Mercury(II) tungstate from neutron powder data

Mercury(II) tungstate powder, HgWO₄, was prepared by boiling a mixture of HgO and H₂WO₄ in water. Rietveld refinements on neutron powder data showed that the monoclinic structure (C2/c) consists of zigzag chains of edge‐sharing HgO₆ and WO₆ octahedra. The Hg atom lies on an inversion centre and the W atom lies on a twofold axis. The Hg atom forms two characteristic short collinear Hg—O bonds.     

Solution behaviour of a formate capped surfactant—the oxidation product of an alcohol ethoxylate

The solution behaviour has been investigated for an alcohol ethoxylate terminated with a formic acid ester. This compound has previously been reported to be an important degradation product in the auto-oxidation of alcohol ethoxylates. In this work we have investigated the solution behaviour of the formic acid ester surfactant C₁₂H₂₅(OCH₂CH₂)₄OCHO (C12E4---OCHO). The pure formate was found to be sparsely soluble in water with no clear point at 0.1%. The critical micelle concentration was found to be 129 μM at 35°C, compared to 50 μM for the parent surfactant C₁₂H₂₅(OCH₂CH₂)₅OH (C12E5). To mimic the behaviour of the oxidised surfactant, the formate was mixed in different ratios with C12E5 and the cloud point, surface tension and critical micelle concentration (cmc) of these mixtures were studied. The gradual increase of formate was found to shift the cloud point and isotropic regions to lower temperatures. The cmc of the mixture was found to be lower than for the pure surfactant. The favourable interaction was analysed according to the non-ideal model by Rubingh and the interaction parameter, β, was determined to be −4±0.53, which is unusually large for a mixture of two non-ionic surfactants. These results indicate that the reduction of cloud point observed during oxidation of non-ionic surfactants can in part be attributed to the formation of formate esters.     

Mass spectrometric identification of a stable catalytic cysteinesulfinic acid residue in an enzymatically active chemically modified glucoamylase mutant.

Mass spectrometric identification of cysteinsulfinic acid resulting in restoration of activity of chemically modified Glu400 Cys catalytic-base glucoamylase (GA) mutants is described. This oxidation unexpectedly occurred during attempts to carboxyalkylate the Cys400 GA mutant using three different alkylation reagents. However, mass spectrometric peptide mapping did not show the presence of carboxyalkylation of the Cys400 residue but suggested an oxidation to cysteinsulfinic acid based on the observed mass increment. The presence of cysteinsulfinic acid was confirmed by employing matrix-assisted laser desorption/ionization mass spectrometry combined with post-source decay analysis. Furthermore, strong enhancement of metastable fragmentation was observed for peptides containing oxidized Cys in comparison with non-oxidized peptide.     

The microstructure of the base oxide on 304L steel

304L stainless steel specimens were subjected to 168 h of oxidation in dry oxygen at 600°C. The composition and microstructure of the oxide as well as the steel near the steel–oxide interface were investigated using SEM and TEM in conjunction with EDS analysis. It was found that the first oxide layers, referred to as the base oxide, consisted of 50–100 nm-sized corundum-type grains. Each grain contained oxides of chromium, iron plus a small amount of manganese in a solid solution with the chemical formula (Cr,Fe,Mn)₂O₃. In the oxide regions closest to the steel–oxide interface, the grain center compositions varied laterally from grain to grain, with the cation balance ranging between very chromium-rich (Cr:Fe=4:1) and very iron-rich (Cr:Fe=1:8). Within each oxide grain, the chromium level was generally higher in the center than near the boundary. This was due to the much quicker diffusion of iron (compared to chromium) at and through the oxide grain boundaries than in the bulk of the oxide grains, creating iron enrichment near the oxide grain boundaries. Compositional variation with respect to the distance from the steel–oxide interface was also noted. Chromium was richer in the oxide regions closer to the steel–oxide interface than farther out in the oxide and depleted from the steel regions bordering the steel–oxide interface. Manganese was also depleted in those steel regions although hardly enriched in the oxide just outside the steel–oxide interface. Nickel was less reactive than chromium, iron or manganese and hence was virtually absent from the oxide.     

ESR studies of thermally oxidized silicon wafers

We have performed ESR measurements on oxidized (111) silicon wafers and found two ESR centers. One, the previously known P_b center,was found to be a two level interface trap by corona bias studies. The other one, previously known as “damaged silicon” center was found to be a silicon center, probably related to the oxide growth process.     

The initial growth of Au on GaAs(001)-c(4 × 4)

The metal growth when depositing a monolayer (ML) of Au at 200° C on MBE-grown surfaces of GaAs(001)-c(4 × 4) was studied by AES and RHEED. The surface interaction can be characterized to proceed in two stages depending on the surface coverage of Au. At a coverage of less than 0.3 ML the gold atoms are mainly dispersed on the surface with a small in depth diffusion. Above 0.4 ML there is a rapid intermixing and a tendency of arsenic accumulation to the surface.     

Response spectrum methods in tank-vehicle design

Existing design rules for tank vehicles have proved insufficient, because vibrations often cause fatigue cracks. Measurements have been performed on the tank to provide a picture of the influence of different road types and filling ratios. Shock response spectrum analysis (SRS) was used to obtain a measure of single-dynamic events. To get a basis for dimensioning against fatigue a calculation of fatigue-damage response spectra (FDRS) has been performed. This relates the vibrations in the tank to the risk of fatigue damage. In lieu of cycle counting by rain-flow count techniques, which has certain disadvantages, a new model, the so called HdM model, for fatigue-life assessment based on level crossing has been used. Further development of the results of the analysis can be used to improve design criteria in transport tank regulations, as well as to determine optimum inspection intervals for, in particular, tanks for hazardous materials.     

Dynamic buckling of a beam with transverse constraints

A nonlinear dynamic system with continuously distributed mass is studied using several approaches: experimentally, numerically as well as analytically. The nonlinearity of the system consists of geometrical constraints imposed on the motion. It is harmonically loaded and it is demonstrated that for certain choices of the loading parameters, periodic, quasi-periodic or chaotic behaviour may occur depending on the initial conditions. An important issue is to investigate the number of degrees of freedom needed in order to analytically model the system accurately enough that the important characteristics of the motion are retained in the solution. It is found that the impact conditions at the constraints are of crucial importance and a new approach is proposed for modelling of the impacts. The method is based on the fact that the free motion can be approximated with quite a few degrees of freedom, while at impact all the infinite number of degrees of freedom are considered.