CN113310962A - Rapid colorimetric fluorescent hypochlorite detection reagent - Google Patents
Rapid colorimetric fluorescent hypochlorite detection reagent Download PDFInfo
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
Abstract
The invention provides a rapid colorimetric fluorescent hypochlorite detection reagent which is prepared from a naphthol compound, an organic solvent and an inorganic solvent. The reagent is contacted with hypochlorite, and within 3s, the colorimetric and fluorescent lights are immediately changed from colorless to bright colors, and can be directly observed by naked eyes without complex analysis equipment, so that the hypochlorite is analyzed at low cost and in real time. Overcomes the defects of long reaction time, only colorimetric or fluorescent single signal in signal response and color fading or discoloration phenomenon based on the prior hypochlorite detection technology, and provides an effective technical means for hypochlorite detection and analysis. Provides effective technical support for trace detection of hypochlorite in non-standard explosives.
Description
Technical Field
The invention belongs to the field of nonstandard explosive detection, and provides a rapid colorimetric fluorescent hypochlorite detection reagent.
Background
The non-standard explosive is easy to obtain raw materials and simple to prepare. The detection of non-standard explosives is of great significance to analysis. Hypochlorite can be used as a raw material of non-standard explosives due to the oxidizability, and can be simply processed with edible salt (sodium chloride as a main component) essential in life to prepare chlorate and perchlorate (Defence Today,2008,4649:46-49) which are raw materials of non-standard explosives with stronger power. In addition, the excessive presence of hypochlorite, one of the important active oxygen species in biological systems, can cause a variety of diseases including cystic fibrosis, kidney disease, cancer, and the like. Therefore, the detection of the sodium hypochlorite is of great significance in the fields of public safety and life health.
At present, the colorimetric detection technology of hypochlorite is mainly carried out by utilizing noble metal etching or colorimetric reaction based on probe molecules. Wherein, the noble metal etching method utilizes the strong oxidation of hypochlorite to etch noble metals such as Ag, Au and the like to generate the change of absorbance so as to achieve the detection purpose (Analytical Methods,2017,9(21): 3151-; colorimetric reactions based on probe molecules utilize oxidation by hypochlorite to cleave thiolactones or carbon-carbon double bonds to form epoxy groups, thereby altering the electron distribution of the chromophore, resulting in a color change (Sensors and activators B: Chemical,2019,283: 524-. The above method is not only expensive, but also poor in stability and interference resistance. Most of fluorescent detection probe molecules of hypochlorite are complicated in synthesis steps, are mainly based on fluorescence quenching or fluorescence spectrum shift to realize detection (Sensors and activators B: Chemical,2018,255:666-671), are not beneficial to trace analysis, and are easy to cause missed detection and false detection due to the difficulty in identifying detection signals.
Based on the detection, the invention develops a rapid colorimetric fluorescent hypochlorite detection reagent. The reagent utilizes hypochlorite oxidation characteristics, naphthalene with high quantum yield is taken as a fluorophore, and a phenolic hydroxyl group is taken as a recognition group to design a naphthol molecule. When the reagent is used for detecting hypochlorite, two signals of colorimetric and fluorescent can be responded from the absence to the presence, so that the aim of detecting hypochlorite by fast colorimetric fluorescence is fulfilled. In addition, the reagent has the advantages of rapid reaction, high sensitivity and simple operation, and is favorable for large-scale popularization and application.
Disclosure of Invention
The invention aims to provide a rapid colorimetric fluorescent hypochlorite detection reagent, which is prepared from a naphthol compound, an organic solvent and an inorganic solvent. The reagent is contacted with hypochlorite, and within 3s, the colorimetric and fluorescent lights are immediately changed from colorless to bright colors, and can be directly observed by naked eyes without complex analysis equipment, so that the hypochlorite is analyzed at low cost and in real time. Overcomes the defects of long reaction time, only colorimetric or fluorescent single signal in signal response and color fading or discoloration phenomenon based on the prior hypochlorite detection technology, and provides an effective technical means for hypochlorite detection and analysis.
The invention relates to a rapid colorimetric fluorescent hypochlorite detection reagent, which is prepared from a naphthol compound, an organic solvent and an inorganic solvent, wherein:
the naphthol compound is 1-naphthol, 2, 3-dihydroxynaphthol, binaphthol, bromonaphthol, chloronaphthol, acetonaphthol, tetrahydronaphthol, S-binaphthol, 4-bromonaphthol or nitro-2-naphthol, and the content of the naphthol compound in the solution is 0.1-40 mmol/L;
the organic solvent is dimethyl sulfoxide, methanol, ethanol, acetonitrile, acetone, ethyl acetate, dichloromethane, petroleum ether or tetrahydrofuran, and the concentration is 10-80%;
the inorganic solvent is ultrapure water;
diluting the organic solvent with ultrapure water to the concentration of 10% -80% to obtain a mixed solvent;
weighing 0.1-100 mg of naphthol compound and dissolving in the mixed solvent to obtain the reagent for rapid colorimetric fluorescence detection of hypochlorite with the concentration of 0.1-40 mmol/L.
The invention relates to a rapid colorimetric fluorescent hypochlorite detection reagent, which is applied to a colorimetric and fluorescent detection method of hypochlorite, and comprises the following steps:
preparing a detection reagent:
diluting the organic solvent with ultrapure water to the concentration of 10%, 15%, 20%, 25%, 30%, 35%, 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75% and 80%, thus obtaining a mixed solvent with the concentration of the organic solvent of 10% -80%;
weighing 0.1mg, 0.5mg, 1mg, 3mg, 5mg, 7mg, 9mg, 12mg, 15mg, 20mg, 25mg, 30mg, 40mg, 50mg and 100mg of naphthol compound and dissolving in an organic mixed solvent to obtain hypochlorite detection reagents with the concentrations of 0.1mmol/L, 0.2mmol/L, 0.6mmol/L, 1mmol/L, 1.5mmol/L, 2mmol/L, 5mmol/L, 10mmol/L, 15mmol/L, 20mmol/L, 25mmol/L, 30mmol/L, 35mmol/L and 40 mmol/L;
the prepared detection reagent is applied to colorimetric and fluorescent detection of hypochlorite:
sodium hypochlorite was weighed and dissolved in ultrapure water to prepare a solution having a concentration of 0.1. mu.M, 1. mu.M, 6. mu.M, 8. mu.M, 10. mu.M, 18. mu.M, 20. mu.M, 30. mu.M, 40. mu.M, 60. mu.M, 90. mu.M, 100. mu.M, 200. mu.M, 300. mu.M, 400. mu.M, 500. mu.M, 600. mu.M, 700. mu.M, 800. mu.M, 900. mu.M, 1000. mu.M, 2000. M, 3000. mu.M, 4000. mu.M, 5000. mu.M, 1mM, 2mM, 4mM, 6mM, 8mM, 10mM, 12mM, 14mM, 16mM, 18mM, 20mM, 22mM, 24mM, 26mM, 28mM, and 30mM of sodium hypochlorite;
measuring 1.5mL of detection reagent in a quartz cuvette by using a pipette, adding 20mL of sodium hypochlorite solutions with different concentrations, testing the spectral change after reaction by using an ultraviolet visible absorption spectrometer and a fluorescence spectrometer after 3s, recording the colorimetric and fluorescence change process in the reaction process by using a digital camera, shooting the colorimetric and fluorescence pictures after reaction, and testing the detection limit of the reagent by naked eyes.
And (3) respectively wiping trace amounts of sodium hypochlorite, calcium hypochlorite, potassium chlorate, potassium perchlorate and ammonium chloride by using sampling paper, dripping 1-2 drops of detection reagent, observing color change, and determining whether hypochlorite is contained.
The rapid colorimetric fluorescent hypochlorite detection reagent can detect hypochlorite in liquid and trace solid hypochlorite residues. In addition, the reagent has excellent selectivity for common inorganic salt interferents.
The invention relates to a rapid colorimetric fluorescent hypochlorite detection reagent, which is mainly used for detecting hypochlorite components in non-standard explosives and solves the problem that the conventional hypochlorite detection reagent cannot be used for detecting and identifying naked eyes directly, rapidly and at low cost.
Compared with the prior art, the invention has the beneficial effects that:
1. the raw materials of the reagent used in the invention can be purchased from commercial markets;
2. the detection reagent can detect hypochlorite by using signals of colorimetric signal and fluorescence signal at the same time;
3. the detection reagent can sensitively and selectively detect hypochlorite;
4. the detection reagent disclosed by the invention is quick in reaction, and hypochlorite can be detected within 3 s;
5. the detection reagent disclosed by the invention is used for detecting hypochlorite, complex analysis equipment is not needed, and the hypochlorite can be directly identified and detected by naked eyes.
Drawings
FIG. 1 is a graph showing fluorescence spectra of 20 mmol/L1-naphthol in 20% dimethylsulfoxide and water mixed solvent for 0-5000mM sodium hypochlorite, and fluorescence images before and after reaction with 1000mM sodium hypochlorite;
FIG. 2 is a graph showing the UV-visible spectrum of 20 mmol/L1-naphthol in 20% dimethylsulfoxide and water mixed solvent for 0-5000mM sodium hypochlorite, and colorimetric images before and after reaction with 1000mM sodium hypochlorite;
FIG. 3 is a colorimetric and fluorescent image of 20 mmol/L1-naphthol detected in 20% mixed solvent of dimethyl sulfoxide and water in 0-5000mM sodium hypochlorite;
FIG. 4 is a graph showing fluorescence spectra of 1 mmol/L2, 3-dihydroxynaphthol in 10% dimethylsulfoxide and water mixed solvent for 0-5000mM sodium hypochlorite, and fluorescence images before and after reaction with 100mM sodium hypochlorite;
FIG. 5 is a graph showing the UV-Vis spectra of 1 mmol/L2, 3-dihydroxynaphthol in 10% dimethylsulfoxide and water mixed solvent for 0-30mM sodium hypochlorite, and colorimetric images before and after reaction with 16mM sodium hypochlorite;
FIG. 6 is a colorimetric image of 1 mmol/L2, 3-dihydroxynaphthol in 10% dimethylsulfoxide and water mixed solvent for detecting 0-30mM sodium hypochlorite and a fluorescence image for detecting 0-5000mM sodium hypochlorite according to the present invention;
FIG. 7 is a colorimetric and fluorescent image of 10 mmol/L2, 3-dihydroxynaphthol of the present invention in 80% dimethylsulfoxide and water mixed solvent for detecting sodium hypochlorite trace solids.
Detailed Description
The present invention will be further illustrated by the following specific examples, but the present invention is not limited to these examples.
Example 1
Weighing 40mg of 1-naphthol and dissolving in a mixed solvent of dimethyl sulfoxide and ultrapure water with the concentration of 20% at room temperature, and uniformly stirring to obtain a rapid colorimetric fluorescent hypochlorite detection reagent with the concentration of 20 mmol/L;
measuring 1.5mL of the prepared hypochlorite detection reagent in a quartz cuvette by using a liquid-transferring gun, adding 20mL of sodium hypochlorite solution with different concentrations of 0-5000 [ mu ] M, testing the spectral change after reaction by using a fluorescence spectrometer after 3s, and recording the fluorescence color change before and after reaction by using a camera, wherein the fluorescence color change is shown in figure 1;
as can be seen from FIG. 1, the fluorescence spectrum peak intensity after the reaction gradually increases with the increase of hypochlorite concentration, and the fluorescence color changes from colorless before the reaction to bright green;
measuring 1.5mL of the prepared hypochlorite detection reagent in a quartz cuvette by using a liquid-transferring gun, adding 20mL of sodium hypochlorite solution with different concentrations of 0-5000 [ mu ] M, testing the change of an absorption spectrum after reaction by using an ultraviolet-visible absorption spectrometer after 3s, and recording the color change of the color before and after the reaction by using a camera, wherein the color change is shown in figure 2;
as can be seen from FIG. 2, the intensity of the UV-visible absorption peak after the reaction increases with the hypochlorite concentration, and the colorimetric color changes from colorless to vivid orange-red before the reaction. The colorimetric fluorescence image of the hypochlorite detection reagent after detecting sodium hypochlorite solutions with different concentrations of 0-5000 μ M is recorded by a camera, and as can be seen from fig. 3, the colorimetric and fluorescent colors gradually deepen as the concentration of sodium hypochlorite increases.
Example 2
Weighing 0.1mg of 2, 3-dihydroxynaphthol and dissolving in a mixed solvent of dimethyl sulfoxide and ultrapure water with the concentration of 10% at room temperature, and uniformly stirring to obtain a rapid colorimetric fluorescent hypochlorite detection reagent with the concentration of 1 mmol/L;
measuring 1.5mL of the prepared hypochlorite detection reagent in a quartz cuvette by using a liquid-transferring gun, adding 20mL of sodium hypochlorite solution with different concentrations of 0-5000 [ mu ] M, testing the spectral change after reaction by using a fluorescence spectrometer after 3s, and recording the fluorescence color change before and after reaction by using a camera, wherein the fluorescence color change is shown in figure 4;
as can be seen from FIG. 4, the fluorescence spectrum peak intensity after the reaction gradually increases with the increase of hypochlorite concentration, and the fluorescence color changes from colorless before the reaction to blue-purple;
measuring 1.5mL of the prepared hypochlorite detection reagent in a quartz cuvette by using a liquid-transferring gun, adding 20mL of sodium hypochlorite solution with different concentrations of 0-30mM, testing the change of the absorption spectrum after reaction by using an ultraviolet-visible absorption spectrometer after 3s, and recording the color change of the color before and after the reaction by using a camera, wherein the color change is shown in figure 5;
as can be seen from FIG. 5, the intensity of the UV-visible absorption peak after the reaction increased with increasing hypochlorite concentration, and the colorimetric color changed from colorless to brown before the reaction. The colorimetric fluorescence images of the hypochlorite detection reagent after detecting sodium hypochlorite solutions with different concentrations are recorded by a camera, and as can be seen from fig. 6, the colorimetric and fluorescent colors gradually deepen as the concentration of the sodium hypochlorite increases;
wiping sodium hypochlorite solid particles with different masses by using sampling paper, dripping 1-2 drops of detection reagent, observing the color change, and as can be seen from figure 7, changing the colorimetric phenomenon of the sodium hypochlorite detection reagent for detecting trace sodium hypochlorite solid particles from colorless to brown and changing the fluorescent phenomenon from colorless to bluish purple; when the mass of the sodium hypochlorite solid is 10ng, obvious characteristic brown can be detected, and when the mass of the sodium hypochlorite solid is 0.5ng, obvious bluish purple fluorescence can be observed, which indicates that the reagent has higher detection sensitivity.
Example 3
Weighing 100mg of binaphthol at room temperature, dissolving in a mixed solvent of methanol with the concentration of 10% and ultrapure water, and uniformly stirring to obtain a rapid colorimetric fluorescent hypochlorite detection reagent with the concentration of 0.1 mmol/L;
measuring 1.5mL of the prepared hypochlorite detection reagent in a quartz cuvette by using a pipette, adding 20mL of sodium hypochlorite solution with different concentrations of 0-30mM, testing the spectral change after reaction by using a fluorescence spectrometer after 3s, and recording the fluorescence color change before and after reaction by using a camera. The fluorescence spectrum peak intensity is gradually enhanced along with the increase of the hypochlorite concentration after the reaction, and the fluorescence color is changed into bluish purple from colorless before the reaction; repeating the experiment, testing the change of the absorption spectrum after reaction by an ultraviolet visible absorption spectrometer after 3s, and recording the change of the colorimetric color before and after the reaction by a camera, wherein the intensity of the ultraviolet visible absorption peak after the reaction is enhanced along with the increase of the concentration of hypochlorite, and the colorimetric color is changed into red from colorless before the reaction;
the calcium hypochlorite solid particles with different masses are wiped by sampling paper, 1-2 drops of detection reagent are dripped, so that the colorimetric phenomenon of the sodium hypochlorite detection reagent for detecting trace calcium hypochlorite solid particles is changed from colorless to red, and the fluorescent phenomenon is changed from colorless to blue-purple.
Example 4
Weighing 1mg of bromonaphthol and dissolving in a mixed solvent of ethanol with the concentration of 80% and ultrapure water at room temperature, and uniformly stirring to obtain a rapid colorimetric fluorescent hypochlorite detection reagent with the concentration of 40 mmol/L;
measuring 1.5mL of the prepared hypochlorite detection reagent in a quartz cuvette by using a liquid-transferring gun, adding 20mL of sodium hypochlorite solution with different concentrations of 0-4000 mu M, testing the spectral change after reaction by using a fluorescence spectrometer after 3s, and recording the fluorescence color change before and after reaction by using a camera; the fluorescence spectrum peak intensity after the reaction is gradually enhanced along with the increase of the hypochlorite concentration, and the fluorescence color is changed from colorless before the reaction to green;
measuring 1.5mL of the prepared hypochlorite detection reagent in a quartz cuvette by using a liquid-transferring gun, adding 20mL of sodium hypochlorite solution with different concentrations of 0-4000 mu M, testing the change of the absorption spectrum after reaction by using an ultraviolet-visible absorption spectrometer after 3s, and recording the color change of the color before and after the reaction by using a camera; after the reaction, the intensity of the ultraviolet visible absorption peak is enhanced along with the increase of the concentration of hypochlorite, and the color of the colorimetric color is changed into orange before the reaction;
the sampling paper is used for wiping potassium hypochlorite solid particles with different masses, 1-2 drops of detection reagent are dripped, and the colorimetric phenomenon of the sodium hypochlorite detection reagent for detecting trace potassium hypochlorite solid particles is changed from colorless to orange red, and the fluorescent phenomenon is changed from colorless to green.
Example 5
Weighing 50mg of chloronaphthol to dissolve in a mixed solvent of acetone with the concentration of 20% and ultrapure water at room temperature, and uniformly stirring to obtain a rapid colorimetric fluorescent hypochlorite detection reagent with the concentration of 35 mmol/L;
measuring 1.5mL of the prepared hypochlorite detection reagent in a quartz cuvette by using a liquid transfer gun, adding 20mL of sodium hypochlorite solution with different concentrations of 0-300 mu M, testing the spectral change after reaction by using a fluorescence spectrometer after 3s, and recording the fluorescence color change before and after reaction by using a camera. The fluorescence spectrum peak intensity is gradually enhanced along with the increase of the hypochlorite concentration after the reaction, and the fluorescence color is changed into bluish purple from colorless before the reaction;
measuring 1.5mL of the prepared hypochlorite detection reagent in a quartz cuvette by using a liquid-transferring gun, adding 20mL of sodium hypochlorite solution with different concentrations of 0-4000 mu M, testing the change of the absorption spectrum after reaction by using an ultraviolet-visible absorption spectrometer after 3s, and recording the color change of the color before and after the reaction by using a camera; after the reaction, the intensity of the ultraviolet visible absorption peak is enhanced along with the increase of the concentration of hypochlorite, and the colorimetric color is changed into brown from colorless before the reaction;
the sampling paper is used for wiping potassium chlorate solid particles with different masses, 1-2 drops of detection reagent are dropped on the sampling paper, and the colorimetric and fluorescence phenomena of the potassium chlorate solid particles with trace amount detected by the sodium hypochlorite detection reagent are unchanged.
Example 6
Weighing 5mg of naphthol acetate at room temperature, dissolving the naphthol acetate in a mixed solvent of ethyl acetate and ultrapure water with the concentration of 30%, and uniformly stirring to obtain a rapid colorimetric fluorescent hypochlorite detection reagent with the concentration of 2 mmol/L;
measuring 1.5mL of the prepared hypochlorite detection reagent in a quartz cuvette by using a liquid-transferring gun, then adding 20mL of sodium hypochlorite solution with different concentrations of 0-2000 mu M, testing the spectral change after reaction by using a fluorescence spectrometer after 3s, and recording the fluorescence color change before and after reaction by using a camera, wherein the fluorescence spectral peak intensity is gradually enhanced along with the increase of the hypochlorite concentration after reaction, and the fluorescence color is changed from colorless before reaction to blue-purple;
measuring 1.5mL of the prepared hypochlorite detection reagent in a quartz cuvette by using a liquid transfer gun, adding 20mL of sodium hypochlorite solution with different concentrations of 0-2000 mu M, testing the change of the absorption spectrum after reaction by using an ultraviolet-visible absorption spectrometer after 3s, and recording the color change of the color before and after the reaction by using a camera; after the reaction, the intensity of the ultraviolet visible absorption peak is enhanced along with the increase of the concentration of hypochlorite, and the color of the colorimetric color is changed into red from colorless before the reaction;
the sampling paper is used for wiping potassium perchlorate solid particles with different qualities, 1-2 drops of detection reagent are dropped on the sampling paper, and the colorimetric and fluorescence phenomena of the potassium perchlorate solid particles with trace amount detected by the sodium hypochlorite detection reagent are not changed.
Example 7
Weighing 20mg of tetrahydronaphthol and dissolving in a mixed solvent of dichloromethane and water with the concentration of 40% at room temperature, and uniformly stirring to obtain a rapid colorimetric fluorescent hypochlorite detection reagent with the concentration of 5 mmol/L;
measuring 1.5mL of the prepared hypochlorite detection reagent in a quartz cuvette by using a liquid-transferring gun, then adding 20mL of sodium hypochlorite solution with different concentrations of 0-30mM, testing the spectral change after reaction by using a fluorescence spectrometer after 3s, and recording the fluorescence color change before and after reaction by using a camera, wherein the fluorescence spectral peak intensity is gradually enhanced along with the increase of the hypochlorite concentration after reaction, and the fluorescence color is changed from colorless before reaction to green;
measuring 1.5mL of the prepared hypochlorite detection reagent in a quartz cuvette by using a liquid-transfering gun, then adding 20mL of sodium hypochlorite solution with different concentrations of 0-30mM, testing the change of an absorption spectrum after reaction by using an ultraviolet visible absorption spectrometer after 3s, and recording the change of the colorimetric color before and after the reaction by using a camera, wherein the intensity of an ultraviolet visible absorption peak is enhanced along with the increase of the concentration of hypochlorite after the reaction, and the colorimetric color is colorless and brown before the reaction;
the sampling paper is used for wiping ammonium chloride solid particles with different masses, 1-2 drops of detection reagent are dripped, and the colorimetric and fluorescence phenomena of the sodium hypochlorite detection reagent for detecting trace ammonium chloride solid particles are unchanged.
Example 8
Weighing 30mg of S-binaphthol at room temperature, dissolving in a mixed solvent of petroleum ether and ultrapure water with the concentration of 60%, and uniformly stirring to obtain a rapid colorimetric fluorescent hypochlorite detection reagent with the concentration of 25 mmol/L;
measuring 1.5mL of the prepared hypochlorite detection reagent in a quartz cuvette by using a liquid-transferring gun, then adding 20mL of sodium hypochlorite solution with different concentrations of 0-5000 [ mu ] M, testing the spectral change after reaction by using a fluorescence spectrometer after 3s, and recording the fluorescence color change before and after reaction by using a camera, wherein the fluorescence spectral peak intensity after reaction is gradually enhanced along with the increase of the hypochlorite concentration, and the fluorescence color is changed from colorless before reaction to green;
measuring 1.5mL of prepared hypochlorite detection reagent in a quartz cuvette by using a liquid-transferring gun, adding 20mL of sodium hypochlorite solution with different concentrations of 0-5000 [ mu ] M, testing the change of an absorption spectrum after reaction by using an ultraviolet visible absorption spectrometer after 3s, recording the change of colorimetric color before and after the reaction by using a camera, wherein the intensity of an ultraviolet visible absorption peak is enhanced along with the increase of the concentration of hypochlorite after the reaction, and the colorimetric color is colorless and red before the reaction;
the sampling paper is used for wiping potassium hypochlorite solid particles with different masses, 1-2 drops of detection reagent are dripped, and the colorimetric phenomenon of the sodium hypochlorite detection reagent for detecting trace potassium hypochlorite solid particles is changed from colorless to red, and the fluorescent phenomenon is changed from colorless to green.
Example 9
Weighing 50mg of 4-bromonaphthol at room temperature, dissolving in a mixed solvent of tetrahydrofuran and ultrapure water with the concentration of 70%, and uniformly stirring to obtain a rapid colorimetric fluorescent hypochlorite detection reagent with the concentration of 10 mmol/L;
measuring 1.5mL of the prepared hypochlorite detection reagent in a quartz cuvette by using a liquid-transferring gun, then adding 20mL of sodium hypochlorite solution with different concentrations of 0-2000 mu M, testing the spectral change after reaction by using a fluorescence spectrometer after 3s, and recording the fluorescence color change before and after reaction by using a camera, wherein the fluorescence spectral peak intensity is gradually enhanced along with the increase of the hypochlorite concentration after reaction, and the fluorescence color is changed from colorless before reaction to blue-purple;
measuring 1.5mL of prepared hypochlorite detection reagent in a quartz cuvette by using a liquid-transfering gun, then adding 20mL of sodium hypochlorite solution with different concentrations of 0-2000 mu M, testing the change of an absorption spectrum after reaction by using an ultraviolet visible absorption spectrometer after 3s, and recording the change of colorimetric color before and after the reaction by using a camera, wherein the intensity of an ultraviolet visible absorption peak is enhanced along with the increase of the concentration of hypochlorite after the reaction, and the colorimetric color is colorless and pink before the reaction;
the sampling paper is used for wiping potassium hypochlorite solid particles with different masses, 1-2 drops of detection reagent are dripped, and the colorimetric phenomenon that the sodium hypochlorite detection reagent detects trace potassium hypochlorite solid particles is changed from colorless to pink, and the fluorescent phenomenon is changed from colorless to blue-purple.
Example 10
Weighing 40mg of nitro-2-naphthol and dissolving in a mixed solvent of dimethyl sulfoxide and ultrapure water with the concentration of 80% at room temperature, and uniformly stirring to obtain a rapid colorimetric fluorescent hypochlorite detection reagent with the concentration of 40 mmol/L;
measuring 1.5mL of the prepared hypochlorite detection reagent in a quartz cuvette by using a liquid-transferring gun, then adding 20mL of sodium hypochlorite solution with different concentrations of 0-2000 mu M, testing the spectral change after reaction by using a fluorescence spectrometer after 3s, and recording the fluorescence color change before and after reaction by using a camera, wherein the fluorescence spectral peak intensity after reaction is gradually enhanced along with the increase of the hypochlorite concentration, and the fluorescence color is changed from colorless before reaction to green;
measuring 1.5mL of prepared hypochlorite detection reagent in a quartz cuvette by using a liquid-transfering gun, then adding 20mL of sodium hypochlorite solution with different concentrations of 0-2000 mu M, testing the change of an absorption spectrum after reaction by using an ultraviolet visible absorption spectrometer after 3s, and recording the change of colorimetric color before and after reaction by using a camera, wherein the intensity of an ultraviolet visible absorption peak is enhanced along with the increase of the concentration of hypochlorite after reaction, and the colorimetric color is colorless and red before reaction;
the sodium hypochlorite solid particles with different masses are wiped by sampling paper, 1-2 drops of detection reagent are dripped, so that the colorimetric phenomenon that the sodium hypochlorite detection reagent detects trace sodium hypochlorite solid particles is changed from colorless to red, and the fluorescent phenomenon is changed from colorless to green.
Claims (1)
1. A rapid colorimetric fluorescent hypochlorite detection reagent is characterized in that the reagent is prepared from naphthol compounds, an organic solvent and an inorganic solvent, wherein:
the naphthol compound is 1-naphthol, 2, 3-dihydroxynaphthol, binaphthol, bromonaphthol, chloronaphthol, acetonaphthol, tetrahydronaphthol, S-binaphthol, 4-bromonaphthol or nitro-2-naphthol, and the content of the naphthol compound in the solution is 0.1-40 mmol/L;
the organic solvent is dimethyl sulfoxide, methanol, ethanol, acetonitrile, acetone, ethyl acetate, dichloromethane, petroleum ether or tetrahydrofuran, and the concentration of the organic solvent is 10-80%;
the inorganic solvent is ultrapure water;
diluting the organic solvent with ultrapure water to the concentration of 10% -80% to obtain a mixed solvent;
weighing 0.1-100 mg of naphthol compound and dissolving in the mixed solvent to obtain the reagent for rapid colorimetric fluorescence detection of hypochlorite with the concentration of 0.1-40 mmol/L.
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