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CN-119977878-B - UO2(II) fluorescence detection material, preparation method and application thereof

CN119977878BCN 119977878 BCN119977878 BCN 119977878BCN-119977878-B

Abstract

The invention discloses a fluorescent detection material of UO 2 (II), a preparation method and application thereof, and solves the technical problem of difficult sensitization in photoluminescence detection of UO 2 (II) in the prior art. The fluorescent detection material of UO 2 (II) has XRD spectrum with characteristic peaks at 2.2 DEG, 16.3 DEG, 28.3 DEG, 29.5 DEG, 41.2 DEG and 50.6 DEG, FT-IR spectrum with characteristic peaks at 1725cm ‑1 、2623cm ‑1 、2524cm ‑1 , XPS full spectrum with characteristic peaks at 1135eV, 531eV and 285 eV. The preparation method comprises the following steps of dissolving 2, 5-pyridine dicarboxylic acid N-oxide, soluble europium salt and triethylamine in water to obtain a reaction solution, placing the reaction solution into a reaction kettle for hydrothermal reaction, and collecting, washing and drying precipitate after the hydrothermal reaction is completed to obtain the fluorescent detection material of UO 2 (II). The method for detecting the UO 2 (II) in the water body comprises the steps of placing the dispersion liquid of the fluorescent detection material of the UO 2 (II) in the first aspect into the water body to be detected, testing the fluorescence intensity of the mixed liquid, and then converting to obtain the concentration of the UO 2 (II) in the water body to be detected according to the linear relation between the fluorescence intensity and the concentration of the UO 2 (II).

Inventors

  • GONG ZHENGJUN
  • TONG YUANJUN
  • LIU QIAN
  • HUANG XIAOYING
  • WANG DONGMEI

Assignees

  • 西南交通大学

Dates

Publication Date
20260512
Application Date
20250110

Claims (5)

  1. 1. The method for detecting the UO 2 (II) in the water body is characterized by comprising the steps of placing a dispersion liquid of a fluorescent detection material of UO 2 (II) into the water body to be detected, testing the fluorescence intensity of the mixed liquid, and then converting to obtain the concentration of UO 2 (II) in the water body to be detected according to the linear relation between the fluorescence intensity and the concentration of UO 2 (II); Wherein the XRD spectrum of the fluorescent detection material of UO 2 (II) has characteristic peaks at 2.2 degrees, 16.3 degrees, 28.3 degrees, 29.5 degrees, 41.2 degrees and 50.6 degrees, the FT-IR spectrum has characteristic peaks at 1725cm -1 、2623cm -1 、2524cm -1 , and the XPS full spectrum has characteristic peaks at about 1135eV, 531eV and 285 eV; The preparation method of the fluorescent detection material of UO 2 (II) comprises the following steps: Dissolving 2, 5-pyridine dicarboxylic acid N-oxide, eu (NO 3 ) 3 •6H 2 O and triethylamine in water to obtain a reaction solution; the reaction liquid is put into a reaction kettle to carry out hydrothermal reaction, the hydrothermal reaction temperature is 130-150 ℃, and the hydrothermal reaction time is 8-16 hours; After the hydrothermal reaction is finished, collecting, washing and drying the precipitate to obtain the fluorescent detection material of UO 2 (II).
  2. 2. The method for detecting UO 2 (II) in a water body according to claim 1, wherein the linear relation between the fluorescence intensity and the concentration of UO 2 (II) is y= 725.23x-318.56, x is the concentration of UO 2 (II) in the mixed solution, and y is the fluorescence intensity of the mixed solution.
  3. 3. The method for detecting UO 2 (II) in a water body according to claim 1, wherein the XPS spectrum of the fluorescent detection material of UO 2 (II) has characteristic peaks at 289.42eV, 288.11eV, 286.10eV and 284.80eV, and the XPS spectrum of O1s has characteristic peaks at 530.91eV and 531.47 eV.
  4. 4. The method for detecting UO 2 (II) in a water body according to claim 1, wherein the fluorescent detection material of UO 2 (II) is in the shape of a nano rod.
  5. 5. The method for detecting UO 2 (II) in a water body according to claim 1, wherein the concentration of 2, 5-pyridinedicarboxylic acid N-oxide in the reaction solution is 0.1 to 0.2mM, the concentration of europium ion is 0.1 to 0.2mM, and the concentration of triethylamine is 2 to 2.5mM.

Description

Fluorescent detection material of UO 2 (II), preparation method and application thereof Technical Field The invention relates to the technical field of UO 2 (II) detection, in particular to a fluorescent detection material of UO 2 (II) and a preparation method and application thereof. Background Over the past few decades, human activity has released significant amounts of uranium into the environment. Therefore, it is becoming increasingly important to develop convenient and cost-effective methods to quantify the released nuclides. UO 2 (II) (UO 22+) is the most soluble and stable toxic substance in uranium and is considered as a key index of nuclear industrial wastewater. Although the specificity and sensitivity of mass spectrometry for uranium detection are high, its complex analysis process and reliance on cumbersome instrumentation make it unusable for rapid emergency assessment in the field. In addition, the necessary pretreatment of the sample, such as filtration and digestion, presents health risks to the operator, since the sample may be radioactive. In contrast, photoluminescence (Photoluminescence, abbreviated as PL) detection methods are expected to gain a great deal of attention in UO 2 (II) analysis due to their simplicity, safety and low cost. However, many photoluminescent probes have inherent reliability problems. For the fluorescent reaction resulting from the capture of electrons by UO 2 (II), accurate quantification is highly susceptible to interference by species with similar or higher electrode potentials, such as Hg 2+ and Fe 3+. Furthermore, in the case where the in-filter effect of UO 2 (II) on the probe produces a fluorescent reaction, the absorption spectra of many co-existing species in the complex environmental matrix may overlap with the excitation or emission spectra of the photoluminescent probe, which overlap may cause unwanted in-filter effects, leading to false positive results. Thus, to successfully trigger efficient photoluminescence of UO 2 (II), not only is a matching energy level required, but also a suitable chemical environment is required, as solvents can significantly affect the sensitization efficiency. However, to date, few have been able to effectively sensitize the intrinsic emission of UO 2 (II) for monitoring purposes. Disclosure of Invention The invention mainly aims to provide a fluorescent detection material of UO 2 (II), a preparation method and application thereof, so as to solve the technical problem of difficult sensitization in photoluminescence detection of UO 2 (II) in the prior art. In order to achieve the above object, according to a first aspect of the present invention, there is provided a fluorescent detection material of UO 2 (II), the technical solution being as follows: the XRD spectrum of the fluorescent detection material of UO 2 (II) has characteristic peaks at 2.2 degrees, 16.3 degrees, 28.3 degrees, 29.5 degrees, 41.2 degrees and 50.6 degrees, the FT-IR spectrum has characteristic peaks at 1725cm -1、2623cm-1、2524cm-1, and the XPS full spectrum has characteristic peaks at about 1135eV, 531eV, 402eV and 285 eV. As a further improvement of the fluorescent detection material of UO 2 (II), the XPS spectrum of C1s has characteristic peaks at 289.42eV, 288.11eV, 286.10eV and 284.80eV, and the XPS spectrum of O1s has characteristic peaks at 530.91eV and 531.47 eV. As a further improvement of the above-mentioned fluorescent detection material of UO 2 (II), it is in the shape of a nano rod. In order to achieve the above object, according to a second aspect of the present invention, there is provided a method for preparing a fluorescent detection material of UO 2 (II), comprising the steps of: The preparation method of the fluorescent detection material of UO 2 (II) according to the first aspect includes the following steps: Dissolving 2, 5-pyridine dicarboxylic acid N-oxide, soluble europium salt and triethylamine in water to obtain a reaction solution; the reaction liquid is put into a reaction kettle for hydrothermal reaction; After the hydrothermal reaction is finished, collecting, washing and drying the precipitate to obtain the fluorescent detection material of UO 2 (II). As a further improvement of the preparation method of the fluorescent detection material of UO 2 (II), the concentration of 2, 5-pyridine dicarboxylic acid N-oxide in the reaction solution is 0.1-0.2 mM, the concentration of europium ions is 0.1-0.2 mM, and the concentration of triethylamine is 2-2.5 mM. As a further improvement of the preparation method of the fluorescent detection material of UO 2 (II), the hydrothermal reaction temperature is 130-150 ℃ and the hydrothermal reaction time is 8-16 hours. In order to achieve the above object, according to a third aspect of the present invention, there is provided a method for detecting UO 2 (II) in a water body, the technical scheme being as follows: the method for detecting the UO 2 (II) in the water body comprises the step