CN114527084A - Reagent for rapidly detecting trinitrotoluene, terbutal, picric acid, dinitrotoluene and sulfur in explosive - Google Patents
Reagent for rapidly detecting trinitrotoluene, terbutal, picric acid, dinitrotoluene and sulfur in explosive Download PDFInfo
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- CN114527084A CN114527084A CN202210166281.2A CN202210166281A CN114527084A CN 114527084 A CN114527084 A CN 114527084A CN 202210166281 A CN202210166281 A CN 202210166281A CN 114527084 A CN114527084 A CN 114527084A
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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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Abstract
The invention provides a reagent for rapidly detecting trinitrotoluene, troxerex, picric acid, dinitrotoluene and sulfur in explosives. The reagent is prepared from an organic probe (E)2- (3-cyano-4- (4- (dimethylamino) styryl) -5, 5-dimethylfuran-2 (5H) -ylidene) malononitrile, a reducing agent sodium borohydride or potassium borohydride and a solvent based on a chemical colorimetric method, and whether trinitrotoluene, tetrol, picric acid, dinitrotoluene and sulfur exist or not is determined according to different changes of colors after reaction. The reagent can be used for rapid qualitative detection of trinitrotoluene, troxerex, picric acid, dinitrotoluene and sulfur in explosives and residues thereof on site. The method has the characteristics of low cost, simple reaction condition, easy preparation, good reproducibility, high sensitivity and the like.
Description
Technical Field
The invention belongs to the field of detection of raw materials of environmental, standard and nonstandard explosives, and relates to a reagent for quickly detecting trinitrotoluene, tetrol, picric acid, dinitrotoluene and sulfur in explosives.
Background
2,4, 6-trinitrotoluene (TNT), Dinitrotoluene (DNT), trolene, and PA are commonly used nitroaromatic explosives. Nitroaromatic explosives are bioaccumulating and highly toxic, their chemical structures are unstable and can adversely affect the ecological environment and public safety (carbon,2017,10: 314-. Improper use can result in release into soil, groundwater, and even food, which can cause anemia, liver damage, cataracts, and cancer (Forensic Science International,2012,222: 340-. The saturated vapor pressure of the nitro-aromatic hydrocarbon explosives under the room temperature condition is relatively low, which causes great difficulty in detection. The use of sulfur in China has a long history, and the invention of gunpowder by sulfur is provided by our ancestors as early as more than a thousand years ago. As the sulfur is widely applied to agricultural production, industry and life, the sulfur comprises sulfur ore, insecticide, oil well, black powder, vulcanized rubber, match head, sulfur soap or paste, has active chemical property, and is combusted or exploded with mixed solution of oxidant. The detection methods of nitroaromatic explosives and sulfur are mainly carried out off-site, and involve complicated instruments, such as gas chromatography (Journal of Chromatographic Science,1998,36: 406-. Most of these techniques are sensitive and efficient, but frequent instrument calibration, lengthy and cumbersome procedures limit their application in field analysis. Liu Yong et al disclose a colorimetric gel paste for detecting explosives, which is prepared from hydrogel, a colorimetric reagent, a humectant and a thickener under the ultraviolet curing condition, has harsh conditions and complex components, and can not detect multiple explosives simultaneously by one paste because different colorimetric reagents are required to be added to prepare corresponding pastes for detecting different explosives. (CN 110849871A)
In the invention, a colorimetric-based detection method provides a detection reagent containing an organic probe and a reducing agent, five substances of trinitrotoluene (TNT), terbutal, Picric Acid (PA), Dinitrotoluene (DNT) and sulfur (S) can be distinguished simultaneously, the reagent is simple to prepare, convenient to operate, rapid, sensitive and high in selectivity, the purpose of detecting various explosives by using one detection reagent can be achieved, and a rapid and effective means is provided for visually detecting the explosives.
Disclosure of Invention
The invention aims to provide a reagent for rapidly detecting trinitrotoluene, terbutaline, picric acid, dinitrotoluene and sulfur in explosives. The reagent is prepared from an organic probe (E)2- (3-cyano-4- (4- (dimethylamino) styryl) -5, 5-dimethylfuran-2 (5H) -ylidene) malononitrile, a reducing agent sodium borohydride or potassium borohydride and a solvent based on a chemical colorimetric method, and whether trinitrotoluene, terbutal, picric acid, dinitrotoluene and sulfur exist is determined according to different changes of colors after reaction. If the substance to be detected contains trinitrotoluene (TNT), the reagent is changed from colorless transparency to ancient pink; if the substance to be detected contains the Cherokee rose, the color of the reagent is changed into the color of the; if the substance to be detected contains Picric Acid (PA), the color of the reagent turns to orange red; if the substance to be detected contains Dinitrotoluene (DNT), the color of the reagent is changed into gentian blue; if the substance to be detected contains sulfur (S), the color of the reagent turns into moss green. The reagent provided by the invention can be used for rapid qualitative detection of TNT, Tetro, PA, DNT and S in explosives and residues thereof in explosion cases, search and elimination sites. The method has the characteristics of low cost, simple reaction condition, easy preparation, good reproducibility, high sensitivity and the like.
The invention relates to a reagent for rapidly detecting trinitrotoluene, terbutaline, picric acid, dinitrotoluene and sulfur in explosives, which is prepared from an organic probe, a reducing agent and a solvent, wherein:
the chemical name of the organic probe is: (E)2- (3-cyano-4- (4- (dimethylamino) styryl) -5, 5-dimethylfuran-2 (5H) -ylidene) malononitrile;
the reducing agent is sodium borohydride or potassium borohydride;
the solvent is N, N-dimethylformamide, dimethyl sulfoxide or ethylene glycol anisole;
the preparation method of the reagent comprises the following steps:
a. dissolving an organic probe (E)2- (3-cyano-4- (4- (dimethylamino) styryl) -5, 5-dimethyl furan-2 (5H) -ylidene) malononitrile into N, N-dimethylformamide, dimethyl sulfoxide or ethylene glycol anisole serving as a solvent to prepare a probe solution with the concentration of 0.01-5 mu g/mu L;
b. and (b) adding the probe solution obtained in the step (a) into a reducing agent sodium borohydride or potassium borohydride according to the mass ratio of 20:1-5:1, and carrying out ultrasonic treatment for 5-20min to obtain a reagent for rapidly detecting the explosives trinitrotoluene, terbuthylazine, picric acid, dinitrotoluene and sulfur.
The reagent for rapidly detecting trinitrotoluene, terbuthylazine, picric acid, dinitrotoluene and sulfur in explosives is characterized in that a solution is changed from colorless transparency to ancient pink when the trinitrotoluene is detected, the solution is changed into southwestern purple when the terbuthylazine is detected, the solution is changed into orange red when the picric acid is detected, the solution is changed into gentian blue when the dinitrotoluene is detected, and the solution is changed into moss green when the sulfur is detected.
The invention relates to a reagent for rapidly detecting trinitrotoluene, terbutal, picric acid, dinitrotoluene and sulfur in explosives, wherein the chemical structure of an organic probe is as follows:
the chemical name of the organic probe is as follows: (E)2- (3-cyano-4- (4- (dimethylamino) styryl) -5, 5-dimethylfuran-2 (5H) -ylidene) malononitrile, designated DMA-CN;
the prepared detection reagent is applied to the colorimetric detection of trinitrotoluene (TNT), terbuthylar, Picric Acid (PA), Dinitrotoluene (DNT) and sulfur (S), and the specific method is as follows:
(1) weighing 0.0227g of trinitrotoluene (TNT) and dissolving in 10mL of acetonitrile to prepare a trinitrotoluene (TNT) solution with the standard solution concentration of 10 mM; weighing 0.0287g of terbutaline, dissolving in 10mL of acetonitrile, and preparing a standard solution of terbutaline with the concentration of 10 mM; weighing 0.0183g of Picric Acid (PA) and dissolving in 10mL of acetone to prepare a Picric Acid (PA) solution with a standard solution concentration of 8 mM; 0.1821g of Dinitrotoluene (DNT) is weighed and dissolved in 10mL of acetone to prepare a Dinitrotoluene (DNT) solution with the standard solution concentration of 0.1M; weighing 1.6g of sulfur (S) and dissolving in 10mL of toluene to prepare a sulfur (S) solution with the standard solution concentration of 5M;
(2) testing the absorbance change and color change of the reagent before and after the trinitrotoluene (TNT), the terbutaline, the Picric Acid (PA), the Dinitrotoluene (DNT) and the sulfur (S) are added by using an ultraviolet-visible spectrophotometer;
(3) the volume of the detection reagent scanned by ultraviolet-visible absorption spectrum is 3mL, and the volumes of standard TNT, Terylene, PA, DNT and S solutions with different concentrations are respectively added to 20 muL.
The invention relates to a reagent for rapidly detecting trinitrotoluene (TNT), tetrol, picric acid, Dinitrotoluene (DNT) in standard explosives and sulfur (S) in non-standard explosives, which mainly aims at detecting the components of trinitrotoluene (TNT), tetrol, Picric Acid (PA), Dinitrotoluene (DNT) in standard explosives and sulfur (S) in non-standard explosives, solves the problem that the current detection means cannot distinguish the poor stability of trinitrotoluene (TNT), tetrol, Picric Acid (PA), Dinitrotoluene (DNT) and sulfur (S) reagents at the same time, and is green, non-toxic, high-stability, rapid, visual and low in cost.
Compared with the prior art, the invention has the beneficial effects that:
1. the detection reagent can simultaneously realize the detection of trinitrotoluene (TNT), terbutal, Picric Acid (PA), Dinitrotoluene (DNT) and sulfur (S), saves the cost and has high detection efficiency;
2. the detection reagent can sensitively and selectively detect trinitrotoluene (TNT), terbutal, Picric Acid (PA), Dinitrotoluene (DNT) and sulfur (S);
3. the detection reagent disclosed by the invention is quick in reaction, and can realize the identification of trinitrotoluene (TNT), terbutal, Picric Acid (PA), Dinitrotoluene (DNT) and sulfur (S) within 1S;
4. the detection reagent provided by the invention is used for detecting trinitrotoluene (TNT), terbuthylazine, Picric Acid (PA), Dinitrotoluene (DNT) and sulfur (S), does not need complex analysis equipment, and can be directly identified and detected by naked eyes;
5. the detection reagent does not need to carry out any pretreatment on the object to be detected, is simple to operate and is convenient to popularize and apply.
Drawings
FIG. 1 shows the reagent of the present invention (solvent is N, N-Dimethylformamide (DMF), NaBH4Mass ratio of DMA-CN is 10:1) and 10mM TNT, and the insets are photographs of color change of the reagent and TNT before and after reaction;
FIG. 2 shows the reagent of the present invention (solvent is dimethyl sulfoxide, KBH4Mass ratio of DMA-CN is 6:1) and 10mM of Terylene, and the insets are photographs of color change of reagents before and after reaction taken by a camera;
FIG. 3 shows the reagent of the present invention (solvent is N, N-Dimethylformamide (DMF), NaBH4The mass ratio of the reagent to the DMA-CN is 14:1), ultraviolet-visible absorption spectrograms before and after reaction with 8mM picric acid, and the insets are photographs of the color change of the reagent before and after the reaction, which are taken by a camera.
FIG. 4 shows the reagent of the present invention (the solvent is ethylene glycol anisole, KBH)4Mass ratio of DMA-CN is 20:1) and 0.1M DNT, and the insets are photographs of color changes of reagents before and after reaction and taken by a camera;
FIG. 5 shows the reagent of the present invention (solvent is N, N-Dimethylformamide (DMF), NaBH4Mass ratio of DMA-CN is 5:1) and ultraviolet-visible absorption spectrograms before and after reaction with 5M sulfur, and the inset is a picture of color change of the reagent before and after reaction taken by a camera.
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
a. Dissolving 10mg of organic probe (E), 2- (3-cyano-4- (4- (dimethylamino) styryl) -5, 5-dimethylfuran-2 (5H) -ylidene) malononitrile, in 50mL of N, N-dimethylformamide as a solvent at room temperature to prepare a probe solution with the concentration of 0.2 mu g/mu L;
b. and (b) adding a reducing agent which is 100mg of sodium borohydride into the probe solution obtained in the step a, and performing ultrasonic treatment for 5min to obtain a detection reagent for rapidly detecting the colorless explosives, namely trinitrotoluene, terbutal, picric acid, dinitrotoluene and sulfur.
Measuring 3mL of detection reagent in a quartz cuvette, adding 20 muL of prepared 10mM trinitrotoluene (TNT) standard solution, performing ultraviolet-visible absorption spectrum scanning by an ultraviolet-visible spectrophotometer, wherein spectrograms before and after trinitrotoluene (TNT) is added are shown in figure 1, and the comparison of the spectrograms before and after reaction shows that an obvious absorption peak appears at 511nm after reaction, directly photographing the reagent before and after reaction (shown in figure 1), and comparing the photos of the reagent before and after reaction shows that the reagent is changed from colorless to paleness pink.
Example 2
a. Dissolving 5mg of organic probe (E), 2- (3-cyano-4- (4- (dimethylamino) styryl) -5, 5-dimethylfuran-2 (5H) -ylidene) malononitrile, in 500mL of dimethyl sulfoxide as a solvent at room temperature to prepare a probe solution with the concentration of 0.01 mu g/mu L;
b. and (b) adding 30mg of potassium borohydride serving as a reducing agent into the probe solution obtained in the step a, and performing ultrasonic treatment for 10min to obtain a reagent for rapidly detecting colorless explosives, namely trinitrotoluene, terbutal, picric acid, dinitrotoluene and sulfur.
Measuring 3mL of detection reagent in a quartz cuvette, adding 20 μ L of prepared 10mM Terra standard solution, performing ultraviolet-visible absorption spectrum scanning by using an ultraviolet-visible spectrophotometer, wherein spectrograms before and after the Terra is added are shown in figure 2, and comparing the spectrograms before and after the reaction to show that an obvious absorption peak appears at a position of 520nm after the reaction, directly photographing the reagent before and after the reaction (shown in an insert picture of figure 2), and comparing the reagent photos before and after the reaction to show that the reagent is changed from colorless to purple in south of Shinan.
Example 3
a. Dissolving 5mg of organic probe (E), 2- (3-cyano-4- (4- (dimethylamino) styryl) -5, 5-dimethylfuran-2 (5H) -ylidene) malononitrile, in 50mL of N, N-dimethylformamide as a solvent at room temperature to prepare a probe solution with the concentration of 0.1 mu g/mu L;
b. and (b) adding a reducing agent of 60mg of sodium borohydride into the probe solution obtained in the step a, and performing ultrasonic treatment for 15min to obtain a reagent for rapidly detecting colorless explosives, namely trinitrotoluene, terbutal, picric acid, dinitrotoluene and sulfur.
Measuring 3mL of detection reagent in a quartz cuvette, adding 20 muL of prepared 8mM picric acid standard solution, performing ultraviolet-visible absorption spectrum scanning by using an ultraviolet-visible spectrophotometer, wherein spectrograms before and after the picric acid is added are shown in figure 3, comparing the spectrograms before and after the reaction, two obvious absorption peaks appear at 420nm and 517nm after the reaction, directly photographing the reagent before and after the reaction (shown in an inset in figure 3), and comparing the reagent photos before and after the reaction to show that the reagent is changed from colorless to orange red after the reaction.
Example 4
a. Dissolving 10mg of organic probe (E), 2- (3-cyano-4- (4- (dimethylamino) styryl) -5, 5-dimethylfuran-2 (5H) -ylidene) malononitrile, in 20mL of ethylene glycol anisole serving as a solvent, at room temperature to prepare a probe solution with the concentration of 2 mu g/mu L;
b. and (b) adding 200mg of reducing agent potassium borohydride into the probe solution obtained in the step a according to the mass ratio of 20:1-5:1, and performing ultrasonic treatment for 20min to obtain the reagent for rapidly detecting the explosive trinitrotoluene, the terbuthylazine, the picric acid, the dinitrotoluene and the sulfur.
3mL of the detection reagent was weighed into a quartz cuvette, and 20. mu.L of the prepared 0.1M Dinitrotoluene (DNT) standard solution was added thereto. The ultraviolet-visible spectrophotometer scans the ultraviolet-visible absorption spectrum, the spectrograms before and after adding Dinitrotoluene (DNT) are shown in figure 4, and the spectrograms before and after reaction are compared to show that an obvious absorption peak appears at 592nm after reaction. Direct photographs of the reagents before and after the reaction were taken (as shown in the inset of fig. 4), and the color of the reagents after the reaction changed from colorless to gentian blue by comparing the photographs of the reagents before and after the reaction.
Example 5
a. Dissolving 100mg of organic probe (E), 2- (3-cyano-4- (4- (dimethylamino) styryl) -5, 5-dimethylfuran-2 (5H) -ylidene) malononitrile, in 20mL of N, N-dimethylformamide as a solvent at room temperature to prepare a probe solution with the concentration of 5 mu g/mu L;
b. and (b) adding a reducing agent of 500mg of sodium borohydride into the probe solution obtained in the step a, and performing ultrasonic treatment for 20min to obtain a reagent for rapidly detecting explosives of trinitrotoluene, terbutaline, picric acid, dinitrotoluene and sulfur.
Measuring 3mL of detection reagent in a quartz cuvette, adding 20 mu L of prepared 5M sulfur standard solution, performing ultraviolet-visible absorption spectrum scanning by an ultraviolet-visible spectrophotometer, wherein spectrograms before and after adding sulfur are shown in figure 5, and comparing the spectrograms before and after reaction to show that an obvious absorption peak appears at 619nm after reaction, directly photographing the reagent before and after reaction (shown in an inset in figure 5), and comparing the photographs of the reagent before and after reaction to show that the reagent after reaction is changed from colorless into moss green.
The above embodiments describe the present invention and it will be appreciated that the use of the reagent in TNT, DNT, toddler, picric acid, S detection in other fields is equally applicable without departing from the spirit of the invention. The ratio of the reagent components in the present invention can be adjusted, and such changes are also within the scope of the present invention.
Claims (2)
1. A reagent for rapidly detecting trinitrotoluene, terbutal, picric acid, dinitrotoluene and sulfur in explosives is characterized in that the reagent is prepared from an organic probe, a reducing agent and a solvent, wherein:
the chemical name of the organic probe is: (E)2- (3-cyano-4- (4- (dimethylamino) styryl) -5, 5-dimethylfuran-2 (5H) -ylidene) malononitrile;
the reducing agent is sodium borohydride or potassium borohydride;
the solvent is N, N-dimethylformamide, dimethyl sulfoxide or ethylene glycol anisole;
the preparation method of the reagent comprises the following steps:
a. dissolving an organic probe (E)2- (3-cyano-4- (4- (dimethylamino) styryl) -5, 5-dimethylfuran-2 (5H) -ylidene) malononitrile in N, N-dimethylformamide, dimethyl sulfoxide or ethylene glycol anisole to prepare a probe solution with the concentration of 0.01-5 mug/muL;
b. and (b) adding the probe solution obtained in the step (a) into a reducing agent sodium borohydride or potassium borohydride according to the mass ratio of 20:1-5:1, and carrying out ultrasonic treatment for 5-20min to obtain a reagent for rapidly detecting the explosives trinitrotoluene, terbuthylazine, picric acid, dinitrotoluene and sulfur.
2. The reagent of claim 1, wherein the reagent is selected from the group consisting of trinitrotoluene, tetrol, picric acid, dinitrotoluene, and sulfur, wherein the solution changes from colorless and transparent to ancient pink when detecting trinitrotoluene, changes to southwestern purple when detecting tetrol, changes to orange red when detecting picric acid, changes to gentian blue when detecting dinitrotoluene, and changes to moss green when detecting sulfur.
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