Preparation and characterization for mineral elements and total dietary fiber and testing for stability of β-carotene of an ARC/CL carrot powder multipurpose candidate reference material

As part of the analytical assurance system of the FAO European Cooperative Research Network on Trace Elements programme an ARC/CL-coded carrot flakes powder (CFP) candidate reference material (RM) has been prepared from a lot of commercial carrot flakes. The candidate RM has been homogenized using a Robot Coupe blender fitted with titanium blades, carefully homogenized in large teflon/polypropylene containers, bottled in 1000 numbered polyethylene containers (20 g samples) and tested for homogeneity. Interlaboratory comparison studies for 9 essential elements, cadmium and total dietary fiber (TDF) based on the AOAC-method resulted in the characterization of the contents of those compounds in the above material. After exclusion of outliers, mean values from at least nine different laboratories based altogether on three independent analytical principles have been used to calculate the recommended concentration ranges for mineral elements. Testing of homogeneity and stability for β-carotene over a period of one year has been additionally carried out. The mean water content in the material amounted to 4.97% and remained stable over a one-year period. Homogeneity of the RM was within 3.0% for almost all included mineral elements as tested for a sample size of 0.5 g. The 95% confidence limits for the mean values of the established recommended concentrations of mineral elements in the present ARC/CL Carrot Powder candidate RM fell within 5% for all the other elements and TDF except for Fe (6.3%) and B (5.7%). The stability of β-carotene in the present candidate RM stored in darkness over a one-year period at room temperature was within 6.3%.     

Fluid queue driven by anM/M/1 queue

A fluid queue receiving its input from the output of a precedingM/M/1 queue is considered. The input can be characterized as a Markov modulated rate process and the well known spectral decomposition technique can be applied. The novel features in this system relate to the nature of the spectrum, which is shown to be composed of a continuous part and one or two discrete points depending on whether the load of the fluid queue is less or greater than the output to input rate ratio. Explicit expressions of the generalized eigenvectors are given in terms of Chebyshev polynomials of the second kind, and the resolution of unity is determined. The solution for the buffer content distribution is obtained as a simple integral expression. Numerical examples are given.     

Computation of AC losses in high-temperature superconductors

A formulation for the computation of AC losses in technical HTS conductors by using commercial FEM packages developed for two-dimensional computation of electromagnetic problems is presented. The formulation takes into account the real current density–electric field characteristic of a conductor and the spatial dependence of the current density. Having presented the formulation, example runs comparing transport current loss behaviour between HTS and LTS conductors are given.     

Ionisation and appearance potentials in the evaluation of nonbonded interactions—IV: Conformational effects in methyl-substituted 1,3-oxathianes

The ionization and appearance potentials for the molecular and [M ? Me]⁺ ions of several stereoisomeric methyl-1,3-oxathianes were measured. The differences between the ionisation and/or appearance potentials are shown to correlate well with the conformational energy differences in question.     

Addition of chlorine,bromine and bromine chloride to some α,β-unsaturated methyl esters

The additions of chlorine, bromine and bromine chloride to trans methyl 2-butenoate 1, trans methyl 2-methyl-2-butenoate 2 and methyl 3-methyl-2-butenoate 3 under ionic conditions were studied. Bromine chloride addition always gave as a major regioisomer the 2-bromo-3--chloro compound,almost quantitatively in the case of 3. The mechanism of bromonium ion ring-opening (S_N1 or S_N2) is discussed with respect to the double bond substitution and regioisomer proportions. The dihalo products were identified by MS, ¹H and ¹³C NMR.     

Thermoanalytical study on the reactions of selected rare earth oxides with ammonium halides

A comparative study has been made on the reactions of RE oxides (RE = Y, La, Gd and Lu) with ammonium bromide, and of yttrium oxide with ammonium halides NH₄X (X = F, Cl, Br and I) at different temperatures. Most of the reactions take place in three stages, with formation of two intermediate compounds, REX₃ · 3 NH₃ and REX₃ · 1.5 NH₃. The endothermic reactions begin between 200 and 300°C and the formation of the RE oxyhalide is completed between 340 and 470°C. These temperatures were observed to rise with the increasing atomic number of RE in the series LaOBrLuOBr, and of halide in the series YOFYOI.     

Determination of chromium in human milk and urine by graphite-furnace atomic absorption spectrometry

Low-temperature ashing and dry ashing at 500°C are compared for the analysis of urine and human milk. Dry ashing gives superior accuracy. The importance of contamination control, background correction and temperature control are stressed. Both urine and human milk contain about 1 ng Cr ml^-1.     

Preparation, thermal stability and luminescence properties of selected rare earth oxycarbonates

A comparative TG and DTG study of the preparation and thermal stability of selected rare earth oxycarbonates, (REO)₂CO₃ (RE = La and Gd), shows that the ease of formation as well as the stability of these compounds decreases strongly with increasing atomic number of the host cation. According to X-ray powder diffraction analyses, the RE oxycarbonates obtained as decomposition products of acetate and carbonate hydrates belong to the tetragonal IA-type. UV- and dye laser-excited luminescence studies of Eu³⁺-doped (LaO)₂CO₃ and (GdO)₂CO₃ reveal the presence of two different sites for the host cation. One of the sites resembles closely that prevailing in the tetragonal RE oxysalts, i.e. oxyhalides, oxysulphates, oxymolybdates and oxynitrates. A crystal field analysis carried out on the ⁷F₁ and ⁷F₂ level schemes according to a C_2v site symmetry confirms this hypothesis.     

Probing lattice defects in Sr2MgSi2O7:Eu2+,Dy3+

The Sr₂MgSi₂O₇:Eu²⁺,Dy³⁺ materials were prepared with a solid state reaction and their microscopic structure (at 295 K only) and luminescence were studied at selected temperatures between 150 and 295 K. Undisturbed Sr crystal planes were common in the TEM images of the undoped Sr₂MgSi₂O₇ material, whereas with Eu²⁺ doping more disturbed planes were observed even in the nanometer scale. With Dy³⁺ co-doping, a large number of small lattice domains created by the discontinuities in the crystal structure was observed. The domains with different orientations seem to be centered around point defects. The decay curves of Sr₂MgSi₂O₇:Eu²⁺,Dy³⁺ showed fast (ms scale) persistent luminescence. The intensity of persistent luminescence increased considerably between 200 and 250 K while remaining constant in the ranges of 150–200 and 250–295 K. The changes were used to study the depth of the traps. In general, Dy³⁺ co-doping was found to deepen the traps.