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Detection method of nitrite ion based on rare earth metal organic framework materials

A metal-organic framework and nitrite ion technology, which is applied to the analysis of materials, material excitation analysis, and material analysis through optical means, can solve the problem of sensitive detection environment and achieve simple detection process, wide linear range, and low detection. out of bounds effect

Inactive Publication Date: 2021-05-14
TIANJIN NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, fluorescent probes are sensitive to the detection environment when detecting objects.

Method used

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  • Detection method of nitrite ion based on rare earth metal organic framework materials
  • Detection method of nitrite ion based on rare earth metal organic framework materials
  • Detection method of nitrite ion based on rare earth metal organic framework materials

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Example 1 Synthesis and determination based on rare earth metal organic framework materials

[0031] The general chemical formula of metal-organic framework materials is: {[Tb(L)(H 2 O)(DMF)]·DMF} n (In one unit, there are two DMF molecules, one participates in coordination, and the other shows as free state); This method uses rare earth salt Tb(NO 3 ) 3 4H 2 O is a rare earth source, with p-terphenyl-3,4",5-tricarboxylic acid as a ligand, the structural formula is:

[0032]

[0033] Ligand p-terphenyl-3,4",5-tricarboxylic acid (L) can be purchased from the market, or synthesized according to the following method

[0034] Add diethyl-5-iodoisophthalic acid (348mg, 1.0mmol) in 5mL DMF, then continuously add 4-bromophenylboronic acid (210mg, 1.05mmol), di(cyanophenyl)palladium dichloride ( 20mg, 0.053mmol) and potassium carbonate (400mg, 2.90mmol), the reaction was carried out under nitrogen. Stir under nitrogen overnight at 80°C, add water to stop the reaction, e...

Embodiment 2

[0043] Embodiment 2 prepares multiple solutions for subsequent implementation

[0044] (1) Weigh an appropriate amount of the rare earth cluster metal-organic framework material prepared in Example 1 and dissolve it in high-purity water to prepare a concentration of 320 mg L -1 Suspension, ultrasonically disperse evenly, and store in a dark place for later use.

[0045] (2) Weigh an appropriate amount of anion salt: NaNO 2 , NaNO 3 , NaAc, NaF, NaCl, NaBr, NaI, Na 2 SO 4 ,NaSCN,NaClO 4 ,NaIO 3 Dissolve in high-purity water, prepare a solution with a concentration of 20mM, and put it in the refrigerator for use.

[0046] (3) Weigh an appropriate amount of NaNO 2 Dissolve in high-purity water, prepare a high-standard solution with a concentration of 100mM, use this as the mother solution to dilute step by step, and prepare a series of NO with different concentrations (0.12mM-40mM) 2 - The gradient salt solution was stored in the refrigerator for later use.

Embodiment 3

[0047] The determination of the ultraviolet absorption spectrum and the fluorescence emission spectrum of the metal organic framework material used in embodiment 3

[0048] In order to investigate the fluorescence emission properties of metal-organic framework materials, the excitation wavelength of the system was determined. The absorbance of the system was detected by an ultraviolet-visible spectrophotometer, and the fluorescence intensity of the system was tested by a fluorescence spectrophotometer at an excitation wavelength of 300 nm, an excitation slit of 10 nm, an emission slit of 10 nm, and a photomultiplier tube voltage of 650V. as attached Figure 6 As shown, curve 1 is the ultraviolet absorption spectrum, and curve 2 is the fluorescence emission spectrum. The fluorescence emission intensity of the metal organic framework material used in the present invention changes with the change of the excitation wavelength, and it has a strong fluorescence intensity when the e...

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Abstract

The invention discloses a method for detecting nitrite ions based on a rare earth cluster metal organic framework material. The general chemical formula of the metal organic framework material is [Tb(L)(H 2 O)(DMF)]·DMF, the method uses rare earth salt Tb(NO 3 ) 3 4H 2 O is a rare earth source, and p-terphenyl-3,4", 5-tricarboxylic acid is used as a ligand, and is synthesized by a hydrothermal method. The rare earth cluster metal-organic framework material disclosed by the invention has unique fluorescence emission properties. Probe can realize the analytical detection for benzaldehyde.Detection method provided by the present invention has wider linear range and lower detection limit, and detection process is simple, easy and simple to handle, can realize quick and sensitive detection to nitrite ion, The complex surface modification and functionalization processes required by conventional probe materials are avoided.

Description

technical field [0001] The invention belongs to the field of preparation of rare earth metal organic framework materials and fluorescence sensing, and in particular relates to a rare earth metal organic framework material used as a fluorescent probe to selectively identify and detect nitrite ions. Background technique [0002] Metal-Organic Frameworks (MOFs) are new organic-inorganic porous materials formed by infinite coordination of metal ions and organic ligands. Due to its regular and controllable pores, large specific surface area, good thermal stability, abundant unsaturated metal sites and other excellent properties, it is a potential novel functional material in the adsorption and separation of gases, multiple It has great potential application value in phase catalysis, drug delivery, biosensing, bioimaging and other fields. In recent years, rare earth metal-organic framework complexes (Ln-MOFs) have special advantages over other metal MOFs due to the high coordinat...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/64C08G83/00
CPCC08G83/008G01N21/6428
Inventor 李妍程月丁斌
Owner TIANJIN NORMAL UNIVERSITY
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