We describe herein an unprecedented mechanochemical "parallel synthesis" of 3,4-dihydro-2H-benzo[e][1,3]oxazine derivatives via a one pot three component reaction. The new milling system uses a multiposition jar (variable sizes are possible), allowing for the processing of up to 12 samples simultaneously, leading to the formation of a fungicide and a building block for polymer preparation with higher throughput compared to standard milling devices.
The flow injection introduction of samples that would be difficult by conventional nebulisation owing to dissolved solid content, viscosity or quenching effects on flame reactions is demonstrated. The various ways of achieving sample dilution by control of volume injected, tube dimensions and flow-rate are discussed and a manifold described for producing solutions for calibration purposes and diluting off-range samples. The important characteristics of the nebuliser and instrument for flow injection work are evaluated. A simple manifold for investigating interference effects is described and its use illustrated for some well known effects. The possibilities of achieving pre-treatment by solvent extraction and extension to include indirect methods are discussed and the role of flow injection procedures in the method development for, and the extension of the range of application of, flame atomic-absorption spectrometry is critically evaluated.
A comparison of six commercially available curve fitting algorithms for calibration in flame atomic absorption spectrometry (FAAS) has been made. Programs using the algorithms were written in BASIC for a microcomputer and, where possible, tested against the commercial version. Calibration curves for magnesium, chromium and nickel produced by the algorithms were compared, on t h e basis of the sum of squares of the percentage deviations and its root mean square, with each other and with linear interpolation and manual fitting. The standard deviations of the goodness of fit parameters were calculated t o indicate significant differences between the fits obtained. With the exception of the simple parabola, linear interpolation and manual methods, which were significantly poorer, the algorithms performed similarly. In general the errors in curve fitting were well below 5% for the commercial algorithms.
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