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Elemental Detection Method Based on Total Reflection X-ray Fluorescence Analysis

A technology of fluorescence analysis and detection method, which is applied in the direction of using wave/particle radiation for material analysis, analyzing materials, measuring devices, etc. It can solve the problems of test result error, TXRF instrument result error, TXRF instrument linear reduction, etc.

Active Publication Date: 2019-02-26
YIWEN ENVIRONMENTAL SCI & TECH GUANGZHOU
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Based on the above-mentioned total reflection principle, when using the TXRF instrument to test elements in soil or sewage samples, especially trace elements, the thickness, area and uniformity of the sample film will have a great impact on the test results , the difference in each film production will lead to a decrease in the linearity of the TXRF instrument, resulting in a large error in the test results
In addition, the TXRF instrument is mostly used in vehicle environment testing, and the fluctuation of the TXRF instrument itself caused by environmental factors will also bring certain errors to the results.

Method used

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  • Elemental Detection Method Based on Total Reflection X-ray Fluorescence Analysis

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] This embodiment is based on the element detection method of total reflection X-ray fluorescence analysis, comprising the following steps:

[0035] Preparation of yttrium nitrate internal standard solution:

[0036] (1) Measure 25mL of acetylacetone analytical grade reagent and add it to a 250mL volumetric flask, dilute to 250mL with analytical pure MIBK, and mix thoroughly to make a 10% acetylacetone-MIBK mixture.

[0037] (2) Accurately measure the yttrium nitrate standard solid of 0.1077g, join in the MIBK mixed solution of above-mentioned acetylacetone, fully shake, make the yttrium nitrate solid dissolve completely, obtain internal standard solution, then the yttrium concentration in this internal standard solution is 100mg / L.

[0038] Detection:

[0039] (1) Take 200 μL of the sample solution to be tested (soil digestion solution, containing lead element, obtained by extraction with analytically pure MIBK), add 10 μL of the mother solution, and prepare a test sol...

Embodiment 2

[0043] This embodiment is based on the element detection method of total reflection X-ray fluorescence analysis, comprising the following steps:

[0044] Preparation of yttrium nitrate internal standard solution:

[0045] (1) Measure 12.5mL acetylacetone analytical grade reagent and add it to a 250mL volumetric flask, dilute to 250mL with analytical pure MIBK, and mix thoroughly to make a 5% acetylacetone-MIBK mixture.

[0046] (2) Accurately measure the yttrium nitrate standard solid of 0.1077g, join in the MIBK mixed solution of above-mentioned acetylacetone, fully shake, make the yttrium nitrate solid dissolve completely, obtain internal standard solution, then the yttrium concentration in this internal standard solution is 100mg / L.

[0047] Detection:

[0048] (1) Take 200 μL of the sample solution to be tested (soil digestion solution, the same as in Example 1), add 20 μL of internal standard solution, and prepare a test solution containing about 10 mg / L of internal sta...

Embodiment 3

[0052] This embodiment is based on the element detection method of total reflection X-ray fluorescence analysis, and the preparation of the yttrium nitrate internal standard solution is the same as that in Example 3, including the following steps:

[0053] Preparation of yttrium nitrate internal standard solution:

[0054] (1) Measure 37.5mL of acetylacetone analytical grade reagent and add it to a 250mL volumetric flask, dilute to 250mL with analytical pure MIBK, and mix thoroughly to make a mixed solution of acetylacetone and MIBK with a volume concentration of 15%.

[0055] (2) Accurately measure the yttrium nitrate standard solid of 0.1077g, join in the MIBK mixed solution of above-mentioned acetylacetone, fully shake, make the yttrium nitrate solid dissolve completely, obtain internal standard solution, then the yttrium concentration in this internal standard solution is 100mg / L.

[0056] Detection:

[0057](1) Take 200 μL of the sample solution to be tested (soil diges...

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Abstract

The invention relates to a method for detecting elements on the basis of total-reflection X-ray fluorescence analysis. The method includes steps of acquiring to-be-detected samples and adding solvents into the to-be-detected samples to obtain to-be-detected sample solution; adding internal standard liquid into the to-be-detected sample solution to obtain to-be-detected liquid; adding the to-be-detected liquid onto sample slide glass dropwise, drying the to-be-detected liquid to form films and detecting the films by the aid of total-reflection X-ray fluorescence spectrometer. The internal standard liquid contains yttrium elements with the concentration of 50-150 mg / L. The method for detecting the elements has the advantages that TXRF (total-reflection X-ray fluorescence analysis) is used as a detection process, solution containing the yttrium elements with the certain concentration is added into the to-be-detected sample solution in the form of the internal standard liquid, and accordingly change of peak areas of the to-be-detected elements can be corrected; tests carried out by TXRF instruments are excellent in linearity by the aid of correcting algorithms, interference of environmental factors can be correspondingly eliminated, accordingly, the accuracy of ultimate test results can be greatly improved, and the method is particularly applicable to detecting trace elements in soil or sewage.

Description

technical field [0001] The invention relates to element determination, in particular to an element detection method based on total reflection X-ray fluorescence analysis. Background technique [0002] The total reflection X-ray fluorescence spectrometer (TXRF) is currently being more and more widely used in the field of on-site emergency testing due to its advantages of high test accuracy and easy portability. [0003] The excitation principle of the TXRF instrument is different from that of the ordinary XRF instrument. It requires the X-ray to grazing the surface of the sample test platform at an angle lower than the critical angle in air or vacuum, eliminating the coherence of the primary X-ray on the reflector. Or irrelevant scattering phenomenon, which reduces the scattering background and improves the lower limit of detection. [0004] Based on the above-mentioned total reflection principle, when using the TXRF instrument to test elements in soil or sewage samples, esp...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N23/223
CPCG01N23/223G01N2223/076
Inventor 石平徐剑飞
Owner YIWEN ENVIRONMENTAL SCI & TECH GUANGZHOU