X-luminoscope fusion sample preparation method

Abstract

The invention discloses an X-luminoscope fusion sample preparation method, comprising the following steps: grinding a solid sample into powder of not less than 200 meshes for later use, wiping a crucible, a stirrer and a medicine spoon to be clean by using alcohol, placing in an oven for drying for 30min and more, taking out and placing on a tray, wiping the inner wall of a die to be clean by using alcohol, naturally withering for later use; weighing a certain mass of PE material to be put into a crucible, heating until the solvent is completely fused; weighing a certain mass of sample powder in S1 to place in a crucible in the S4, turning on the stirrer, stirring while heating, stopping stirring and heating after 30min; fetching melt at the upper layer in the crucible in S5 with a medicine spoon in a die in the S3, wherein the melt is about 2 / 3 of the height of the die, naturally cooling to completely solidify to obtain the sample sheet. The borate flux is replaced by the PE material, the manufactured sample sheet is hard to break, crack and pollute, easy to de-mold and store, the sample preparation time is effectively shortened, and the sample preparation cost is greatly reduced.

Description

technical field [0001] The invention relates to a melting sample preparation method for an X fluorescence instrument. Background technique [0002] At present, the X-ray fluorescence instrument fusion sample preparation method is mainly the borate fusion sample preparation method. The operation process is as follows: mix the sample and borate flux, heat the mixture in a platinum crucible until the mixture melts, pour the melt into dilute acid, and Stir until completely dissolved, the liquid mixed melt is poured into a platinum mold, and after cooling, a solid melt sheet with a flat and smooth surface is obtained. The resulting solution will contain all the elements in the original sample, unless the sample size exceeds the maximum solubility of the sample in the solvent; the inventor finds in the course of the research that the borate flux used in the borate fusion sample preparation method has Very high hygroscopicity, so it is difficult to preserve in the air, and the pre...

AI Technical Summary

Problems solved by technology

The resulting solution will contain all the elements in the original sample, unless the sample size exceeds the maximum solubility of the sample in the solvent; the inventor finds in the course of the research that the borate flux used in the borate fusion sample preparation method has Very high hygroscopicity, so it is difficult to preserve in the air, and the prepared samples are easily dampened, so that the calibration samples must be remelted before reuse, which increases the complexity of the experiment

In addition, the samples prepared by this method are prone to adhesion, crystallization, and bursting, and the success rate of sample preparation is not high.

In this method, the sample needs to be oxidized before melting, and the temperature of the melting sample must reach more than 1,000 degrees. The crucible used must be a platinum crucible, which requires high sample preparation and high cost.