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The dual roles of microanalysis and trace analysis are qssessed. The former is generally concerned with the analysis of very small samples for major constituents and the latter with the determination of very minor constituents in samples of normal (or macro) size. This contribution describes a technique of ultramicrotrace analysis in which both principles are combined. Trace constituents are analysed in samples of ultramicro proportions viz 1 111. A flameless technique of atomic absorption and atomic fluorescence is evolved which allows amounts of some elements to be detected down to 10-15 g and to be determined with a precision of 2—3 at 10-14 g levels. The samples are evaporated on a resistively heated carbon (graphite) rod and the temperature is then swept up to Ca. 2600°C by increasing the voltage to Ca. 12 V. This produces a transient cloud of atoms which are studied by a fast response detection system for atomic absorption or fluorescence signals. The technique is absolutely specific for each element and allows most elements to be determined with a sensititivity far surpassing that of x-ray fluorescence and challenging and sometimes even surpassing neutron activation analysis, mass spectrometry and electron probe microanalysis using apparatus at a fraction of the cost and generally available, with only slight modification, in almost every inorganic trace analysis laboratory.

The determination of very small amounts of materials by the techniques of atomic-absorption and atomic-fluorescence spectroscopy