Determination of deoxynivalenol in cereals and cereal products by immunoaffinity column cleanup with liquid chromatography: interlaboratory study

An interlaboratory study was performed on behalf of the UK Food Standards Agency to evaluate the effectiveness of an immunoaffinity column cleanup liquid chromatographic (LC) method for the determination of deoxynivalenol in a variety of cereals and cereal products at proposed European regulatory limits. The test portion was extracted with water. The sample extract was filtered a applied to an immunoaffinity column. After being washed with water, the deoxynivalenol was eluted with acetonitrile or methanol. Deoxynivalenol was quantitated by reversed-phase LC with UV determination. Samples of artificially contaminated wheat-flour, rice flour, oat flour, polenta, and wheat based breakfast cereal, naturally contaminated wheat flour, and blank (very low level) samples of each matrix were sent to 13 collaborators in 7 European countries. Participants were asked to spike test portions of all samples at a range of deoxynivalenol concentrations equivalent to 200-2000 ng/g deoxynivalenol. Average recoveries ranged from 78 to 87%. Based on results for 6 artificially contaminated samples (blind duplicates), the relative standard deviation for repeatability (RSDr) ranged from 3.1 to 14.1%, and the relative standard deviation for reproducibility (RSDR) ranged from 11.5 to 26.3%. The method showed acceptable within-laboratory and between-laboratory precision for all 5 matrixes, as evidenced by HorRat values < 1.3.     

Synthesis and Characterization of trans‐PdII Trimethylsilylchalcogenolates

The trans‐bis(trimethylsilyl)chalcogenolate palladium complexes, trans‐[Pd(ESiMe₃)₂(PnBu₃)₂] [E = S ( 1 ) and Se ( 2 )] were synthesized in good yields and high purity by reacting trans‐[PdCl₂(PBu₃)₂] with LiESiMe₃ (E = S, Se), respectively. These complexes were characterized by ¹H, ¹³C{¹H}, ³¹P{¹H} (and ⁷⁷Se{¹H}) NMR spectroscopy and single‐crystal X‐ray analysis. The reaction of 2 with propionyl chloride led to the formation of trans‐[Pd(SeC(O)CH₂CH₃)₂(PnBu₃)₂] ( 3 ), a trans‐bis(selenocarboxylato) palladium complex and thus established a new method for the formation of this type of complex. Complex 3 was characterized by ¹H, ¹³C{¹H}, ³¹P{¹H} and ⁷⁷Se{¹H} NMR spectroscopy and a single‐crystal X‐ray structure analysis.     

Radiative decay of doubly excited states in helium below the He+ (N = 2) ionization threshold

The radiative decay of (1)P(o) doubly excited states in helium has been investigated using a novel apparatus in which metastable atoms and vacuum ultraviolet photons are detected. The intensity ratio of the energetically narrow (sp,2n-)(1)P(o) and (2p,nd)(1)P(o) series to the broader (sp,2n+)(1)P(o) series is strikingly enhanced in comparison with conventional photoabsorption, photoion, or photoelectron measurements using synchrotron radiation. The experimental approach is a new way forward for the study of energetically narrow doubly excited states.     

Spontaneous quantum Hall states in chirally stacked few-layer graphene systems

Chirally stacked N-layer graphene systems with N≥2 exhibit a variety of distinct broken symmetry states in which charge density contributions from different spins and valleys are spontaneously transferred between layers. We explain how these states are distinguished by their charge, spin, and valley Hall conductivities, by their orbital magnetizations, and by their edge state properties. We argue that valley Hall states have [N/2] edge channels per spin valley.     

Fermi velocity enhancement in monolayer and bilayer graphene

In single-layer graphene sheets non-local interband exchange leads to a renormalized Fermi-surface effective mass which vanishes in the low carrier-density limit. We report on a comparative study of Fermi surface effective mass renormalization in single-layer and AB-stacked bilayer graphene. We explain why the mass does not approach zero in the bilayer case, although its value is still strongly suppressed.     

Chirality and correlations in graphene

Graphene is described at low energy by a massless Dirac equation whose eigenstates have definite chirality. We show that the tendency of Coulomb interactions in lightly doped graphene to favor states with larger net chirality leads to suppressed spin and charge susceptibilities. Our conclusions are based on an evaluation of graphene's exchange and random-phase-approximation correlation energies. The suppression is a consequence of the quasiparticle chirality switch which enhances quasiparticle velocities near the Dirac point.     

Experimental methods of X-ray stress analysis

A technique is described for measuring residual stresses in steels and composite materials by X-ray diffraction. Specimen preparation, X-ray diffractometer alignment, diffraction-peak location, and the determination of the elastic modulus, Poisson's ratio and stress factor are covered. Application examples include measurement of heat-treating and shot-peening stresses in steels and grinding and temperature stresses in WC-Co composites.     

Subitising activity relative to units construction: a case study

Subitising, a quick apprehension of the numerosity of a small set of items, has been found to change from an individual's reliance on perceptual to conceptual processes. In this study, we utilised a constructivist teaching experiment methodology to investigate how the subitising activity of one preschool student, Amy, related to her construction of prenumerical units. Subitising and counting tasks were designed to assess and perturb Amy's thinking relative to her construction of units, and to observe changes in Amy's activity associated with the different tasks. Findings indicate that as Amy's subitising activity changed from perceptual to conceptual, she constructed subitised motor units and subitised figurative units. Implications of this study suggest that the construction of subitised units may support young children's later development of arithmetic units.     

Hierarchies of holonomy groupoids for foliated bundles

We give a new construction of the holonomy groupoid of a regular foliation in terms of a partial connection on a diffeological principal bundle of germs of transverse parametrisations, which may be viewed as a systematisation of Winkelnkemper’s original construction using ideas from gauge theory. We extend these ideas to construct a novel holonomy groupoid for any foliated bundle, which we prove sits at the top of a hierarchy of diffeological jet holonomy groupoids associated with the foliated bundle. This shows that while the Winkelnkemper holonomy groupoid is the smallest Lie groupoid that integrates a foliation, it is far from the smallest diffeological groupoid that does so.

     

Asymmetric transmission through a photorefractive crystal of barium titanate

We have investigated the feasibility of using a barium titanate crystal as a unidirectional device. The nonlinear interaction between a beam and its own reflection from the back face of the crystal causes an effective increase or decrease in the transmission through the crystal, depending on whether the incident beam propagates along or against the crystal c-axis, respectively. This effect was investigated for several wavelengths and compared with theory. It is possible to make a device that has an average transmission of ≈94% and a transmission asymmetry of 1% by using a crystal whose front and back faces are cut so that their normals are at angle of ≈30° to the crystal c-axis.