Spectra-Physics fluorescence detector

The basic instrumentation used for spectrometric measurements has already been described in the previous chapter (p. 277). Methods of excitation, monochromators and detectors used in atomic emission and absorption techniques are included in Table 8.1. Sources of radiation physically separated from the sample are required for atomic absorption, atomic fluorescence and X-ray fluorescence spectrometry (cf. molecular absorption spectrometry), whereas in flame photometry, arc/spark and plasma emission techniques, the sample is excited directly by thermal means. Diffraction gratings or prism monochromators are used for dispersion in all the techniques including X-ray fluorescence where a single crystal of appropriate lattice dimensions acts as a grating. Atomic fluorescence spectra are sufficiently simple to allow the use of an interference filter in many instances. Photomultiplier detectors are used in every technique except X-ray fluorescence where proportional counting or scintillation devices are employed. Photographic recording of a complete spectrum facilitates qualitative analysis by optical emission spectrometry, but is now rarely used. 

Several kinds of detection systems have been applied to CE [1,2,43]. Based on their specificity, they can be divided into bulk property and specific property detectors [43]. Bulk-property detectors measure the difference in a physical property of a solute relative to the background. Examples of such detectors are conductivity, refractive index, indirect methods, etc. The specific-property detectors measure a physico-chemical property, which is inherent to the solutes, e.g. UV absorption, fluorescence emission, mass spectrum, electrochemical, etc. These detectors usually minimize background signals, have wider linear ranges and are more sensitive. In Table 17.3, a general overview is given of the detection methods that are employed in CE with their detection limits (absolute and relative). 

Element concentrations from XRF spectra. The pXRF spectrum consists of various peaks due to fluorescence, scattering, and detector artifacts such as escape and pileup peaks. The basic procedure for obtaining quantitative compositional information from XRF spectra is to fit a background spectrum, subtract the background, fit the remaining peaks to obtain net peak areas, and use these net areas to compute concentrations, where the concentration calculations include information on the analysis conditions and physical state and major element composition of the sample. 

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