Micro Fluorescent X-Ray Analyzer

Abstract

AbstractA micro fluorescent X-ray analyzer with a focusing type of spectrometer has been developed to analyze samples of small amounts such as extracted inclusions or precipitates from metals or small areas in samples from 0.1 to 2.0 mm in diameter. This instrument is expected especially to analyze powder samples of small quantity because average values from such samples can be obtained and because surface conditions of the samples scarcely affect the results compared with their effect in electron probs microanalysis. A commercial X-ray tube is combined with a device of slits limiting incident X-rays, a focusing spectrometer with a Rowland circle of 4-in. radius, and a microscope of low magnification for observing the analyzing point on the samples. The wavelength range of the spectrometer with LiF and ADP analyzing crystals is from 1.20 to 9.94 Å, and, therefore, higher elements than aluminum in atomic number can be analyzed. The authors exerted their efforts to obtain the higher X-ray intensities in order to analyze smaller areas. The X-ray intensities obtained are satisfactory, except for light elements. For example, the detected X-ray intensity of pure nickel is 1650 cps with the use of a 0.1-mm diameter specimen, and that of pure sulfur is 52 cps with the use of a 0.1-ramdiameter specimen; however, with a 1-mm-diameter specimen, the intensity of pure nickel is over 5000 cps and that of pure sulfur is 1650 cps. These correspond to the intensities from 20-mm-diameter specimens of those elements when a flat-crystal spectrometer is used. The calibration curve for quantitative analysis generally varies with the sample area under analysis, but the same curves are obtained if the sample area is larger than 1 mm in diameter. Then, powder samples are analyzed quantitatively by using a plastic sample holder of 1-mm diameter and 0.3-mm depth. This instrument has good ability for microanalyzing trace elements by, for example, the ion-exchenge membrane method. The sensitivity represented is nearly 5000 cps/μg for Ni Kα from NiSO4 that is soaked and dried in thin rice paper. Some applications of the micro fluorescent X-ray analyzer to precipitates in steels and corrosion products are reported.