CN113109334B - TATP detection reagent, preparation method of standard colorimetric card, TATP qualitative detection method and TATP quantitative detection method - Google Patents

TATP detection reagent, preparation method of standard colorimetric card, TATP qualitative detection method and TATP quantitative detection method Download PDF

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CN113109334B
CN113109334B CN202110568873.2A CN202110568873A CN113109334B CN 113109334 B CN113109334 B CN 113109334B CN 202110568873 A CN202110568873 A CN 202110568873A CN 113109334 B CN113109334 B CN 113109334B
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何毅
张桂华
余玲
邹心仪
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Southwest University of Science and Technology
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Abstract

The invention discloses a TATP detection reagent, which comprises hydrochloric acid, ferrous solution and TMB solution,the volume ratio of the hydrochloric acid to the ferrous solution to the TMB solution is 6:13: 14. In the invention, hydrochloric acid (HCl) provides an acidic environment for the reaction (which is more beneficial to TMB dissolution and color development), and simultaneously catalyzes TATP to decompose and form H2O2；Fe2+And H2O2Reaction of H2O2Decomposition into hydroxyl radicals, Fe2+Is oxidized into Fe3+(ii) a TMB as a colour developer, the production of hydroxyl radicals and the oxidation of Fe3+The TMB is oxidized under the combined action to develop color, and the three supplement each other and are not enough. Therefore, the TATP can be detected frequently and rapidly on site, and qualitative detection can be realized.

Description

TATP detection reagent, preparation method of standard colorimetric card, TATP qualitative detection method and TATP quantitative detection method
Technical Field
The invention relates to the field of explosive detection, in particular to a TATP detection reagent, a preparation method of a standard colorimetric card, a TATP qualitative detection method and a TATP quantitative detection method.
Background
In recent years, there has been a rapid spread of terrorist attacks worldwide, seriously threatening the safety and stability of the international society. Triacetone trioxide (TATP) is a new type of peroxide explosive and is also known as the "parent to the" dusting ". Because the preparation raw materials are easy to obtain and the preparation process is simple, the preparation method is often used in terrorist attacks and crimes by international terrorists. TATP is extremely sensitive to flame, heat, shock and friction, while one TATP molecule can produce four gas molecules, in less than one second, hundreds of grams of solid TATP can produce hundreds of thousands of liters of gas, resulting in flameless explosion. Therefore, the development of the on-site rapid detection technology of the peroxide explosive TATP has important significance for social safety.
At present, the method for detecting TATP mainly adopts instrumental methods, for example, infrared spectroscopy detection method, gas chromatography detection method, liquid chromatography detection method, mass spectrometry, ion mobility spectrometry and other detection methods, but such instruments are large-scale equipment and expensive equipment, and are difficult to carry due to large equipment volume, and professional detection personnel are required to operate the instruments, so that the instrumental method for detecting TATP is not suitable for frequent and rapid field detection environments.
In order to solve the above problems, researchers have studied to change the research direction, and in the process, it is desirable to find a method for detecting TATP by color comparison. Through diligent efforts, researchers propose a colorimetric method to replace the original instrumental method for detection, TATP is decomposed and broken under the action of certain enzymes to generate hydrogen peroxide, the hydrogen peroxide reacts with certain color development and fluorescent substances in the presence of peroxidase, and the detection is carried out through a spectral instrument or qualitative observation by naked eyes. After the research of this stage, the existing ubiquitous enzyme-catalyzed reaction is found to have low efficiency for decomposing and breaking bonds of TATP to generate hydrogen peroxide, and a pretreatment step is required, so that the application of the reaction in the actual environment is greatly limited, and the research finally finds that the problem that although the reaction is large in size, heavy in weight, difficult to carry and capable of being operated by professional detection personnel is solved, the applicability of the reaction in the detection environment for frequently and rapidly detecting TATP on site is still low.
Disclosure of Invention
Aiming at the problems, the invention provides a TATP detection reagent, a preparation method of a standard colorimetric card, a TATP qualitative detection method and a quantitative detection method, which are suitable for frequently and rapidly detecting TATP on site.
In order to solve the technical problem, the invention provides a TATP detection reagent which comprises hydrochloric acid, a ferrous solution and a TMB solution, wherein the volume ratio of the hydrochloric acid to the ferrous solution to the TMB solution is 6:13: 14. Wherein TMB is 3,3',5,5' -tetramethyl benzidine.
The working principle of the technical scheme is as follows:
on the basis of preparation of the hydrochloric acid, the ferrous solution and the TMB solution according to the volume ratio of 6:13:14, the hydrochloric acid (HCl) provides an acid environment for reaction (is more beneficial to dissolving and developing the TMB), and simultaneously catalyzes TATP to decompose to form H2O2；Fe2+And H2O2Reaction of H2O2Decomposition into hydroxyl radicals, Fe2+Is oxidized into Fe3+(ii) a TMB as developer, generated hydroxyl radical and Fe3 generated by oxidation+The TMB is oxidized under the combined action to develop color, and the three substances supplement each other and are absent at the volume ratio of (6:13: 14). Therefore, the TATP can be detected frequently and rapidly on site, and qualitative detection can be realized.
In a further technical scheme, the concentration of the ferrous solution is 7-170 mu M; the concentration of the TMB solution is 2-100 mu M.
Ferrous solution (Fe)2+Solution) and TMB solution, and correspondingly, in the general TATP detection process, the concentration of the ferrous solution is 7-170 mu M; the concentration of the TMB solution is 2-100 mu M. Effective detection can be achieved. If the content of TATP is higher in a special environment, the concentration of the ferrous solution can be more than 170 mu M, the concentration of the TMB solution can be more than 100 mu M, but the concentration of the ferrous solution can not be lower than 7 mu M all the time, the concentration of the TMB solution can not be lower than 2 mu M all the time, and otherwise, the TMB (color developing agent) can not be developed.
In a further embodiment, the hydrochloric acid concentration is controlled to be 20 to 500mM, so as to adjust the pH of the prepared solution after the hydrochloric acid, the ferrous iron solution and the TMB solution are prepared in a volume ratio of 6:13:14 to 1.2 to 3.0 (e.g., 1.2, 1.4, 1.7, 2.0, 2.3, 2.7, 3.0).
The detection performance of the TATP detection reagent is better optimized by adjusting the pH value of the prepared solution to be 1.2-3.0. When the volume ratio of the hydrochloric acid to the ferrous solution to the TMB solution is 6:13:14, the concentration of the ferrous solution is 7-170 mu M, the concentration of the TMB solution is 2-100 mu M, when the concentration of the hydrochloric acid is controlled to be 20-500 mM, the detection performance of the TATP detection reagent is better (when the volume ratio of the hydrochloric acid to the ferrous solution to the TMB solution is 6:13:14, the concentration of the ferrous solution is 0.1mM, the concentration of the TMB solution is 0.1mM, and the concentration of the hydrochloric acid is 100mM, the detection performance of the TATP detection reagent is most preferable), and on the basis, when the pH of the prepared solution is more than 3 or less than 1.2, the color developing agent (TMB) does not develop color, so that the TATP detection reagent has the characteristic of clear demarcation point in the aspect of color development, on the basis, the pH value of the prepared solution is adjusted to be 1.2-3.0, so that the occurrence of false detection is directly avoided. In addition, if the hydrochloric acid is too much, the absorbance is reduced, the effect is deteriorated, and the self-oxidation of TMB is caused to affect the detection result, thereby causing a problem of wasting resources.
In order to solve the problems, the invention discloses a preparation method of a standard colorimetric card, which comprises the following steps: preparing an ethanol solution of TATP, and diluting the ethanol solution of TATP into a plurality of TATP water solutions with different concentrations by using pure water; preparing the detection reagent in the technical scheme; respectively mixing the prepared detection reagent with each part of TATP aqueous solution according to a volume ratio of 99:1, standing in a water bath at a set temperature environment of 60 ℃ for a set time period of 6-10min (for example, 6min, 7min, 8min, 9min and 10min), and recording the color of the detection reagent which is respectively acted with each part of TATP aqueous solution after the standing time is finished; and establishing a TATP standard colorimetric card according to the color.
In the method for preparing the standard colorimetric card, since TATP is insoluble in water, an ethanol solution of TATP needs to be prepared first, and in order to reduce the influence of an ethanol solvent, the ethanol solution is diluted by pure water into a plurality of TATP aqueous solutions with different concentrations (for example, 0.05mM, 0.1mM, 0.3mM, 0.5mM, 1mM, 2mM, 3mM and the like). The standard colorimetric card is manufactured, so that the cost is low, frequent and rapid TATP detection on site is greatly facilitated, and the color comparison card is convenient to carry, transport and manufacture in batches.
In a further technical scheme, the colors are recorded in a picture form, and the colors in the picture are extracted through the mobile terminal. And the colors in the pictures are extracted through the mobile terminal to realize sharing and unify the standards.
In order to solve the problems, the invention discloses a TATP qualitative detection method, which comprises the following steps: wiping the surface of the object to be detected by using filter paper wetted by deionized water; preparing 5mL of detection solution of the detection reagent in the technical scheme, and filling the detection solution into a detection bottle; and putting the filter paper wiped with the object to be detected into a detection bottle filled with the detection solution, putting the detection bottle into a thermos cup filled with water at a set temperature environment of 60 ℃, standing for a set time of 6-10min (for example, 6min, 7min, 8min, 9min and 10min), observing the color of the detection solution, and obtaining a qualitative conclusion.
The TATP qualitative detection method establishes a detection method of TATP on the solid surface (the surface of an article to be detected), wherein TATP is broken and is Fe2+Catalytically produced hydroxyl radicals and Fe3+The TMB is oxidized under the combined action to develop color, and has specific ultraviolet absorption wavelength of 450nm, so that the anti-interference capability is strong, the sensitivity is high, and the detection limit can be as low as 0.12 mu M. The reaction is a color reaction, colorless transparency is changed into yellow before and after the reaction, the color development is obvious, whether TATP is contained or not is judged rapidly on site, the detection time is saved, meanwhile, the detection method is stable, the prices of related reaction raw materials are not high, and the detection requirements of governments, common enterprises and institutions can be met. In addition, no special reagents such as solid acids and nanoparticles are required, and no complicated pretreatment step is required.
In order to solve the problems, the invention discloses a TATP quantitative detection method, which comprises the following steps:
(1) preparing the detection reagent in the technical scheme;
(2) mixing the detection reagent and a sample to be detected according to a volume ratio of 99:1, standing in a water bath at a set temperature environment of 60 ℃ for a set time of 6-10min (for example, 6min, 7min, 8min, 9min and 10min), and observing the color;
(3) comparing the color observed in step (2) with the TATP standard color chart of claim 4 to obtain a corresponding TATP content range value in the sample to be tested.
The TATP quantitative detection method establishes a method for detecting TATP in liquid, wherein TATP is broken and is Fe2+Catalytic generationAnd Fe and a hydroxyl radical of3+The TMB is oxidized under the combined action to be colored, the sensitivity is high, the reaction is a color development reaction, the color is changed into yellow from colorless transparency before and after the reaction, the color development is obvious, whether the TATP is contained or not is judged rapidly on site, meanwhile, the content range value of the TATP is detected, correct counter measures can be made at the first time by definitely detecting the content range value of the TATP, the detection time is saved, meanwhile, the detection method is stable, the price of related reaction raw materials is not high, and the detection requirements of governments, common enterprises and institutions can be met. In addition, no special reagents such as solid acids and nanoparticles are required, and no complicated pretreatment step is required.
In order to solve the problems, the invention discloses a TATP quantitative detection method, which comprises the following steps: preparing an ethanol solution of TATP, and diluting the ethanol solution of TATP into a plurality of TATP water solutions with different concentrations by using pure water; preparing the detection reagent in the technical scheme; respectively mixing the prepared detection reagent with each diluted TATP aqueous solution according to a volume ratio of 99:1, standing in a water bath at a set temperature environment of 60 ℃ for a set time of 6-10min (for example, 6min, 7min, 8min, 9min and 10min), and measuring all absorbance values and obtaining a corresponding standard curve after the standing time is finished; mixing the detection reagent and a sample to be detected according to a volume ratio of 99:1, standing in a water bath at a set temperature environment of 60 ℃ for a set time of 6-10min (for example, 6min, 7min, 8min, 9min and 10min), measuring the absorbance value of a solution in which the detection reagent and the sample to be detected are mixed after standing is finished, and comparing the absorbance value of the sample to be detected with the standard curve to obtain the corresponding TATP content in the sample to be detected.
The TATP quantitative detection method establishes a method for detecting TATP in liquid, wherein TATP is broken and is Fe2+Catalytically produced hydroxyl radicals and Fe3+TMB is oxidized under the combined action to be developed, and has specific ultraviolet absorption wavelength of 450nm, so that the anti-interference capability is strong, the absorption intensity of the wavelength at 450nm is directly measured by an ultraviolet visible spectrophotometer, the linear relation between the TATP concentration and the corresponding absorption intensity is established, the sensitivity is high, and the detection limit can be as low as 0.12 mu M. The reactionFor the color reaction, colorless transparency is changed into yellow before and after the reaction, the color development is obvious, whether the TATP is contained or not is judged rapidly on site, meanwhile, the TATP content value is detected, the most correct response measures can be taken at the first time by accurately detecting the TATP content value, the detection time is saved, meanwhile, the detection method is stable, the price of related reaction raw materials is not high, and the detection requirements of governments, common enterprises and institutions can be met. In addition, no special reagents such as solid acids and nanoparticles are required, and no complicated pretreatment step is required.
The invention has the beneficial effects that:
1. according to the invention, on the basis of the preparation of the hydrochloric acid, the ferrous solution and the TMB solution according to the volume ratio of 6:13:14, the hydrochloric acid (HCl) provides an acid environment for the reaction (which is more beneficial to the dissolution and color development of the TMB), and simultaneously catalyzes the decomposition of TATP to form H2O2；Fe2+And H2O2Reaction of H2O2Decomposition into hydroxyl radicals, Fe2+Is oxidized into Fe3+(ii) a TMB as developer, generated hydroxyl radical and Fe3 generated by oxidation+The TMB is oxidized under the combined action to develop color, and the three supplement each other and are not enough. Therefore, the TATP can be detected frequently and rapidly on site, and qualitative detection can be realized.
2. In the present invention, ferrous solution (Fe)2+Solution) and TMB solution, and correspondingly, in the general TATP detection process, the concentration of the ferrous solution is 7-170 mu M; the concentration of the TMB solution is 2-100 mu M. Effective detection can be achieved. If the content of TATP is higher in a special environment, the concentration of the ferrous solution can be more than 170 mu M, the concentration of the TMB solution can be more than 100 mu M, but the concentration of the ferrous solution can not be lower than 7 mu M all the time, the concentration of the TMB solution can not be lower than 2 mu M all the time, and otherwise, the TMB (color developing agent) can not be developed.
3. In the invention, the detection performance of the TATP detection reagent is better optimized by adjusting the pH value of the prepared solution to be 1.2-3.0. When the volume ratio of the hydrochloric acid to the ferrous solution to the TMB solution is 6:13:14, the concentration of the ferrous solution is 7-170 mu M, the concentration of the TMB solution is 2-100 mu M, when the concentration of the hydrochloric acid is controlled to be 20-500 mM, the detection performance of the TATP detection reagent is better (when the volume ratio of the hydrochloric acid to the ferrous solution to the TMB solution is 6:13:14, the concentration of the ferrous solution is 0.1mM, the concentration of the TMB solution is 0.1mM, and the concentration of the hydrochloric acid is 100mM, the detection performance of the TATP detection reagent is most preferable), and on the basis, when the pH of the prepared solution is more than 3 or less than 1.2, the color developing agent (TMB) does not develop color, so that the TATP detection reagent has the characteristic of clear demarcation point in the aspect of color development, on the basis, the pH value of the prepared solution is adjusted to be 1.2-3.0, so that the occurrence of false detection is directly avoided. In addition, if the hydrochloric acid is too much, the absorbance is reduced, the effect is deteriorated, and the self-oxidation of TMB is caused to affect the detection result, thereby causing a problem of wasting resources.
4. In the method for preparing the standard colorimetric card, an ethanol solution of TATP needs to be prepared first because TATP is insoluble in water, and in order to reduce the influence of the ethanol solvent, the ethanol solution of TATP needs to be diluted with pure water into multiple TATP aqueous solutions with different concentrations (for example, 0.05mM, 0.1mM, 0.3mM, 0.5mM, 1mM, 2mM, 3mM, etc.), and in order to enable the whole color development process to be simple and stable in color development, the prepared detection reagents are mixed with each TATP aqueous solution at a volume ratio of 99:1, and the mixture is placed in a water bath at 60 ℃ for standing for 6-10 min. The standard colorimetric card is manufactured, so that the cost is low, frequent and rapid TATP detection on site is greatly facilitated, and the color comparison card is convenient to carry, transport and manufacture in batches.
5. In the invention, the colors in the pictures are extracted through the mobile terminal to realize sharing and unify the standard.
6. In the invention, the TATP qualitative detection method establishes a method for detecting TATP on the solid surface (the surface of an article to be detected), wherein TATP is broken and is Fe2+Catalytically produced hydroxyl radicals and Fe3+The TMB is oxidized under the combined action to develop color, and has specific ultraviolet absorption wavelength of 450nm, so that the anti-interference capability is strong, the sensitivity is high, and the detection limit can be as low as 0.12 mu M. The reaction is a color reaction, and the reaction is carried out before and afterThe color is transparent and changed into yellow, the color development is obvious, whether TATP is contained or not is judged rapidly on site, the detection time is saved, meanwhile, the detection method is stable, the prices of related reaction raw materials are not high, and the detection requirements of governments, common enterprises and institutions can be met. In addition, no special reagents such as solid acids and nanoparticles are required, and no complicated pretreatment step is required.
7. In the invention, the TATP quantitative detection method establishes a method for detecting TATP in liquid, wherein TATP is broken and is Fe2+Catalytically produced hydroxyl radicals and Fe3+The TMB is oxidized under the combined action to be colored, the sensitivity is high, the reaction is a color development reaction, the color is changed into yellow from colorless transparency before and after the reaction, the color development is obvious, whether the TATP is contained or not is judged rapidly on site, meanwhile, the content range value of the TATP is detected, correct counter measures can be made at the first time by definitely detecting the content range value of the TATP, the detection time is saved, meanwhile, the detection method is stable, the price of related reaction raw materials is not high, and the detection requirements of governments, common enterprises and institutions can be met. In addition, no special reagents such as solid acids and nanoparticles are required, and no complicated pretreatment step is required.
8. In the invention, the TATP quantitative detection method establishes a method for detecting TATP in liquid, wherein TATP is broken and is Fe2+Catalytically produced hydroxyl radicals and Fe3+TMB is oxidized under the combined action to be developed, and has specific ultraviolet absorption wavelength of 450nm, so that the anti-interference capability is strong, the absorption intensity of the wavelength at 450nm is directly measured by an ultraviolet visible spectrophotometer, the linear relation between the TATP concentration and the corresponding absorption intensity is established, the sensitivity is high, and the detection limit can be as low as 0.12 mu M. The reaction is a color reaction, the color is changed into yellow from colorless transparency before and after the reaction, the color development is obvious, whether the TATP is contained or not is judged rapidly on site, the most correct counter measures can be taken at the first time by accurately detecting the content value of the TATP, the detection time is saved, meanwhile, the detection method is stable, the price of related reaction raw materials is not high, and the detection requirements of governments, common enterprises and institutions can be met. In addition, no addition is requiredAnd special reagents such as solid acid and nano particles are added, and complex pretreatment steps are not needed.
Drawings
FIG. 1 is a color reaction chart of color development using different color-developing substrates in example 6 of the present invention;
FIG. 2 is a graph showing ultraviolet absorption spectra of color development using different color-developing substrates in example 6 of the present invention;
FIG. 3 is a bar graph of the UV absorption peaks of the catalyzed reactions using different variable valence metal ions in inventive example 6;
FIG. 4 is a scattergram of UV absorption peaks at different pH's in inventive example 7;
FIG. 5 shows different concentrations of Fe in inventive example 72+A scatter diagram of the ultraviolet absorption peak value of the catalytic reaction coloration;
FIG. 6 is a scattergram of UV absorption peaks for example 7 of the present invention with TMB added at different concentrations;
FIG. 7 shows that the UV absorption peak value curve is fitted by measuring the UV every 5min at different temperatures in example 7 of the present invention;
FIG. 8 is a scattergram showing the relationship between the peak value of ultraviolet absorption and time, which was measured every 2min by heating in a water bath at 60 ℃ in example 7 of the present invention;
FIG. 9 is a color reaction chart of TATP at various concentrations in inventive example 8;
FIG. 10 is a graph showing the ultraviolet absorption spectrum of TATP at various concentrations in inventive example 8;
FIG. 11 is a graph of a fitted ultraviolet absorption peak of TATP at various concentrations in inventive example 8;
fig. 12 is a TATP standard color chart produced in example 8 of the present invention;
FIG. 13 is a diagram showing the ultraviolet absorption spectrum of a solution measured in example 9 of the present invention after wiping filter paper is placed in 5mL of TATP detection solution and water bath is carried out at 60 ℃ for 6-10min when detecting the residual TATP on the solid surface;
FIG. 14 is a bar graph of the UV absorption peak for measuring the TATP content in a real liquid environment in inventive example 9;
FIG. 15 is a test strip of TATP made in example 10 of the present invention;
fig. 16 is a flowchart of a qualitative TATP detection method in embodiment 3 of the present invention.
Detailed Description
The embodiments of the present invention will be further described with reference to the accompanying drawings.
Example 1:
the invention provides a TATP detection reagent, which comprises hydrochloric acid, a ferrous solution and a TMB solution, wherein the volume ratio of the hydrochloric acid to the ferrous solution to the TMB solution is 6:13: 14.
The working principle of the technical scheme is as follows:
hydrochloric acid (HCl) provides an acidic environment for the reaction (which is more beneficial to TMB dissolution and color development), and simultaneously catalyzes TATP to decompose to form H2O2；Fe2+Generated by reaction with hydrogen peroxide, which decomposes into hydroxyl radicals, Fe2+Is oxidized into Fe3+(ii) a TMB as a colour developer, the production of hydroxyl radicals and the oxidation of Fe3+The TMB is oxidized under the combined action to develop color, and the three supplement each other and are not enough. Therefore, the TATP can be detected frequently and rapidly on site, and qualitative detection can be realized.
In another embodiment, the concentration of the ferrous solution is 7-170 μ M; the concentration of the TMB solution is 2-100 mu M. For example, the ferrous solution has a concentration of 10 μ M; the concentration of the TMB solution is 2 mu M; the concentration of the ferrous solution is 100 mu M; the concentration of the TMB solution is 3 mu M; the concentration of the ferrous solution is 170 mu M; the concentration of the TMB solution is 4 mu M; the concentration of the ferrous solution is 10 mu M; the concentration of the TMB solution is 50 mu M; the concentration of the ferrous solution is 120 mu M; the concentration of the TMB solution is 46 mu M; the concentration of the ferrous solution is 168 mu M; the concentration of the TMB solution is 60 mu M; the concentration of the ferrous solution is 24 mu M; the concentration of the TMB solution is 100 mu M; the concentration of the ferrous solution is 100 mu M; the concentration of the TMB solution is 100 mu M; the concentration of the ferrous solution is 170 mu M; the concentration of the TMB solution is 100 mu M. The solution preparation method comprises the following steps: ferrous solution: 0.020g of FeCl was weighed2·4H2O powder (or 0.028g of FeSO)4·7H2O powder) to prepare 100mL of ferrous solution with the concentration of 1mM for standby, and diluting the ferrous solution by 5.9,10 and 100 times respectively to obtain ferrous solutions with the concentration of 170 MuM, 100 MuM and 10 MuM, and the like to obtain other solution concentrations; TMB solution: 0.0024g of TMB powder was weighed out and 100mL of 0.1mM TMB solution was made up with 1mM HCl and diluted 2,50 fold to give 50. mu.M, 2. mu. MTMB solution, and so on to give other solution concentrations.
Ferrous solution (Fe)2+Solution) and TMB solution, and correspondingly, in the general TATP detection process, the concentration of the ferrous solution is 7-170 mu M; the concentration of the TMB solution is 2-100 mu M. Effective detection can be achieved. If the content of TATP is higher in a special environment, the concentration of the ferrous solution can be more than 170 mu M, the concentration of the TMB solution can be more than 100 mu M, but the concentration of the ferrous solution can not be lower than 7 mu M all the time, the concentration of the TMB solution can not be lower than 2 mu M all the time, and otherwise, the TMB (color developing agent) can not be developed.
In another embodiment, the hydrochloric acid concentration is controlled to be 20 to 500mM, so as to adjust the pH of a preparation solution after preparing the hydrochloric acid, the ferrous iron solution and the TMB solution in a volume ratio of 6:13:14 to 1.2 to 3.0. Wherein the hydrochloric acid has a concentration of 20 to 500mM, such as 20mM, 250mM, 500mM, etc., and the solution is prepared by mixing hydrochloric acid: the purchased 36-38% concentrated hydrochloric acid is diluted by deionized water by 24,48 and 600 times to obtain 500mM,250mM and 20mM hydrochloric acid, and the like to obtain other solution concentrations. In addition, any combination of the concentration of the ferrous iron solution and the concentration of the TMB solution can be combined with any concentration of hydrochloric acid.
The detection performance of the TATP detection reagent is better optimized by adjusting the pH value of the prepared solution to be 1.2-3.0. When the volume ratio of the hydrochloric acid to the ferrous solution to the TMB solution is 6:13:14, the concentration of the ferrous solution is 7-170 mu M, the concentration of the TMB solution is 2-100 mu M, when the concentration of the hydrochloric acid is controlled to be 20-500 mM, the detection performance of the TATP detection reagent is better (when the volume ratio of the hydrochloric acid to the ferrous solution to the TMB solution is 6:13:14, the concentration of the ferrous solution is 0.1mM, the concentration of the TMB solution is 0.1mM, and the concentration of the hydrochloric acid is 100mM, the detection performance of the TATP detection reagent is most preferable), and on the basis, when the pH of the prepared solution is more than 3 or less than 1.2, the color developing agent (TMB) does not develop color, so that the TATP detection reagent has the characteristic of clear demarcation point in the aspect of color development, on the basis, the pH value of the prepared solution is adjusted to be 1.2-3.0, so that the occurrence of false detection is directly avoided. In addition, if the hydrochloric acid is too much, the absorbance is reduced, the effect is deteriorated, and the self-oxidation of TMB is caused to affect the detection result, thereby causing a problem of wasting resources.
Example 2:
a preparation method of a standard colorimetric card comprises the following steps: preparing an ethanol solution of TATP, and diluting the ethanol solution of TATP into a plurality of TATP water solutions with different concentrations by using pure water; preparing the detection reagent in the technical scheme; respectively mixing the prepared detection reagent with each part of TATP aqueous solution according to a volume ratio of 99:1, standing in a water bath at 60 ℃ for 6-10min, and recording the color of the detection reagent which acts on each part of TATP aqueous solution after the standing time is finished; and establishing a TATP standard colorimetric card according to the color.
In the method for preparing the standard colorimetric card, since TATP is insoluble in water, an ethanol solution of TATP needs to be prepared first, and in order to reduce the influence of an ethanol solvent, the ethanol solution is diluted by pure water into a plurality of TATP aqueous solutions with different concentrations (for example, 0.05mM, 0.1mM, 0.3mM, 0.5mM, 1mM, 2mM, 3mM and the like). The standard colorimetric card is manufactured, so that the cost is low, frequent and rapid TATP detection on site is greatly facilitated, and the color comparison card is convenient to carry, transport and manufacture in batches.
In another embodiment, the colors are recorded in the form of a picture, and the colors in the picture are extracted by the mobile terminal. And the colors in the pictures are extracted through the mobile terminal to realize sharing and unify the standards.
Example 3:
as shown in fig. 16, a qualitative TATP detection method includes the following steps: wiping the surface of the object to be detected by using filter paper wetted by deionized water; preparing 5mL of detection solution of the detection reagent in the technical scheme, and filling the detection solution into a detection bottle; and putting the filter paper wiped with the object to be detected into a detection bottle filled with the detection solution, putting the detection bottle into a thermos cup filled with water at 60 ℃, standing for 6-10min, observing the color of the detection solution and obtaining a qualitative conclusion.
The TATP qualitative detection method establishes a detection method of TATP on the solid surface (the surface of an article to be detected), wherein TATP is broken and is Fe2+Catalytically produced hydroxyl radicals and Fe3+The TMB is oxidized under the combined action to develop color, has specific ultraviolet absorption wavelength of 450nm, strong anti-interference capability and high sensitivity, and can reach the detection limit of 0.12 mu M. The reaction is a color reaction, colorless transparency is changed into yellow before and after the reaction, the color development is obvious, whether TATP is contained or not is judged rapidly on site, the detection time is saved, meanwhile, the detection method is stable, the prices of related reaction raw materials are not high, and the detection requirements of governments, common enterprises and institutions can be met. In addition, no special reagents such as solid acids and nanoparticles are required, and no complicated pretreatment step is required.
Example 4:
a TATP quantitative detection method comprises the following steps:
(1) preparing the detection reagent in the technical scheme;
(2) mixing the detection reagent and a sample to be detected according to a volume ratio of 99:1, standing in a water bath at 60 ℃ for 6-10min, and observing the color;
(3) comparing the color observed in step (2) with the TATP standard color chart of claim 4 to obtain a corresponding TATP content range value in the sample to be tested.
The TATP quantitative detection method establishes a method for detecting TATP in liquid, wherein TATP is broken and is Fe2+Catalytically produced hydroxyl radicals and Fe3+Co-acting to oxidize TMBThe color is high, the sensitivity is high, the reaction is a color development reaction, the color is changed from colorless transparency to yellow before and after the reaction, the color development is obvious, whether the TATP is contained or not is judged rapidly on site, meanwhile, the content range value of the TATP is detected, correct countermeasures can be made at the first time by definitely detecting the content range value of the TATP, the detection time is saved, meanwhile, the detection method is stable, the prices of related reaction raw materials are not high, and the detection requirements of governments, common enterprises and institutions can be met. In addition, no special reagents such as solid acids and nanoparticles are required, and no complicated pretreatment step is required.
Example 5:
a TATP quantitative detection method comprises the following steps: preparing an ethanol solution of TATP, and diluting the ethanol solution of TATP into a plurality of TATP water solutions with different concentrations by using pure water; preparing the detection reagent in the technical scheme; respectively mixing the prepared detection reagent with each diluted TATP aqueous solution according to a volume ratio of 99:1, standing in a water bath at 60 ℃ for 6-10min, measuring all absorbance values after standing time is finished, and obtaining a corresponding standard curve; mixing the detection reagent and a sample to be detected according to a volume ratio of 99:1, standing in a water bath at 60 ℃ for 6-10min, measuring the absorbance value of the mixed solution of the detection reagent and the sample to be detected after standing, and comparing the absorbance value of the sample to be detected with the standard curve to obtain the corresponding TATP content in the sample to be detected.
The TATP quantitative detection method establishes a method for detecting TATP in liquid, wherein TATP is broken and is broken by TATP and is broken by Fe2+Catalytically produced hydroxyl radicals and Fe3+The TMB is oxidized under the combined action to be developed, has specific ultraviolet absorption wavelength of 450nm, the absorption intensity of the wavelength at 450nm is directly measured by an ultraviolet visible spectrophotometer, the linear relation between the TATP concentration and the corresponding absorption intensity is established, the sensitivity is high, and the detection limit can be as low as 0.12 mu M. The reaction is a color development reaction, the color is changed from colorless transparency to yellow before and after the reaction, the color development is obvious, whether the TATP is contained or not is judged rapidly on site, the TATP content value is detected, the most correct response measures can be taken at the first time by accurately detecting the TATP content value, and the section is thatThe detection time is about, meanwhile, the detection method is stable, the prices of the involved reaction raw materials are not high, and the detection requirements of governments, common enterprises and institutions can be met. In addition, no special reagents such as solid acids and nanoparticles are required, and no complicated pretreatment step is required.
Example 6:
as shown in fig. 1-3, a selection of TATP detection reagents comprises the following steps:
1.1 selection of chromogenic substrates:
(1) preparing a TATP detection solution: diluting 120 times of purchased 36-38% concentrated hydrochloric acid to obtain 100mM hydrochloric acid; 0.0020g of FeCl was weighed2·4H2O powder (or 0.0028g of FeSO)4·7H2O powder), 100mL ferrous solution with the concentration of 0.1mM is prepared for standby; weighing a certain mass of chromogenic substrate solid (3,3',5,5' -Tetramethylbenzidine (TMB), 2 '-dinitro-bis-3-ethylbenzthiazoline-6-sulfonic Acid (ABTS), 1, 2-diaminobenzene (OPD) and 3,3' -Diaminobenzidine (DAB)), preparing 100mL of TMB, ABTS, OPD and DAB solution with the concentration of 0.1mM by using 1mM hydrochloric acid for standby, mixing the hydrochloric acid, the ferrous solution and different chromogenic substrate solutions according to the volume ratio of 6:13:14, and mixing the mixed solution with the total volume of 1.485mL to obtain a TATP detection solution;
(2) preparing TATP solution to be tested: firstly, preparing 10mM TATP ethanol solution, and then diluting by 10 times with deionized water to obtain 1mM TATP water solution;
(3) mixing the TATP detection solution and the solution to be detected according to the volume ratio of 99:1, heating in a water bath at 60 ℃ for 6-10min, measuring the absorbance of the obtained reaction solution within the range of 300-600 nm by using an ultraviolet-visible spectrophotometer, and recording ultraviolet data.
Because ABTS color development sensitivity is low; the OPD is easy to deteriorate by light; compared with TMB, the DAB solution is more complex to prepare, a large amount of precipitate is generated when DAB is directly dissolved by 1mM hydrochloric acid according to the experiment, and the color development of the final reaction is not obvious, so that TMB is adopted as a color developing agent. It can be known that, when hydrochloric acid, ferrous solution and different chromogenic substrate solutions are mixed according to the volume ratio of 6:13:14, the mixed solution with the total volume of 1.485mL is the TATP detection solution, the TATP detection solution and the solution to be detected are mixed according to the volume ratio of 99:1, and the mixture is placed in a water bath at 60 ℃ and heated for 6-10min, ABTS, OPD and DAB cannot achieve the actual use effect. Frequent and rapid detection of TATP in the field cannot be achieved.
1.2 selection of catalytic ions
(1) Preparing a TATP detection solution: diluting 120 times of purchased 36% -38% concentrated hydrochloric acid to obtain 100mM hydrochloric acid; weighing a certain mass of variable valence metal compound, and preparing 100mL of metal ion solution (Fe) with the concentration of 0.1mM2+、Fe3+、Ni+、Cu2 +、Co2+、Mn2+、Zn2+) Standby; 0.0024g of TMB powder was weighed out and 100mL of a 0.1mM TMMB solution was prepared with 1mM hydrochloric acid for use. Mixing hydrochloric acid, a metal ion solution and a TMB solution according to the volume ratio of 6:13:14, wherein the total volume of the mixed solution is 1.485mL, namely the TATP detection solution;
(2) preparing TATP solution to be tested: firstly, preparing 10mM TATP ethanol solution, and then diluting by 10 times with deionized water to obtain 1mM TATP water solution;
(3) mixing the TATP detection solution and the solution to be detected according to the volume ratio of 99:1, heating in a water bath at 60 ℃ for 6-10min, measuring the absorbance of the obtained reaction solution within the range of 300-600 nm by using an ultraviolet-visible spectrophotometer, and recording ultraviolet data.
As shown in FIG. 3, only Fe2+And Fe3+The ions catalyze the reaction due to the use of Fe3+The blank group of the catalyzed solution also turns yellow, and the blank group and the experimental group cannot be distinguished by naked eyes, so that the blank group and the experimental group can be known to be distinguished by naked eyes, wherein hydrochloric acid, ferrous solution and different chromogenic substrate solutions are mixed according to the volume ratio of 6:13:14, the mixed solution with the total volume of 1.485mL is TATP detection solution, the TATP detection solution and the solution to be detected are mixed according to the volume ratio of 99:1, and the mixture is placed in a water bath at 60 ℃ for heating for 6-10min, so that Fe3+、Ni+、Cu2+、Co2+、Mn2+、Zn2+The actual using effect cannot be achieved. Frequent and rapid detection of TATP in the field cannot be achieved. So we use Fe2+As a catalyst.
Example 7:
as shown in fig. 4-8, a TATP detection reagent condition optimization method includes the following steps:
2.1pH optimization:
(1) preparing a TATP detection solution: diluting the purchased concentrated hydrochloric acid of 36% -38% by different times to obtain a series of hydrochloric acids (0mM, 5mM, 10mM, 30mM, 100mM, 170mM, 230mM, 330mM, 500mM) with different concentrations; 0.0020g of FeCl was weighed2·4H2O powder (or 0.0028g of FeSO)4·7H2O powder), 100mL ferrous solution with the concentration of 0.1mM is prepared for standby; 0.0024g of TMB powder was weighed out and 100mL of a 0.1mM TMB solution was prepared with 1mM hydrochloric acid for use. Mixing hydrochloric acid, a ferrous solution and a TMB solution according to a volume ratio of 6:13:14, wherein the total volume of the mixed solution is 1.485mL, namely the TATP detection solution, and the obtained TATP detection solution only has different pH values;
(2) preparing TATP solution to be tested: firstly, preparing 10mM TATP ethanol solution, and then diluting by 10 times with deionized water to obtain 1mM TATP water solution;
(3) mixing the TATP detection solution and the solution to be detected according to a volume ratio of 99:1, heating the mixture in a water bath at 60 ℃ for 6-10min, measuring the absorbance of the obtained reaction solution in a range of 300-600 nm by using an ultraviolet-visible spectrophotometer, recording the peak value of a curve, taking the ultraviolet absorption peak value as a vertical coordinate, taking the final pH value in the solution as a horizontal coordinate, and making a scatter diagram of the relation between the absorption peak value and the pH value concentration. It can be known that when hydrochloric acid, a ferrous solution and different chromogenic substrate solutions are mixed according to a volume ratio of 6:13:14, a mixed solution with a total volume of 1.485mL is a TATP detection solution, the TATP detection solution and a solution to be detected are mixed according to a volume ratio of 99:1, and the mixture is placed in a water bath at 60 ℃ and heated for 6-10min, the pH value is greater than 3.0, or the pH value is less than 1.2, and the actual use effect cannot be achieved. Frequent and rapid detection of TATP in the field cannot be achieved.
2.2Fe2+Concentration optimization
(1) Preparing a TATP detection solution: diluting 120 times of purchased 36% -38% concentrated hydrochloric acid to obtain 100mM hydrochloric acid; weighing certain mass of FeCl2·4H2O powder (or 0.0028g of FeSO)4·7H2O powder) Preparing a series of ferrous solutions (0.007mM, 0.01mM, 0.03mM, 0.04mM, 0.07mM, 0.1mM, 0.15mM and 0.17mM) with different concentrations for later use; 0.0024g of TMB powder was weighed out and 100mL of a 0.1mM TMB solution was prepared with 1mM hydrochloric acid for use. Mixing hydrochloric acid, ferrous solution and TMB solution according to the volume ratio of 6:13:14, wherein the total volume of the mixed solution is 1.485mL, namely the TATP detection solution, and the obtained TATP detection solution is only Fe2+The concentrations are different;
(2) preparing TATP solution to be tested: firstly, preparing 10mM TATP ethanol solution, and then diluting by 10 times with deionized water to obtain 1mM TATP water solution;
(3) mixing the TATP detection solution and the solution to be detected according to a volume ratio of 99:1, heating the mixture in a water bath at 60 ℃ for 6-10min, measuring the absorbance of the obtained reaction solution in the range of 300-600 nm by using an ultraviolet-visible spectrophotometer, recording the peak value of a curve, taking the ultraviolet absorption peak value as a vertical coordinate, and taking Fe in the solution2+The final concentration is taken as an abscissa, and an absorption peak value and Fe are drawn2+Scatter plot of concentration relationship. It can be known that when hydrochloric acid, a ferrous solution and different chromogenic substrate solutions are mixed according to the volume ratio of 6:13:14, a mixed solution with the total volume of 1.485mL is a TATP detection solution, the TATP detection solution and a solution to be detected are mixed according to the volume ratio of 99:1, and the mixture is placed in a water bath at 60 ℃ for heating for 6-10min, the concentration of the ferrous solution is less than 7, the actual use effect cannot be achieved, and frequent and rapid TATP detection on site cannot be achieved. The concentration of the ferrous solution is 7-170 mu M, so that the practical use effect can be met. The concentration of the ferrous solution is more than 170 μ M, which increases the cost, and generally only aims at the condition that the detection requirement is particularly high or the detection environment is special.
2.3TMB concentration optimization
(1) Preparing a TATP detection solution: diluting 120 times of purchased 36% -38% concentrated hydrochloric acid to obtain 100mM hydrochloric acid; 0.0020g of FeCl was weighed2·4H2O powder (or 0.0028g of FeSO)4·7H2O powder), 100mL ferrous solution with the concentration of 0.1mM is prepared for standby; weighing a certain amount of TMB powder, and preparing into a series of TMB solutions (0mM, 0.002mM, 0.006mM, 0.01mM, 0.02 mM) with different concentrations with 1mM hydrochloric acidmM, 0.06mM, 0.1 mM). Mixing hydrochloric acid, ferrous solution and TMB solutions with different concentrations according to the volume ratio of 6:13:14, wherein the mixed solution with the total volume of 1.485mL is TATP detection solution, and the obtained TATP detection solution only has different TMB concentrations;
(2) preparing TATP solution to be tested: firstly, preparing 10mM TATP ethanol solution, and then diluting by 10 times with deionized water to obtain 1mM TATP water solution;
(3) mixing the TATP detection solution and the solution to be detected according to the volume ratio of 99:1, heating the mixture in a water bath at 60 ℃ for 6-10min, measuring the absorbance of the obtained reaction solution in the range of 300-600 nm by using an ultraviolet-visible spectrophotometer, recording the peak value of a curve, taking the ultraviolet absorption peak value as a vertical coordinate, taking the final concentration of TMB in the solution as a horizontal coordinate, and making a scatter diagram of the relation between the absorption peak value and the TMB concentration. It can be known that when hydrochloric acid, a ferrous solution and different chromogenic substrate solutions are mixed according to the volume ratio of 6:13:14, a mixed solution with the total volume of 1.485mL is a TATP detection solution, the TATP detection solution and a solution to be detected are mixed according to the volume ratio of 99:1, and the mixture is placed in a water bath at 60 ℃ for heating for 6-10min, the concentration of the TMB solution is less than 2 mu M, so that the practical use effect cannot be achieved, and frequent and rapid TATP detection on site cannot be achieved. The concentration of the TMB solution is 2-100 mu M, so that the practical use effect can be met. The TMB solution with the concentration of more than 100 mu M can increase the cost, and generally only aims at the condition that the detection requirement is particularly high or the detection environment is special.
2.4 optimization of the reaction temperature
(1) Preparing a TATP detection solution: diluting 120 times of purchased 36% -38% concentrated hydrochloric acid to obtain 100mM hydrochloric acid; 0.0020g of FeCl was weighed2·4H2O powder (or 0.0028g of FeSO)4·7H2O powder), 100mL ferrous solution with the concentration of 0.1mM is prepared for standby; 0.0024g of TMB powder was weighed out and 100mL of a 0.1mM TMB solution was prepared with 1mM hydrochloric acid for use. Mixing hydrochloric acid, a ferrous solution and a TMB solution according to a volume ratio of 6:13:14, wherein the total volume of the mixed solution is 1.485mL, namely TATP detection solution;
(2) preparing TATP solution to be tested: firstly, preparing 10mM TATP ethanol solution, and then diluting by 10 times with deionized water to obtain 1mM TATP water solution;
(3) mixing the TATP detection solution and the solution to be detected according to a volume ratio of 99:1, heating the mixture in water bath at different temperatures (30 ℃, 40 ℃,50 ℃,60 ℃ and 70 ℃), measuring the absorbance within the range of 300nm to 600nm by using an ultraviolet-visible spectrophotometer every 5min, recording the peak value of a curve, taking the ultraviolet absorption peak value as a vertical coordinate and the heating time as a horizontal coordinate, making a scatter diagram of the relation between the absorption peak value and the heating time at different temperatures, and fitting.
2.5 optimization of the reaction time
(1) Preparing a TATP detection solution: the reaction temperature (1) was optimized as 2.4 in example 7;
(2) preparing TATP solution to be tested: firstly, preparing 10mM TATP ethanol solution, and then diluting by 10 times with deionized water to obtain 1mM TATP water solution;
(3) mixing the TATP detection solution and the solution to be detected according to the volume ratio of 99:1, heating in a water bath at 60 ℃, measuring the absorbance within the range of 300-600 nm by using an ultraviolet-visible spectrophotometer every 2min, recording the peak value of a curve, taking the ultraviolet absorption peak value as a vertical coordinate, taking the heating time as a horizontal coordinate, and making a scatter diagram of the relation between the absorption peak value and the time. Therefore, the TATP can be frequently and rapidly detected on site by placing the TATP in a water bath at 60 ℃ for heating for 6-10min, so that the actual using effect can be more satisfied.
Example 8:
as shown in fig. 9-12, the detection range and detection limit of a TATP detection reagent comprises the following steps:
(1) preparing a TATP detection solution: the reaction temperature (1) was optimized as in example 7 at 2.4;
(2) preparing TATP solution to be tested: firstly, preparing 10mM TATP ethanol solution, and diluting the TATP ethanol solution into TATP to-be-detected solutions with different concentrations by using pure water; the concentration of the TATP solution to be detected after dilution is 0mM, 0.05mM, 0.1mM, 0.3mM, 0.5mM, 1mM, 2mM and 3mM respectively;
(3) mixing the TATP detection solution and the solution to be detected according to the volume ratio of 99:1, heating the mixture in a water bath at 60 ℃ for 6-10min, measuring the absorbance of the obtained reaction solution in the range of 300-600 nm by using an ultraviolet-visible spectrophotometer, and fitting ultravioletStandard curve of absorption peak versus TATP concentration. Obtaining a linear relation graph with the ordinate as an absorption peak value and the abscissa as the TATP concentration, wherein the linear relation formula of the TATP concentration and the absorption peak value is A-0.03452C +0.0362, and the square R of the correlation coefficient of the linear relation formula is20.98675, the detection concentration range of the reagent is 0.5-30 mu M, and the detection limit is 0.12 mu M;
(4) and recording the colors of the TATP with different concentrations in the reaction by using a mobile phone, and extracting RGB values by using an AI (analog to digital) element to manufacture a TATP colorimetric card. And standardizing the color comparison card to realize the sharing of the standard color comparison card.
Example 9:
as shown in fig. 13 and 14, a TATP detection reagent for detecting the content of TATP in an actual sample includes the following steps:
4.1 solid surface (e.g., backpack, luggage, etc.) detection
(1) Preparing a TATP detection solution: the reaction temperature (1) was optimized as in example 7 at 2.4;
(2) dripping a drop of 10mM TATP ethanol solution on the solid surface by using a dropper, and wiping the solid surface on which the TATP solution is dripped by using filter paper soaked with deionized water after ethanol volatilizes;
(3) immersing the filter paper with the solid surface wiped in a small bottle filled with 5mL of TATP detection liquid, placing the small bottle in a water bath at 60 ℃ and heating for 6-10min, and measuring the absorbance of the obtained reaction liquid in the range of 300-600 nm by using an ultraviolet-visible spectrophotometer.
4.2 detection of TATP in actual liquid Environment
(1) Preparing a TATP detection solution: the reaction temperature (1) was optimized as in example 7 at 2.4;
(2) preparing a TATP solution to be tested: diluting 10mM ethanol-soluble TATP solution with actual liquid (deionized water, pond water, lake water, bath lotion, soap water, hand cream, hand lotion, mineral water, and soda water) to obtain 1mM TATP solution to be tested (or diluting with deionized water to obtain solution if the actual liquid is too viscous);
(3) mixing the TATP detection solution and the solution to be detected according to the volume ratio of 99:1, heating the mixture in a water bath at 60 ℃ for 6-10min, measuring the absorbance of the obtained reaction solution in the range of 300-600 nm by using an ultraviolet-visible spectrophotometer, recording the peak value of a curve, and drawing a histogram of the absorption peak value and different solvents by using the ultraviolet absorption peak value as a vertical coordinate and different actual solutions as horizontal coordinates.
Example 10:
as shown in fig. 15, the preparation of the TATP detection reagent test paper includes the following steps:
(1) preparing a TATP detection solution: diluting 120 times of purchased 36% -38% concentrated hydrochloric acid to obtain 1M hydrochloric acid; 0.02g of FeCl was weighed2·4H2O powder (or 0.0028g of FeSO)4·7H2O powder), 100mL of ferrous solution with the concentration of 1mM is prepared; 0.024g of TMB powder was weighed out and 100mL of a 1mM TMB solution was prepared with 1mM hydrochloric acid. Mixing hydrochloric acid, a ferrous solution and a TMB solution according to a volume ratio of 6:13:14, wherein a mixed solution with a total volume of 1.485mL is a TATP detection solution (the concentration of each substance is 10 times of that of the TATP detection solution);
(2) manufacturing test paper: cutting the purchased filter paper into paper strips of 0.8cm multiplied by 1cm, adhering the paper strips to plastic strips of 0.8cm multiplied by 5cm to prepare blank test paper, soaking the blank test paper in the TATP detection solution prepared in the step (1) in the embodiment 10, drying the paper strips in an oven after the paper strips are completely soaked, soaking the paper strips in the TATP detection solution prepared in the step (1) in the embodiment 10 again, and drying the paper strips in the oven after the paper strips are completely soaked to obtain the TATP test paper;
(3) dropping TATP ethanol solutions (0mM, 5mM, 10mM, 50mM and 100mM) with different concentrations on a dropper TATP test paper;
(4) and respectively putting the test paper dropwise added with TATP ethanol solutions with different concentrations into clean small bottles, putting the small bottles into a water bath at 60 ℃ for 6-10min, and taking out the test paper.
Example 11:
in order to adapt to complex detection environment (establishing the condition of simultaneous existence of a solid surface and liquid), the TATP qualitative detection method comprises the following steps: wiping the surface of the object to be detected by using filter paper wetted by deionized water; preparing 5mL of detection solution of the detection reagent in the technical scheme, and filling the detection solution into a detection bottle; putting the filter paper wiped with the object to be detected into the detector filled with the detection liquidAnd (4) placing the test bottle into a thermos cup filled with water of 60 ℃, standing for 6-10min, observing the color of the test solution, and obtaining a qualitative conclusion. The TATP qualitative detection method establishes a detection method of TATP on the solid surface (the surface of an article to be detected), wherein TATP is broken and is Fe2+Catalytically produced hydroxyl radicals and Fe3+The TMB is oxidized under the combined action to develop color, has specific ultraviolet absorption wavelength of 450nm, strong anti-interference capability and high sensitivity, and can reach the detection limit of 0.12 mu M. The reaction is a color reaction, colorless transparency is changed into yellow before and after the reaction, the color development is obvious, whether TATP is contained or not is judged rapidly on site, the detection time is saved, meanwhile, the detection method is stable, the prices of related reaction raw materials are not high, and the detection requirements of governments, common enterprises and institutions can be met. In addition, no special reagents such as solid acids and nanoparticles are required, and no complicated pretreatment step is required. A TATP quantitative detection method comprises the following steps: (1) preparing the detection reagent in the technical scheme; (2) mixing the detection reagent and a sample to be detected according to a volume ratio of 99:1, standing in a water bath at 60 ℃ for 6-10min, and observing the color; (3) comparing the color observed in step (2) with the TATP standard color chart of claim 4 to obtain a corresponding TATP content range value in the sample to be tested. The TATP quantitative detection method establishes a method for detecting TATP in liquid, wherein TATP is broken and is Fe2+Catalytically produced hydroxyl radicals and Fe3+The TMB is oxidized under the combined action to be colored, the sensitivity is high, the reaction is a color development reaction, the color is changed into yellow from colorless transparency before and after the reaction, the color development is obvious, whether the TATP is contained or not is judged rapidly on site, meanwhile, the content range value of the TATP is detected, correct counter measures can be made at the first time by definitely detecting the content range value of the TATP, the detection time is saved, meanwhile, the detection method is stable, the price of related reaction raw materials is not high, and the detection requirements of governments, common enterprises and institutions can be met. In addition, no special reagents such as solid acids and nanoparticles are required, and no complicated pretreatment step is required. A TATP quantitative detection method comprises the following steps: ethanol solution for preparing TATPDiluting the solution into multiple TATP aqueous solutions with different concentrations by using pure water; preparing the detection reagent in the technical scheme; respectively mixing the prepared detection reagent with each diluted TATP aqueous solution according to a volume ratio of 99:1, standing in a water bath at 60 ℃ for 6-10min, measuring all absorbance values after standing time is finished, and obtaining a corresponding standard curve; mixing the detection reagent and a sample to be detected according to a volume ratio of 99:1, standing in a water bath at 60 ℃ for 6-10min, measuring the absorbance value of the mixed solution of the detection reagent and the sample to be detected after standing, and comparing the absorbance value of the sample to be detected with the standard curve to obtain the corresponding TATP content in the sample to be detected. The TATP quantitative detection method establishes a method for detecting TATP in liquid, wherein TATP is broken and is Fe2+Catalytically produced hydroxyl radicals and Fe3+The TMB is oxidized under the combined action to be developed, has specific ultraviolet absorption wavelength of 450nm, the absorption intensity of the wavelength at 450nm is directly measured by an ultraviolet visible spectrophotometer, the linear relation between the TATP concentration and the corresponding absorption intensity is established, the sensitivity is high, and the detection limit can be as low as 0.12 mu M. The reaction is a color reaction, the color is changed into yellow from colorless transparency before and after the reaction, the color development is obvious, whether the TATP is contained or not is judged rapidly on site, the most correct counter measures can be taken at the first time by accurately detecting the content value of the TATP, the detection time is saved, meanwhile, the detection method is stable, the price of related reaction raw materials is not high, and the detection requirements of governments, common enterprises and institutions can be met. In addition, no special reagents such as solid acids and nanoparticles are required, and no complicated pretreatment step is required.
Example 12
Any two or more of examples 1 to 11 are combined.
The above-mentioned embodiments only express the specific embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the present invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.

Claims (6)

1. The TATP detection reagent is characterized by comprising hydrochloric acid, a ferrous solution and a TMB solution, wherein the volume ratio of the hydrochloric acid to the ferrous solution to the TMB solution is 6:13: 14; the concentration of the ferrous solution is 7-170 mu M; the concentration of the TMB solution is 2-100 mu M; the hydrochloric acid concentration is 20-500 mM, and the pH of a preparation solution obtained after the hydrochloric acid, the ferrous solution and the TMB solution are prepared according to the volume ratio of 6:13:14 is 1.2-3.0.
2. The preparation method of the standard colorimetric card is characterized by comprising the following steps of:
preparing an ethanol solution of TATP, and diluting the ethanol solution of TATP into a plurality of TATP water solutions with different concentrations by using pure water;
formulating the detection reagent of claim 1;
respectively mixing the prepared detection reagent with each part of TATP aqueous solution according to a volume ratio of 99:1, standing at a set temperature for a set time, and recording the color of the detection reagent which is respectively acted with each part of TATP aqueous solution;
and establishing a TATP standard colorimetric card according to the color.
3. The method for preparing a standard colorimetric card according to claim 2,
and recording the colors in a picture form, and extracting the colors in the picture through the mobile terminal.
4. A TATP qualitative detection method is characterized by comprising the following steps:
wiping the surface of the object to be detected by using filter paper wetted by deionized water;
preparing a test solution of the test reagent according to claim 1 and filling the test solution into a test bottle;
and putting the filter paper wiped with the object to be detected into a detection bottle filled with the detection solution, putting the detection bottle into an environment with a set temperature, standing for a preset time, observing the color of the detection solution, and obtaining a qualitative conclusion.
5. A TATP quantitative detection method is characterized by comprising the following steps:
(1) formulating the detection reagent of claim 1;
(2) mixing the detection reagent and a sample to be detected according to a volume ratio of 99:1, standing in a set temperature environment for a set time, and observing the color;
(3) comparing the color observed in step (2) with the TATP standard color chart of claim 2 to obtain a corresponding TATP content range value in the sample to be tested.
6. A TATP quantitative detection method is characterized by comprising the following steps:
preparing an ethanol solution of TATP, and diluting the ethanol solution of TATP into a plurality of TATP water solutions with different concentrations by using pure water;
formulating the detection reagent of claim 1;
respectively mixing the prepared detection reagent with each diluted TATP aqueous solution according to a volume ratio of 99:1, standing in a set temperature environment for a set time, and then measuring all absorbance values to obtain a corresponding standard curve;
mixing the detection reagent and a sample to be detected according to a volume ratio of 99:1, standing in a set temperature environment for a set time, measuring the absorbance value of a solution formed by mixing the detection reagent and the sample to be detected,
and comparing the absorbance value of the sample to be detected with the standard curve to obtain the corresponding TATP content in the sample to be detected.
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