Effects of thermal and mechanical treatments on a titanium-based conversion coating for aluminium alloys

The influence of mechanical deformation and heating on the protective performance of a chromium-free conversion treatment for aluminium alloys has been assessed by polarisation and AC impedance measurements. Protection is unlikely to be seriously compromised by typical production operations.     

Alpha olefin sulfonates from a commercial SO3-Air reactor

Alpha olefin sulfonate (AOS) can be made by SO₃-air sulfonation of straight chain alpha olefins followed by saponification of the neutralized product. The sulfonation step forms unsaturated sulfonic acids, sultones and sultone sulfonic acids. Hydrolysis of the various sultones yields a mixture of unsaturated and hydroxy sulfonates. Sulfonation of commercial mixtures of straight chain alpha olefins in a large-scale SO₃ falling film unit has given AOS of 1.5–3.0% oil based on active content and tristimulus color of about 40% saturation (2% solution) which is readily bleachable with 1–3% NaOCl to about 10–15% saturation. Performance of AOS made from C₁₅−C₁₈ alpha olefin is comparable to that of the high-foaming C₁₁−C₁₄ LAS in both detergency and dishwashing foam. It is superior to similar products made from internal straight chain olefins. The product shows a low order of toxicity and biodegrad-ability slightly better than that of LAS. A C₁₅−C₁₆ AOS blend is especially attractive in liquid detergent formulations. Presented at the AOCS Meeting, Los Angeles, April 1966.     

High-precision measurement of pixel positions in a charge-coupled device

The high level of spatial uniformity in modern CCD's makes them excellent devices for astrometric instruments. However, at the level of accuracy envisioned by the more ambitious projects such as the Astrometric Imaging Telescope, current technology produces CCD's with significant pixel registration errors. We describe a technique for making high-precision measurements of relative pixel positions. We measured CCD's manufactured for the Wide Field Planetary Camera II installed in the Hubble Space Telescope. These CCD's are shown to have significant step-and-repeat errors of 0.033 pixel along every 34th row, as well as a 0.003-pixel curvature along 34-pixel stripes. The source of these errors is described. Our experiments achieved a per-pixel accuracy of 0.011 pixel. The ultimate shot-noise limited precision of the method is less than 0.001 pixel.     

Error analysis of the rapid lifetime determination method for double-exponential decays and new windowing schemes

The rapid lifetime determination method (RLD) is a mathematical technique for extremely rapid evaluations of lifetimes in exponential decays. It has been applied in luminescence microscopy and single-molecule lifetime evaluation. To date, the primary application has been in single-exponential evaluations. We present extensions of the method to double exponentials. Using Monte Carlo simulations, we assess the performance of both the double-exponential decay with known lifetimes and the double-exponential decay with unknown preexponential factors and lifetimes. Precision is evaluated as a function of the noise level (Poisson statistics), the ratios of the lifetimes, the ratios of their preexponential factors, and the fitting window. Optimum measurement conditions are determined. RLD is shown to work well over a wide range of practical experimental conditions. If the lifetimes are known, the preexponential factors can be determined with good precision even at low total counts (10(4)). With unknown preexponential factors and lifetimes, precisions decrease but are still acceptable. A new gating scheme (overlapped gating) is shown to offer improved precision for the case of a single-exponential decay. Theoretical predictions are tested against actual experimental data from a laser-based lifetime instrument.     

The thermal alkylation of phenol with olefins

Linear alkylphenols from α-olefins can be made by reaction at 260–425 C without added catalyst. By proper choice of conditions, up to 95% monoalkylphenol having the phenol moiety attached at the 1-and 2-carbon of the side chain (primarilyortho orientation) can be obtained.     

Development and validation of an analytical method for total amitraz in fruit and honey with quantification by gas chromatography-mass spectrometry

The EU maximum residue limit (MRL) definition for amitraz is 'the sum of amitraz plus all its metabolites containing the 2,4-aniline moiety, expressed as amitraz'. A rapid and sensitive method has been developed and validated in-house for the determination of total amitraz in pears, strawberries, oranges and honey. Samples were hydrolysed (under acidic followed by alkaline conditions) to convert amitraz to 2,4-dimethyaniline, which was then partitioned into 2,2,4-trimethylpentane prior to quantification by gas chromatography-mass spectrometry. The method was validated at 0.02 and 0.1 mg kg^-1 amitraz (well below MRL requirements) with a lowest calibrated level (LCL) for 2,4-dimethylaniline of 0.002 mg kg^-1 (equivalent to 0.0024 mg kg^-1 amitraz). A single partition step yielded recoveries of ∼60% (with % CV values in the range 3.3-8.2), which is satisfactory for screening purposes. A second partition increased recoveries by 10-20%, making the method suitable for the quantification of residues.     

Improved clean-up for the determination of lasalocid in 'difficult' food matrices

Methodology has been developed for the determination of lasalocid in analytically 'difficult' matrices such as processed and spiced foods. The procedure was based on an existing silica-based solid-phase extraction (SPE) clean-up to which was added a novel NH 2 SPE step before HPLC with fluorescence detection. Use of the additional step enabled the determination of lasalocid in matrices such as baby food, meat pies ('pasties'), etc. Analysis of these matrices was not possible using the standard clean-up on its own. Chromatography showed a massive reduction in the amount of co-extractives and interferences. Validation data were obtained down to the 10-40 μg kg -1 level for a range of products. Recoveries ranged from 74% at 10 μg kg -1 for pork sausages to 96% at 40 μg kg -1 for meat pies.     

The effect of ischemic preconditioning on the recovery of skeletal muscle following tourniquet ischemia

It has been well documented that ischemic preconditioning limits ischemic-reperfusion injury in cardiac muscle, but the ability of ischemic preconditioning to limit skeletal muscle injury is less clear. Previous reports have emphasized the beneficial effects of ischemic preconditioning on skeletal muscle structure and capillary perfusion but have not evaluated muscle function. We investigated the morphologic and functional consequences of ischemic preconditioning, followed by a 2-hour period of tourniquet ischemia on muscles in the rat hindlimb. The 2-hour ischemia was imposed without preconditioning, or was preceded by three brief (10 minutes on/10 minutes off) preischemic conditioning intervals. We compared muscle morphology, isometric contractile function, and muscle fatigue properties in predominantly fast-twitch, tibialis anterior muscles 3 (n = 8) and 7 (n = 8) days after ischemia-reperfusion. Two hours of ischemia, followed by reperfusion, results in a 20 percent reduction of muscle mass (p < 0.05) and a 33 percent reduction in tetanic tension (p < 0.05) when compared with controls (n = 8) at 3 days. The same protocol, when preceded by ischemic preconditioning, results in similar decreases in muscle mass and contractile function. Neuromuscular transmission was also impaired in both ischemic groups 7 days after ischemia. Nerve-evoked maximum tetanic tension was 69 percent of the tension produced by direct muscle stimulation in the ischemia group and 65 percent of direct tension in the ischemic preconditioning/ischemia group. In summary, ischemic preconditioning, using the same protocol reported to be effective in limiting infarct size in porcine muscle, had no significant benefit in limiting injury or improving recovery in the ischemic rat tibialis anterior. The value of ischemic preconditioning in reducing imposed ischemic-reperfusion-induced functional deficits in skeletal muscle remains to be demonstrated.     

Meeting maximum residue limits: an improved screening technique for the rapid detection of antimicrobial residues in animal food products

A rapid, high-throughput antimicrobial screening assay was developed using either a physical fluid extraction or a solvent extraction technique coupled to the commercially available Premi®Test. The solvent extraction approach was fully validated for a wide range of tissues and the fluid extraction approach partially validated for porcine muscle. Both procedures can detect a wide range of antimicrobial compounds at or below maximum residue limit concentrations. The use of a solvent extraction provides an enhanced test capable of detecting a wider range of drugs than the fluid extraction approach at or below half maximum residue limit levels in a variety of matrices. Biochemical methods for the class-specific identification of β-lactams and sulphonamides following initial screening were developed and validated. The approach is a significant improvement on existing methodologies as a tool for residues monitoring in surveillance programmes.     

All-GaAs/AlGaAs readout circuit for quantum-well infrared detectorfocal plane array

We report the fabrication and testing of an all-GaAs/AlGaAs hybrid readout circuit operating at 77 K designated for use with an GaAs/AlGaAs background-limited quantum-well infrared photodetector focal plane array (QWIP FPA). The circuit is based on a direct injection scheme, using specially designed cryogenic GaAs/AlGaAs MODFET's and a novel n⁺ -GaAs/AlGaAs/n⁺-GaAs semiconductor capacitor, which is able to store more than 15 000 electrons/μm² in a voltage range of ±0.7 V. The semiconductor capacitor shows little voltage dependence, small frequency dispersion, and no hysteresis. We have eliminated the problem of low-temperature degradation of the MODFET I-V characteristics and achieved very low gate leakage current of about 100 fA in the subthreshold regime. The MODFET electrical properties including input-referred noise voltage and subthreshold transconductance were thoroughly tested. Input-referred noise voltage as low as 0.5 μV/√Hz at 10 Hz was measured for a 2×30 μm² gate MODFET. We discuss further possibilities for monolithic integration of the developed devices