM). The method was tested for the following pesticides: carbofuran, diethofencarb, penconazole, hexaconazole, metalaxyl, folpet, bromopropylate, dichlofluanid, alpha-endosulfan, beta-endosulfan, parathion ethyl, procymidone, iprodione, vinclozolin, myclobutanil and chlorothalonil. Limits of detection, repeatability and linearity for standard calibration in strawberries were obtained. Positive and negative effects of the matrix between the extracting solution of strawberries and water were observed. Stabilities of these compounds in the extracting solution of strawberries were determined. The solvent-free SPME procedure was found to be quicker and more cost effective than the solvent extraction methods commonly used.

Low-frequency vibrations of a nucleoside analog.

This paper reports on the first coherent neutron scattering measurements ever carried out on the vibrational spectrum of a nucleoside analog. Frequencies up to 3.5 Thz belonging to some half-dozen dispersion curves have been measured in a plane normal to the [1 10] direction in a triclinic crystal of 5-iodo-2'-deoxyuridine (5-iodouridine). The number of phonon branches observed suggests that the deoxyribose sugar and pyrimidine in this molecule are the vibrating entities at low frequencies. Comparisons, notably of elastic properties, are made with previous measurements on crystalline forms of DNA and various nucleic acid base derivatives. The observed frequencies are discussed with reference to a simple force constant model.