Abstract：During the determination of aluminum in ferro-aluminum by X-ray fluorescence spectrometry(XRF) with pressed powder pellet, the detection accuracy will be reduced due to the influence of particle size effect. Usually, when a single sample preparation method with sample size less than 0.075 0 mm is adopted to overcome the particle size effect, the relative standard deviation (RSD, n=10) of X-ray fluorescence intensity of aluminum is up to 4.3%. Based on many experiments, a method of particle size recombination was proposed in the study. The mass ratio of sample with four particle sizes, i.e., 0.250-0.125 mm, 0.125-0.075 0 mm, 0.075 0-0.045 0 mm and less than 0.045 0 mm, was adjusted to 2∶2∶1∶5. Accordingly, the RSD(n=10) of X-ray fluorescence intensity of aluminum was reduced to 1.2%, which effectively reduced the influence of particle size effect. Four aspects were discussed, including the particle size recombination on determination results of aluminum, the influence of two sample preparation methods on measuring intensity, the sample surface difference of different preparation methods, and the significance difference accuracy of different analysis methods. It indicated that the proposed particle size recombination method could effectively eliminate the influence of particle size effect on the results of pressed powder pellet. The determination results of aluminum in ferro-aluminum by proposed method had no significant difference with the determination accuracy of EDTA titration.
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