けい光X線分析法による窯業原料および製品中のフッ素の定量

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A test instrument was specially designed based on the investigations on the selections of X-ray tube, analyzing crystal, window material and counter gas used for the detector, and fluorine in ceramics and their raw materials was determined with special reference to the conditions for excitation of FKα, the energy resolution and the influence of particle size of samples. An end window rhodium target 3 kW X-ray tube was superior to the others in the wave distribution of incident X-rays, the intensity of excited FKα, geometrical relationship between filament, target and sample, the thickness of window material and the peak to background ratio of the fluorescent X-rays. Although mica was excellent in the resolution and LMD was also excellent in the intensity of reflected FKα, KAP was conclusively most suitable for the analyzing crystal. Polypropylene film of 1 μ thickness with vacuum evaporated aluminum was selected as the window material and a mixture of 30% CO2+70% He was used for the gas flow proportional counter so as to effectuate the gas discrimination. Large current under low potential operating condition of X-ray tube was preferable to decrease the matrix effect of coexisting elements and to increase the peak to background ratio. The peak shift of FKα, caused by the difference of chemical bonding of the fluorine compounds, was clearly recognized, and hence the setting of the detector system must be precise. The effect of particle size could be eliminated by its reduction to 2 μ. The reproducibility and the estimated analytical error were σR = 0.50% and σe = 0.112% as absolute weight percentage in fluorspar (about 33 wt%F) andσR= 0.059% and σe=0.016% in cement clinker (<1 wt%F), respectively. The determination was done within 20 minutes.

けい光X線分析法による窯業原料および製品中のフッ素の定量

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