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X-Ray Fluorescence Analytical Techniques - CNSTN : Centre ...

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I. Introduction<br />

SECTION IV<br />

WAVELENGTH DISPERSIVE X-RAY<br />

FLUORESCENCE (WD-XRF)<br />

Wavelength Dispersive X-<strong>Ray</strong> <strong>Fluorescence</strong> Spectrometry (WD-XRF) is the oldest<br />

method of measurement of X-rays, introduced commercially in the 1950’s. This name is<br />

descriptive in that the radiation emitted from the sample is collimated with a Soller collimator,<br />

and then impinges upon an analyzing crystal. The crystal diffracts the radiation to different<br />

extents, according to Bragg’s law, depending upon the wavelength or energy of the Xradiation.<br />

This angular dispersion of the radiation permits the sequential or simultaneous<br />

detection of X-rays emitted by elements in the sample. Simultaneous instruments normally<br />

contain several sets of analyzing crystals and detectors; one is adjusted for each desired<br />

analyte in the sample. These instruments tend to be very expensive, but efficient for the<br />

routine determination or preselected elements.<br />

WD-XRF is a technique that has become indispensable when fast, accurate elemental<br />

analysis is needed, as when controlling a melt in a steel works or the raw mix at a cement<br />

plant. One reason for its popularity in these applications is that its ease of use, and the<br />

ruggedness of the equipment, allows quality results to be obtained in plant conditions by<br />

operators without advanced analytical skills. Furthermore, its inherent precision, speed, and<br />

simplicity of sample preparation can often eliminate many of the problems encountered with<br />

solution based methods like ICP or Atomic Absorption spectroscopy.<br />

WD-XRF spectrometers are usually larger and more expensive than other<br />

spectrometers. Because the analyzing crystal d-spacing determines wavelength sensitivity,<br />

they are usually more sensitive than other spectrometers. To overcome losses in X-ray optics<br />

of the WD-XRF spectrometers and to maximize primary radiation intensity, X-ray tubes are<br />

usually employed. The sample is usually held under vacuum to reduce contamination and<br />

avoid absorption of light element characteristic radiation in air.<br />

Typical uses of WD-XRF include the analysis of oils and fuel, plastics, rubber and<br />

textiles, pharmaceutical products, foodstuffs, cosmetics and body care products, fertilizers,<br />

minerals, ores, rocks, sands, slags, cements, heat-resistant materials glass, ceramics,<br />

semiconductor wafers; the determination of coatings on paper, film, polyester and metals; the<br />

sorting or compositional analysis of metal alloys, glass and polymeric materials; and the<br />

monitoring of soil contamination, solid waste, effluent, cleaning fluids, sediments and air<br />

filters.<br />

II. Principle of WD-XRF<br />

WD-XRF spectrometers measure X-ray intensity as a function of wavelength. This is<br />

done by passing radiation emanating from the specimen through an analyzing diffraction

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