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X-ray fluorescence spectrum trace sample preparation and sample preparing method thereof

A fluorescence spectrum and X-ray technology, which is applied in the field of X-ray fluorescence spectrum micro-analysis of micro-sample sample preparation and sample preparation, can solve the problems of unstable detection results of boric acid materials, insufficient measurement intensity, uneven detection light intensity, etc. , to achieve strong practicability and promotion value, good test results, easy and practical operation

Inactive Publication Date: 2009-04-22
PANGANG GROUP RESEARCH INSTITUTE CO LTD +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to overcome the unevenness of the detection light intensity in the prior art when using the spectrum to analyze trace samples, the measurement intensity is not large enough, the sensitivity is not high, and it cannot be continuous Insufficient analysis and the use of large amounts of boric acid materials caused unstable test results, and a new sample preparation and sample preparation method for microanalysis of X-ray fluorescence spectroscopy was proposed

Method used

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  • X-ray fluorescence spectrum trace sample preparation and sample preparing method thereof
  • X-ray fluorescence spectrum trace sample preparation and sample preparing method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0015] (1) Get 12 grams of boric acid powder with a purity of 99.5%, put it into a standard mold with a diameter of 40 mm and punch it into boric acid sheets, and the thickness of the sheet is 3 mm;

[0016] (2) Take three points with the same arc length on the concentric circle of 1 / 2 radius of the boric acid sheet, use a drill bit with a diameter of 2mm to drill holes, two holes with a depth of 2.5mm, and one with a depth of 2.0mm hole;

[0017] (3) Take sample 1, 0.0083g, put it into a hole with a diameter of 2mm and a depth of 2.5mm on the boric acid sheet, tamp and flatten it with a thin steel rod while loading, until the sample is kept at the same height as the edge of the hole; Sample 2, 0.0073g, and sample 3, 0.0040g, were successively loaded into the other two holes with a depth of 2.5mm and a depth of 2.0mm according to the same method as above.

[0018] (4) put the packed sample preparation on the X-ray fluorescence spectrometer to carry out the detection and analy...

Embodiment 2

[0023] (1) Get 10 grams of dried boric acid powder with a purity of 99.8%, and put it into a 30 mm standard mold with a bottom diameter of 30 mm to stamp and form boric acid sheets. The molding pressure is 45 tons, and the sheet thickness is 3 mm.

[0024] (2) Use a drill bit with a diameter of 3 mm to drill a hole at the center of the bottom surface of the boric acid sheet, and the depth is 3 mm.

[0025] (3) Take 0.0095g of anthracite sample, put it into the sample hole of the boric acid sheet with a diameter of 3mm and a depth of 3mm, tamp and flatten it with a thin steel rod while loading, until the sample is at the same height as the edge of the hole.

[0026] (4) the packed anthracite sample sample preparation is placed on the X-ray fluorescence spectrometer to carry out the detection and analysis of the sample, and the detection and analysis results are as follows:

[0027]

[0028] Due to the use of micro-sample preparation, X-ray fluorescence micro-area analysis ca...

Embodiment 3

[0030] (1) Get 11 grams of boric acid powder with a purity of 99.6%, put it into a standard mold with a diameter of 40 mm and punch it into a boric acid sheet, and the thickness of the sheet is 4 mm;

[0031] (2) Take four points with equal arc lengths on the concentric circles with a radius of 25mm of the boric acid sheet, take a point at the center point, and use drill bits with diameters of 1mm, 1.5mm, and 2mm to drill holes, and the hole depths are 2.5mm Two holes, two holes of 2.0mm, the depth of the center point is 1.5mm;

[0032] (3) Take sample 1, 0.009g, and put it into two holes with a diameter of 2mm and a depth of 2.5mm on the boric acid sheet; take sample 2, 0.0083g, and put it into two holes with a diameter of 1.5mm and a depth of 2mm on the boric acid sheet , Take sample 2, 0.0075g, put it into the central hole with a diameter of 1mm and a depth of 1.5mm on the boric acid sheet, and use the same method to compact it with a thin steel rod and flatten it until the...

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Abstract

The invention discloses an X ray fluorescence spectrum micro sample preparation and a preparation method thereof, which comprises the following steps: boric acid powder is punched, formed in a standard mold, and made into boric acid tablets; and then the diameter and the depth of the holes of samples are determined according to the number of the samples to be tested and the quantity of each kind of detected samples; a drilling device which has the equal diameter with the holes of the samples is selected; a plurality of sample wells which are uniformly distributed or symmetrical, or unevenly distributed or unsymmetrical are bored on the boric acid tablets along the circle less than the excircle diameter of the boric acid tables and the bottoms of the sample wells are impervious; then each kind of different samples to be tested are loaded into the corresponding sample wells, compressed and planished; finally, the sample preparation is put on the X ray fluorescence spectrometer for detecting and analyzing. The invention can detect and analyze micro samples, has the advantages of large measuring strength, high sensitivity, simultaneously continuous analysis on a plurality of samples, saving usage amount of boric acid, simple operation, high detection efficiency, etc.

Description

technical field [0001] The invention relates to the technical field of spectral analysis and detection, in particular to a micro-sample preparation method for X-ray fluorescence spectrum micro-analysis and a sample preparation method. Background technique [0002] The qualitative and quantitative analysis of trace samples has always been a difficult problem. The methods currently used are: one is the ICP method, which is not easy to analyze because it needs to digest the sample (dissolve with acid) and introduce more interfering elements. In addition, the analysis time of the ICP method is longer. long. In addition, X-ray fluorescence spectrometer is used for qualitative and quantitative analysis of trace samples. The usual methods are as follows, one is to put the sample into the center of a special sample device, the other is to put the sample into the center of the mold, use boric acid as the bottom to press the tablet, and then use a small-diameter sample box mask and a...

Claims

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Application Information

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IPC IPC(8): G01N1/36G01N23/223
Inventor 周铭徐本平
Owner PANGANG GROUP RESEARCH INSTITUTE CO LTD
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