The effect of aluminium coating on elemental standards in X-ray microanalysis

The standardisation of frozen hydrated bulk biological specimens using gelatin standards is described. The relationship between corrected elemental X-ray counts and ionic concentration was found to be linear, and minimum detectable limits for each element are stated. Variations in uncorrected standard curves were found to be due to changes in aluminium coating thickness. There was an inverse relationship between coating thickness and elemental X-ray counts. The factors causing this are discussed. To avoid errors arising from inconsistent aluminium thickness, experimental material should only be compared with standards of similar aluminium net counts. This can be achieved most easily by mounting and analysing specimen and standard together.     

Swelling of Hot-Pressed A12O3

Fully dense aluminas, prepared by hot-pressing, were found to swell during annealing at 1600°C in air, but not during annealing in a reducing atmosphere (po₂= 10^-7 Pa). The reaction followed the relation p - po = -K log t, where p_o and p are the initial and final densities, respectively, t is the time, and AT is a constant. The rate of swelling was enhanced by MgO solute. The reduction in density resulted from the nucleation and growth of grain-boundary pores. Pore formation was attributed to the reaction of carbon and sulfur impurities at the boundaries with oxygen, which had diffused down the grain boundaries from the ambient, to form CO/CO₂ and SO₂ gas at high pressures. Preliminary results indicate that this reaction can be avoided by preannealing powders in flowing oxygen prior to hot-pressing. The consequences of internal gas-forming reactions to other processes such as high-temperature creep and sintering are also discussed.     

Parameter-Free Equation-of-State Calculations for MgO and ZrO2

The electronic band structure of ZrO₂ is calculated for the fluorite structure using the self-consistent augmented-plane-wave method in the muffin-tin approximation. The crystal charge density is then site decomposed by fitting Slater orbitals to the wave functions in the muffin tins. The resultant charge densities for Zr⁴⁺ and O²⁻ are then used in the Gordon-Kim method to derive pair potentials, from which a number of structural, elastic, and thermodynamic properties are calculated and compared with experimental results and similar calculations for MgO.     

Stability studies on methyl and ethyl fatty acid esters of sunflowerseed oil

Fatty acid esters, high in linoleic acid, were prepared and stored for long-term engine tests. Storage tests with these esters were undertaken to obtain more information on optimal storage requirements and general stability characteristics. Samples were kept at three temperature levels (20 C, 30 C and fluctuating around 50 C) for a 90-day period and were removed at regular intervals for chemical and physical analysis. The influence of air, temperature, light, TBHQ and contact with mild steel was evaluated by comparing the free fatty acid, peroxide, anisidine, ultraviolet absorption, viscosity and induction periods. A statistical model was used to evaluate the data and to reduce the large number of data points to comparable curves. Storage of esters in contact with air, especially at a temperature above 30 C, resulted in significant increases in peroxide, ultraviolet absorption, free fatty acid, viscosity and anisidine values. Exclusion of air retarded oxidation at all temperature levels. A direct relationship between viscosity increases and oxidation parameters was evident. Exposure to light caused a small increase in the oxidation parameters of esters stored at the highest temperature level. Addition of TBHQ prevented oxidation of samples stored under moderate conditions. Under unfavorable storage conditions the anti-oxidant was no longer effective. Mild steel had very little effect on the oxidation parameters. Only the anisidine values of samples stored at the highest temperature level were slightly increased. Methyl esters performed slightly better than ethyl esters during the storage test. The following practical guidelines for storage of fatty acid ester fuels are: (i) airtight containers should be used; (ii) the storage temperature should be <30 C; (iii) mild steel (rust free) containers may be used, and (iv) TBHQ has a beneficial effect on oxidation stability.