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Method for rapidly detecting fluorinions in environment

A technology for detecting environment and fluoride ions, applied in the field of analytical chemistry, can solve the problems of low sensitivity, high cost of fluoride ion nuclear magnetic resonance, limited application and development, etc., and achieve the effect of simple operation, rapid and highly selective detection, and good stability.

Inactive Publication Date: 2018-06-15
ANYANG INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are many methods for detecting fluoride ions, such as capillary electrophoresis, nuclear magnetic resonance, etc., but unfortunately, the sensitivity of capillary electrophoresis is low, the reproducibility of the fluoride ion selective electrode is poor, and the cost of fluoride ion NMR is high, which severely limits its use. Application and Development

Method used

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  • Method for rapidly detecting fluorinions in environment
  • Method for rapidly detecting fluorinions in environment
  • Method for rapidly detecting fluorinions in environment

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Preparation of colorimetric probes:

[0037]

[0038] Dissolve 185mg (1mmol) of 2-amino-6-chlorobenzothiazole, 232mg (1.2-1.5mmol) of 4-(diethylamino) salicylaldehyde and 3 drops of acetic acid in 50mL of absolute ethanol, and heat to reflux for 10 reactions After 1 hour, the crude product was obtained by filtration under reduced pressure, and then recrystallized with absolute ethanol to obtain a light yellow pure product with a yield of 91%.

[0039] 1 HNMR (400MHz, CDCl 3 ):12.64(s,1H),8.93(s,1H),7.79-7.75(m,2H),7.40-7.37(dd,J 1 =8.4Hz,J 2 =2Hz, 1H), 7.26-7.24(d, J=8.4Hz, 1H), 6.33-6.19(dd, J 1 =9.2Hz,J 2 =2.4Hz, 1H), 6.184(s, 1H), 3.47-3.41(q, J=7.2Hz, 4H), 1.26-1.22(t, J=7.2Hz, 6H); 13 CNMR (101MHz, CDCl 3 ): 136.22, 129.91, 127.07, 122.66, 121.15, 108.78, 105.64, 97.46, 45.01, 12.73; ESI-MS calculated value: 359.9, measured value: 359.9.

Embodiment 2

[0041] Test method: (a) Different concentrations of F - (0-10μM) compared to the influence of color fluorescent probe (10μM) on the absorption spectrum; (b) different concentrations of F - (0-10 μM) compared to the effect of the color fluorescent probe (10 μM) on the emission spectrum. The above determinations were carried out in DMSO, and all spectroscopic tests were performed at 25°C F - Measured immediately after addition. See results figure 1 and figure 2 .

[0042] From figure 1 It can be seen that with the F in the colorimetric fluorescent probe solution - As the concentration increases, the peak at 445nm of the absorption spectrum decreases, while a new peak occurs at 516nm, and the intensity increases, and at 0-10μM F - There is a good linear relationship between the concentration range and the absorption value. From figure 2It can be seen that with the F in the colorimetric fluorescent probe solution - As the concentration increases, the peak at 500nm of t...

Embodiment 3

[0044] Effects of different analytes (20 μM) on the UV absorption spectrum and fluorescence emission of the probe (10 μM). Analytes include: Fluoride F - , Chloride ion Cl - , bromide ion Br - , iodide ion I - , hydrogen sulfate ion HSO 4 - , nitrate ion NO 3 - , dihydrogen phosphate ion H 2 PO 4 - and acetate ion AcO - , their concentration was 20 μM. All test conditions are done in DMSO, and all spectra are at 25°C F - Measured immediately after addition. Pipette 100 μL of the probe stock solution (1 mM) into a 10 mL volumetric flask, dry it, add 9 mL of dimethyl sulfoxide, then pipette 20 μL of the above analyte stock solution (10 mM) into the volumetric flask, and then use dimethylsulfoxide Dilute to 10mL with sulfoxide. Shake well and measure immediately. The result is as image 3 and Figure 4 shown.

[0045] From image 3 and Figure 4 It can be seen that the probe has high selectivity to fluoride ions and can react with fluoride ions transferably. ...

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Abstract

The invention discloses a method for rapidly detecting fluorinions in an environment, and belongs to the technical field of analytical chemistry. The method comprises the following steps: mixing a sample to be detected with a colorimetric probe in an organic solvent; measuring the ultraviolet absorption spectrum at 350-600 nm and the fluorescence emission spectrum at 400-680 nm; and calculating the concentration of the fluorinions in the sample to be detected according to the measured ultraviolet absorption intensity at 450 nm and the measured fluorescence emission intensity at 555 nm. The method can highly selectively identify the fluorinions, and also can quantitatively and qualitatively analyze the fluorinions in a naked eye observation manner. The method achieves fast effective response to the fluorinions and real-time detection of the fluorinions.

Description

technical field [0001] The invention relates to a method for rapidly detecting fluoride ions in the environment, in particular to a method for detecting fluoride ions using a thiazole Schiff base as a colorimetric fluorescent probe for fluoride ions, and belongs to the technical field of analytical chemistry. Background technique [0002] In the environment and organisms, anions are ubiquitous, such as air, water, and soil in the environment, in organs, cells, and even cell fluids of the human body, and play an extremely important role in the environment and ecosystem. Role. Fluoride ion, which has the smallest radius among anions, is an essential element for biological life activities, and plays an important role in dental health care and osteoporosis treatment. In order to contain sufficient fluoride ions in the human body, people use it as an important additive, often used in toothpaste, medicine and drinking water. However, excessive fluorine not only has toxic effects...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/64G01N21/33
CPCG01N21/33G01N21/643
Inventor 王芳杨立国王凯王书红王建广王艳飞郭尧杜亚威牛永生侯绍刚
Owner ANYANG INST OF TECH
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