CO laser stabilization using the optogalvanic Lamb-dip

Frequency stabilization of the CO laser using a CO lamb-dip is achieved in the range from 5.0–6.3 m. The CO saturation signal is obtained from a low-pressure discharge in absorption and is detected using optogalvanic, detection. The frequency stability and reproducibility has been verified to be better than 100 kHz; this is an improvement of more than one order of magnitude compared with locking techniques using CO laser gain profiles.Alexander von Humboldt Awardee from National Bureau of Standards, Boulder, Colorado, USA     

Analysis of the 3-dimensional electron distribution in silicon using directional Compton profile measurements

A method of reconstructing the electron momentum density (p), and its Fourier transform,B(t), from a series of directional Compton profiles is described. It is based on a double Fourier inversion technique and an expansion in lattice harmonic functions. The effect of random errors has been analysed, and the implications for the data collection discussed. We have used the reconstruction technique to obtain (p) andB(t) for silicon from six directional Compton profiles measured with 412 KeV gamma-radiation. The experimental result is in good agreement with earlier measurements and with available solid state theories. A recent Wannier function calculation for silicon using orthogonalised bond orbitals provides a useful tool for identifying the physical origins of the observed anisotropies. A comparison between the information presented in position and momentum space shows that the ease of interpretation depends upon the degree to which the various interactions give rise to localised features in each representation.     

Multiresidue determination of fluoroquinolones in shrimp by liquid chromatography-fluorescence-mass spectrometry

An efficient multiresidue method for analysis of fluoroquinolones in shrimp has been developed in which quantitation by fluorescence and confirmation by Multiple Stage Mass Spectrometry (MS) is achieved simultaneously. In this method, shrimp tissue is extracted with ammoniacal acetonitrile and the extract is defatted and then evaporated. After dissolution in basic phosphate buffer, fluoroquinolones in the extract are separated by liquid chromatography and quantitated, taking advantage of their intense fluorescence. Eluate from the fluorescence detector enters the MS, which allows for confirmation by monitoring ratios of 2 prominent product ions in the MS3 or MS2 spectrum. Using this method, 8 fluoroquinolones have been analyzed in shrimp samples fortified at 10, 25, 50, or 100 ppb levels. Recoveries for desethyleneciprofloxacin, norfloxacin, ciprofloxacin, danofloxacin, enrofloxacin, orbifloxacin, sarafloxacin, and difloxacin ranged from 75 to 92%, with relative standard deviation values of <6%. The limits of quantitation ranged from 0.1 to 1 ng/g. Enrofloxacin and ciprofloxacin were also successfully determined in enrofloxacin-incurred shrimp using this method.     

Triamidoamine complexes of chromium(III) and chromium(IV)

Treatment of [CrCl3(THF)3] with slightly more than 1 equiv of Li3(N3N) [(N3N)(3-) = ((Me3SiNCH2CH2)3N)(3-)] affords the triamidoamine complex [Cr(N3N)] (1) in 75% yield. 1 is oxidized by PhICl2, CuCl2, or AgCl to give the chromium(IV) complex [Cr(N3N)Cl] (2) in moderate yields. Alternatively, complex 2 is obtained directly from [CrCl3(THF)3] in 50% yield after treatment with 0.5 equiv of Li3(N3N). Both compounds are high-spin complexes bearing three and two unpaired electrons, respectively. Their molecular structures are described revealing a trigonal monopyramidal and trigonal bipyramidal coordination geometry of the chromium center, respectively.     

η-Allylpentacarbonylvanadium

The preparation of η-C₃H₅V(CO)₅ from allyl chloride and sodium hexacarbonylvanadate (–I) is reported. Composition, IR and NMR spectra are in accordance with a π-bonded C₃H₅-moiety; the preparation has been extended to give complexes with substituted allyl groups. Furthermore (1-3-η-2-butenyl)pentacarbonylvanadium can be obtained by the addition of butadiene to HV (CO)₆.     

Phenotyping apolipoprotein E*3-leiden transgenic mice by two-dimensional polyacrylamide gel electrophoresis and mass spectrometric identification

Apolipoprotein E (ApoE) plays an important role in cholesterol and triglyceride metabolism, being one of the major structural components of chylomicrons and very low density lipoprotein (VLDL) remnants. ApoE functions as a ligand in the receptor-mediated uptake of these remnants from the blood by the liver. A variant form of ApoE, apolipoprotein E*3-Leiden, shows reduced affinity for the low density lipoprotein (LDL) receptor, and results in the dominant expression of type III hyperlipoproteinemia. Two-dimensional electrophoresis (2-DE) has been used to characterise protein expression in serum samples from control and transgenic mice expressing the human ApoE*3-Leiden mutation, fed a cholesterol-rich diet, and transgenic mice fed a normal diet. For the identification of proteins, single silver-stained spots were excised from the 2-DE gels and subjected to in-gel enzymatic digestion. Extracted peptides were analysed by matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF-MS). This proteomic approach has enabled the ApoE*3-Leiden variant to be positioned in a 2-DE separation of serum proteins, and has identified changes in the expression of haptoglobin, indicating that this protein may provide a marker for the potential onset of atherosclerosis.     

Application of the essential work of fracture concept to nanostructured polymer materials

The first part of the paper deals with a critical discussion of the methodical basis of essential work of fracture (EWF) concept with respect to the specimen geometry (especially the notch depth) and application to polymers. In the second part, an in situ testing device, which combines a tensile testing machine with an optical strain-field measuring system, has successfully demonstrated possibility of characterization of fracture behaviour of polystyrene-polybutadiene block copolymers and block copolymer/homopolymer blends as examples of nanostructured polymer materials. It has been shown that knowledge of the time evolution of the strain field close to the crack tips leads to a simple verification of the basic precondition for the applicability of the EWF concept, the precondition “plastic zone coalescence-before-stable crack propagation”.     

Neutron diffraction study of [H(4)Co(4)(C(5)Me(4)Et)(4)], a tetrahedral metal cluster complex with four face-bridging hydride ligands

A single-crystal neutron diffraction analysis of the cluster complex [H(4)Co(4)(C(5)Me(4)Et)(4)] was carried out on the new quasi-Laue diffractometer VIVALDI at the Institut Laue-Langevin. The structure consists of four face-bridging hydrides attached to a tetrahedral cobalt metal core. Average distances and angles in the core of the molecule are as follows: Co-Co = 2.571(8), Co-C = 2.158(6), Co-H = 1.749(7), H.H = 2.366(9) A; Co-H-Co = 94.6(3), H-Co-H = 85.1(3) degrees. The hydride ligands are located off the Co-Co-Co planes by an average distance of 0.923(8) A. It is suggested that the dimensions of the HCo(3) fragments found in this molecule provide reasonable estimates for analogous distances and angles associated with chemisorbed H atoms situated on the 3-fold hollows of a cobalt surface. Crystallographic details: space group P2(1)/a (monoclinic); a = 21.979(2), b = 10.924(1), c = 34.406(2) A; beta = 90.81(1) degrees; Z = 8. Final agreement factor: R(F) = 0.099 for 3779 reflections [I > 2sigma(I)] collected at 20 K.