Apparatus for Vacuum X-Ray Fluorescence Analysis of Light Elements

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Abstract
Air absorption in the conventional x‐ray fluorescence analysis equipment limits detection to elements heavier than calcium. To avoid absorption of the longer‐wavelength x‐rays from lighter elements, a vacuum system, or one filled with H2 or He, is required. A vacuum apparatus has been developed for the analysis of elements from magnesium to titanium. It contains the x‐ray tube for exciting fluorescence; a specimen holder for six specimens; a collimator to limit the fluorescent radiation to a parallel beam; and a single‐crystal, Geiger counter spectrometer to analyze the radiation. A pressurized, double‐film, nitrocellulose window is used for the Geiger counter because the usual mica windows are opaque to radiation from elements lighter than sulfur. For calcium Kα, the increase in intensity resulting from evacuating the chamber is 100‐fold, with far greater increases for the lighter elements. Alkali halides and gypsum were tested as analyzing crystals. An application of the equipment to the measurement of sulphur in oil indicates that 0.5 percent sulfur can be detected with ±0.03 percent accuracy in 5 to 10 minutes.