CN114527084B - Reagent for rapidly detecting trinitrotoluene, tredrone, picric acid, dinitrotoluene and sulfur in explosive - Google Patents
Reagent for rapidly detecting trinitrotoluene, tredrone, picric acid, dinitrotoluene and sulfur in explosive Download PDFInfo
- Publication number
- CN114527084B CN114527084B CN202210166281.2A CN202210166281A CN114527084B CN 114527084 B CN114527084 B CN 114527084B CN 202210166281 A CN202210166281 A CN 202210166281A CN 114527084 B CN114527084 B CN 114527084B
- Authority
- CN
- China
- Prior art keywords
- reagent
- sulfur
- dinitrotoluene
- picric acid
- trinitrotoluene
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
- 239000003153 chemical reaction reagent Substances 0.000 title claims abstract description 74
- DYSXLQBUUOPLBB-UHFFFAOYSA-N 2,3-dinitrotoluene Chemical compound CC1=CC=CC([N+]([O-])=O)=C1[N+]([O-])=O DYSXLQBUUOPLBB-UHFFFAOYSA-N 0.000 title claims abstract description 57
- SPSSULHKWOKEEL-UHFFFAOYSA-N 2,4,6-trinitrotoluene Chemical compound CC1=C([N+]([O-])=O)C=C([N+]([O-])=O)C=C1[N+]([O-])=O SPSSULHKWOKEEL-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 239000000015 trinitrotoluene Substances 0.000 title claims abstract description 56
- OXNIZHLAWKMVMX-UHFFFAOYSA-N picric acid Chemical compound OC1=C([N+]([O-])=O)C=C([N+]([O-])=O)C=C1[N+]([O-])=O OXNIZHLAWKMVMX-UHFFFAOYSA-N 0.000 title claims abstract description 54
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 239000011593 sulfur Substances 0.000 title claims abstract description 43
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 43
- 239000002360 explosive Substances 0.000 title claims abstract description 31
- -1 tredrone Chemical compound 0.000 title claims abstract description 31
- 239000000523 sample Substances 0.000 claims abstract description 31
- 239000002904 solvent Substances 0.000 claims abstract description 18
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 13
- 239000012279 sodium borohydride Substances 0.000 claims abstract description 9
- 229910000033 sodium borohydride Inorganic materials 0.000 claims abstract description 9
- 239000000126 substance Substances 0.000 claims abstract description 9
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000011591 potassium Substances 0.000 claims abstract description 8
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 8
- 125000002147 dimethylamino group Chemical group [H]C([H])([H])N(*)C([H])([H])[H] 0.000 claims abstract description 4
- CUONGYYJJVDODC-UHFFFAOYSA-N malononitrile Chemical compound N#CCC#N CUONGYYJJVDODC-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000002360 preparation method Methods 0.000 claims abstract description 4
- 125000005504 styryl group Chemical group 0.000 claims abstract description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical group CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 33
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 11
- FIBBPEJAEPTGCC-JXMROGBWSA-N C1=CC(N(C)C)=CC=C1\C=C\C1=C(C#N)C(=C(C#N)C#N)OC1(C)C Chemical compound C1=CC(N(C)C)=CC=C1\C=C\C1=C(C#N)C(=C(C#N)C#N)OC1(C)C FIBBPEJAEPTGCC-JXMROGBWSA-N 0.000 claims description 7
- 238000009210 therapy by ultrasound Methods 0.000 claims description 7
- GQNQSLYDYJFYRM-UHFFFAOYSA-N anisole;ethane-1,2-diol Chemical compound OCCO.COC1=CC=CC=C1 GQNQSLYDYJFYRM-UHFFFAOYSA-N 0.000 claims description 6
- 241001071795 Gentiana Species 0.000 claims description 4
- BPJYAXCTOHRFDQ-UHFFFAOYSA-L tetracopper;2,4,6-trioxido-1,3,5,2,4,6-trioxatriarsinane;diacetate Chemical compound [Cu+2].[Cu+2].[Cu+2].[Cu+2].CC([O-])=O.CC([O-])=O.[O-][As]1O[As]([O-])O[As]([O-])O1.[O-][As]1O[As]([O-])O[As]([O-])O1 BPJYAXCTOHRFDQ-UHFFFAOYSA-L 0.000 claims description 4
- 238000006243 chemical reaction Methods 0.000 abstract description 37
- 238000004737 colorimetric analysis Methods 0.000 abstract description 3
- 239000003086 colorant Substances 0.000 abstract description 2
- 230000035945 sensitivity Effects 0.000 abstract description 2
- 238000001514 detection method Methods 0.000 description 25
- 239000000243 solution Substances 0.000 description 23
- 238000000862 absorption spectrum Methods 0.000 description 10
- 239000012086 standard solution Substances 0.000 description 10
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 6
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- 239000010453 quartz Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 238000004880 explosion Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 208000002177 Cataract Diseases 0.000 description 1
- 206010067125 Liver injury Diseases 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- 239000012491 analyte Substances 0.000 description 1
- 238000004164 analytical calibration Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 208000007502 anemia Diseases 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 231100000693 bioaccumulation Toxicity 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 239000003673 groundwater Substances 0.000 description 1
- 230000005802 health problem Effects 0.000 description 1
- 231100000234 hepatic damage Toxicity 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 239000003906 humectant Substances 0.000 description 1
- 239000000017 hydrogel Substances 0.000 description 1
- 238000010249 in-situ analysis Methods 0.000 description 1
- 230000008818 liver damage Effects 0.000 description 1
- 238000004949 mass spectrometry Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 239000003129 oil well Substances 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000004416 surface enhanced Raman spectroscopy Methods 0.000 description 1
- 238000002198 surface plasmon resonance spectroscopy Methods 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 239000004636 vulcanized rubber Substances 0.000 description 1
Classifications
-
- 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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
Landscapes
- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Biochemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
The invention provides a reagent for rapidly detecting trinitrotoluene, special dropen, 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) -subunit) malononitrile, a reducing agent sodium borohydride or potassium borohydride and a solvent based on a chemical colorimetric method, and whether trinitrotoluene, tredrone, picric acid, dinitrotoluene and sulfur exist or not is determined according to different changes of colors after the reaction. The reagent disclosed by the invention can be used for rapidly and qualitatively detecting trinitrotoluene, tredrone, picric acid, dinitrotoluene and sulfur in explosives and residues thereof in a site. 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 environment and standard and non-standard explosive raw material detection, and relates to a reagent for rapidly detecting trinitrotoluene, special droter, picric acid, dinitrotoluene and sulfur in explosives.
Background
2,4, 6-Trinitrotoluene (TNT), dinitrotoluene (DNT), tertrene and PA are common nitroaromatic explosives. Nitroaromatic explosives are bioaccumulative and highly toxic, their chemical structure is unstable, and can have adverse effects on the ecological environment and public safety (carbon, 2017, 10:314-319). Unreasonable use can result in its release into soil, groundwater and even food, causing health problems such as anemia, liver damage, cataracts and cancer to people (Forensic Science International,2012, 222:340-345). The saturated vapor pressure of nitroaromatic explosives at room temperature is relatively low, which makes detection extremely difficult. Sulfur has a long history in our country, and our ancestors invented powder with sulfur as early as one thousand years ago. Because sulfur is widely applied to agricultural production, industry and life, and comprises sulfur mine, pesticide, oil well, black powder, vulcanized rubber, match head, sulfur soap or paste, has active chemical property, and burns or explodes with mixed solution of oxidant. The detection methods of nitroaromatic explosives and sulfur commonly used are mainly performed outside the field, and involve complex instruments such as gas chromatography (Journal of Chromatographic Science,1998, 36:406-416), high performance liquid chromatography (analytical 2014, 139:807-812), mass spectrometry (Journal of MATERIALS CHEMISTRY, 200035:337-346), surface enhanced raman spectroscopy (analytical, 2014, 139:807-812), surface plasmon resonance spectroscopy (Sensors and Actuators, B,2014, 804-811), chemiluminescence, colorimetry, and the like. Most of these techniques are sensitive and efficient, but frequent instrument calibration, tedious and cumbersome procedures limit their application to in situ analysis. Liu Yong et al discloses a colorimetric gel paste for detecting explosives, which consists of hydrogel, colorimetric reagent, humectant and thickener, and is prepared under ultraviolet light curing conditions, wherein the conditions are harsh, the components are complex, different colorimetric reagents are required to be added for detecting different explosives to prepare corresponding pastes, and multiple explosives cannot be detected simultaneously by one paste. (CN 110849871A)
According to the colorimetric-based detection method, a detection reagent containing an organic probe and a reducing agent is provided, five substances including trinitrotoluene (TNT), special dropen, picric Acid (PA), dinitrotoluene (DNT) and sulfur (S) can be distinguished at the same time, the reagent is simple to prepare, convenient and quick to operate, sensitive and high in selectivity, the purpose of detecting various explosives by the detection reagent can be achieved, and meanwhile, a quick and effective means is provided for realizing visual detection of the explosives.
Disclosure of Invention
The invention aims at providing a reagent for rapidly detecting trinitrotoluene, tedrone, 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) -subunit) malononitrile, a reducing agent sodium borohydride or potassium borohydride and a solvent based on a chemical colorimetric method, and whether trinitrotoluene, tredrone, picric acid, dinitrotoluene and sulfur exist or not is determined according to different changes of colors after the reaction. If trinitrotoluene (TNT) is contained in the object to be detected, the reagent changes from colorless and transparent into paleo pink; if the object to be detected contains the special drove, the color of the reagent is changed into a lithiumann purple color; if Picric Acid (PA) is contained in the object to be detected, the color of the reagent becomes orange; if the analyte contains Dinitrotoluene (DNT), the color of the reagent changes to gentian blue; when sulfur (S) is contained in the sample, the color of the reagent becomes moss green. The reagent disclosed by the invention can be used for quick qualitative detection of TNT, special yield, PA, DNT and S in explosives and residues thereof in explosion cases and explosion searching and discharging sites. 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, special droner, 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-dimethylfuran-2 (5H) -subunit) malononitrile in N, N-dimethylformamide, dimethyl sulfoxide or ethylene glycol anisole as a solvent to prepare a probe solution with the concentration of 0.01-5 mug/mug;
b. And d, adding a reducing agent into the probe solution obtained in the step a to obtain sodium borohydride or potassium borohydride according to the mass ratio of 20:1-5:1, and performing ultrasonic treatment for 5-20min to obtain the reagent for rapidly detecting the explosive trinitrotoluene, the terdrone, the picric acid, the dinitrotoluene and the sulfur.
The reagent for rapidly detecting trinitrotoluene, special yield, picric acid, dinitrotoluene and sulfur in explosives is characterized in that the solution changes from colorless transparent to paleo pink when the trinitrotoluene is detected, the solution changes from southwest purple when the special yield is detected, the solution changes from orange red when the picric acid is detected, the solution changes from gentian blue when the dinitrotoluene is detected, and the solution changes from moss green when the sulfur is detected.
The invention relates to a reagent for rapidly detecting trinitrotoluene, special droner, 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: (E) 2- (3-cyano-4- (4- (dimethylamino) styryl) -5, 5-dimethylfuran-2 (5H) -ylidene) malononitrile, designated as DMA-CN;
The prepared detection reagent is applied to colorimetric detection of trinitrotoluene (TNT), tredroner, picric Acid (PA), dinitrotoluene (DNT) and sulfur (S), and the specific method is as follows:
(1) 0.0227g of trinitrotoluene (TNT) was weighed and dissolved in 10mL of acetonitrile to prepare a trinitrotoluene (TNT) solution having a standard solution concentration of 10 mM; 0.0287g of the tertrefoil is weighed and dissolved in 10mL of acetonitrile to prepare a tertrefoil solution with the standard solution concentration of 10 mM; 0.0183g of Picric Acid (PA) was dissolved in 10mL of acetone to prepare a Picric Acid (PA) solution having a standard solution concentration of 8 mM; 0.1821g of Dinitrotoluene (DNT) was weighed and dissolved in 10mL of acetone to prepare a Dinitrotoluene (DNT) solution with a standard solution concentration of 0.1M; 1.6g of sulfur (S) is weighed and dissolved in 10mL of toluene to prepare a sulfur (S) solution with standard solution concentration of 5M;
(2) Testing the change of the absorbance of the reagent before and after adding trinitrotoluene (TNT), tedroner, picric Acid (PA), dinitrotoluene (DNT) and sulfur (S) by using an ultraviolet-visible spectrophotometer, and the change of the color;
(3) The volume of the detection reagent scanned by ultraviolet-visible absorption spectrum is 3mL, and the volumes of standard TNT, tedroner, PA, DNT and S solutions with different concentrations are respectively added to be 20 mu L.
The reagent for rapidly detecting trinitrotoluene (TNT), special-bend, picric acid, dinitrotoluene and sulfur in explosives is mainly used for detecting trinitrotoluene (TNT), special-bend, picric Acid (PA), dinitrotoluene (DNT) and sulfur (S) in non-standard explosives, solves the problem that the trinitrotoluene (TNT), special-bend, picric Acid (PA), dinitrotoluene (DNT) and sulfur (S) cannot be simultaneously distinguished by the current detection means, and has poor stability.
Compared with the prior art, the invention has the beneficial effects that:
1. the detection reagent can simultaneously realize the detection of trinitrotoluene (TNT), special droner, 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), tredrone, picric Acid (PA), dinitrotoluene (DNT) and sulfur (S);
3. the detection reagent provided by the invention has a rapid reaction, and can realize the identification of paratrinitrotoluene (TNT), tredrone, picric Acid (PA), dinitrotoluene (DNT) and sulfur (S) within 1S;
4. The detection reagent provided by the invention can be used for detecting trinitrotoluene (TNT), tredroner, picric Acid (PA), dinitrotoluene (DNT) and sulfur (S), and can be directly identified and detected by naked eyes without complex analysis equipment;
5. The detection reagent does not need to carry out any pretreatment on the object to be detected, and is simple to operate and convenient to popularize and apply.
Drawings
FIG. 1 is an ultraviolet-visible absorption spectrum of a reagent (solvent is N, N-Dimethylformamide (DMF), the mass ratio of NaBH 4 to DMA-CN is 10:1) before and after reaction with 10mM TNT, and an illustration is a photograph of color change before and after reaction of the reagent with TNT, taken by a camera;
FIG. 2 is an ultraviolet-visible absorption spectrum of the reagent of the present invention (solvent is dimethyl sulfoxide, mass ratio of KBH 4 to DMA-CN is 6:1) before and after reaction with 10mM of tertrendy, and an inset is a photograph of color change of the reagent before and after reaction taken by a camera;
FIG. 3 is an ultraviolet-visible absorption spectrum of the reagent of the present invention (solvent N, N-Dimethylformamide (DMF), naBH 4 to DMA-CN in a mass ratio of 14:1) before and after reaction with 8mM picric acid, and an inset is a photograph of the color change of the reagent before and after reaction taken with a camera.
FIG. 4 is an ultraviolet-visible absorption spectrum of the reagent of the present invention (the solvent is ethylene glycol anisole, the mass ratio of KBH 4 to DMA-CN is 20:1) before and after the reaction with 0.1M DNT, and the inset is a photograph of the color change of the reagent before and after the reaction taken by a camera;
FIG. 5 is an ultraviolet-visible absorption spectrum of the reagent of the present invention (solvent N, N-Dimethylformamide (DMF), naBH 4 to DMA-CN in a mass ratio of 5:1) before and after reaction with 5M sulfur, and an inset is a photograph of the 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 invention is not limited to these examples.
Example 1
A. At room temperature, 10mg of the organic probe (E) 2- (3-cyano-4- (4- (dimethylamino) styryl) -5, 5-dimethylfuran-2 (5H) -ylidene) malononitrile was dissolved in 50mL of N, N-dimethylformamide as a solvent to prepare a probe solution having a concentration of 0.2. Mu.g/. Mu.L;
b. and d, adding 100mg of sodium borohydride as a reducing agent into the probe solution obtained in the step a, and performing ultrasonic treatment for 5min to obtain a colorless detection reagent for rapidly detecting explosive trinitrotoluene, tredrone, picric acid, dinitrotoluene and sulfur.
3ML of detection reagent is measured and placed in a quartz cuvette, 20 mu L of prepared 10mM trinitrotoluene (TNT) standard solution is added, ultraviolet-visible absorption spectrum scanning is carried out by an ultraviolet-visible spectrophotometer, the spectrograms before and after trinitrotoluene (TNT) addition are shown in figure 1, obvious absorption peaks appear at 511nm after reaction by comparing the spectrograms before and after reaction, direct photographing is carried out on the reagent before and after reaction (shown in figure 1), and the reagent changes from colorless to paleo pink after reaction by comparing the reagent photos before and after reaction.
Example 2
A. At room temperature, 5mg of the organic probe (E) 2- (3-cyano-4- (4- (dimethylamino) styryl) -5, 5-dimethylfuran-2 (5H) -ylidene) malononitrile was dissolved in 500mL of dimethyl sulfoxide as a solvent to prepare a probe solution having a concentration of 0.01. Mu.g/. Mu.L;
b. And d, adding 30mg of potassium borohydride as a reducing agent into the probe solution obtained in the step a, and performing ultrasonic treatment for 10min to obtain a colorless reagent for rapidly detecting explosive trinitrotoluene, tredrone, picric acid, dinitrotoluene and sulfur.
3ML of detection reagent is measured in a quartz cuvette, 20 mu L of prepared 10mM special-bend standard solution is added, ultraviolet-visible spectrum scanning is carried out by an ultraviolet-visible spectrophotometer, the spectrograms before and after the special-bend addition are shown in figure 2, obvious absorption peaks appear at 520nm after the reaction by comparing the spectrograms before and after the reaction, the reagent before and after the reaction is directly photographed (shown in the inset of figure 2), and the reagent changes from colorless to southward purple after the reaction by comparing the reagent photos before and after the reaction.
Example 3
A. At room temperature, 5mg of the organic probe (E) 2- (3-cyano-4- (4- (dimethylamino) styryl) -5, 5-dimethylfuran-2 (5H) -ylidene) malononitrile was dissolved in 50mL of N, N-dimethylformamide as a solvent to prepare a probe solution having a concentration of 0.1. Mu.g/. Mu.L;
b. and d, adding 60mg of sodium borohydride as a reducing agent into the probe solution obtained in the step a, and performing ultrasonic treatment for 15min to obtain a colorless reagent for rapidly detecting explosive trinitrotoluene, tredrone, picric acid, dinitrotoluene and sulfur.
Measuring 3mL of detection reagent in a quartz cuvette, adding 20 mu L of prepared 8mM picric acid standard solution, performing ultraviolet-visible absorption spectrum scanning by an ultraviolet-visible spectrophotometer, wherein the spectrograms before and after picric acid addition are shown in figure 3, comparing the spectrograms before and after reaction to show that two obvious absorption peaks appear at 420nm and 517nm after reaction, directly photographing the reagent before and after reaction (shown in the inset of figure 3), and comparing the reagent photos before and after reaction to show that the reagent changes from colorless to orange.
Example 4
A. At room temperature, 10mg of the organic probe (E) 2- (3-cyano-4- (4- (dimethylamino) styryl) -5, 5-dimethylfuran-2 (5H) -ylidene) malononitrile was dissolved in 20mL of ethylene glycol anisole as a solvent to prepare a probe solution having a concentration of 2. Mu.g/. Mu.L;
b. And d, adding 200mg of 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 tredrone, the picric acid, the dinitrotoluene and the sulfur.
3ML of the detection reagent was measured in a quartz cuvette, and 20. Mu.L of the prepared 0.1M Dinitrotoluene (DNT) standard solution was added. The ultraviolet-visible absorption spectrum scanning is carried out by an ultraviolet-visible spectrophotometer, the spectrograms before and after Dinitrotoluene (DNT) is added are shown in figure 4, and obvious absorption peaks appear at 592nm after the reaction by comparing the spectrograms before and after the reaction. The reagents before and after the reaction were photographed directly (as shown in the inset of fig. 4), and the photographs of the reagents before and after the reaction were compared to see that the reagents changed from colorless to gentian blue.
Example 5
A. 100mg of 2- (3-cyano-4- (4- (dimethylamino) styryl) -5, 5-dimethylfuran-2 (5H) -ylidene) malononitrile as an organic probe (E) was dissolved in 20mL of N, N-dimethylformamide as a solvent at room temperature to prepare a probe solution having a concentration of 5. Mu.g/. Mu.L;
b. And d, adding 500mg of sodium borohydride as a reducing agent into the probe solution obtained in the step a, and performing ultrasonic treatment for 20min to obtain a reagent for rapidly detecting explosive trinitrotoluene, tredrone, 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 the spectrograms before and after sulfur addition are shown in figure 5, comparing the spectrograms before and after reaction to show that obvious absorption peaks appear at 619nm after reaction, directly photographing the reagent before and after reaction (shown in the inset of figure 5), and comparing the reagent photos before and after reaction to show that the reagent turns from colorless to moss green.
The above embodiments describe the present invention, it being understood that the present reagent is equally applicable to TNT, DNT, trending, picric acid, S assays in other fields without departing from the spirit of the present invention. The ratio of the reagent components in the present invention can be varied, and these variations are also within the scope of the present invention.
Claims (1)
1. A reagent for rapidly detecting trinitrotoluene, tredrone, picric acid, dinitrotoluene and sulfur in explosives is characterized by being 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) -subunit) malononitrile in N, N-dimethylformamide, dimethyl sulfoxide or ethylene glycol anisole as a solvent to prepare a probe solution with the concentration of 0.01-5 mug/mug;
b. adding a reducing agent which is sodium borohydride or 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 5-20 min to obtain a reagent for rapidly detecting explosive trinitrotoluene, terdrone, picric acid, dinitrotoluene and sulfur; the reagent for rapidly detecting trinitrotoluene, special yield, picric acid, dinitrotoluene and sulfur in explosives is characterized in that the solution changes from colorless transparent to paleo pink when trinitrotoluene is detected, the solution changes from ston purple when special yield is detected, the solution changes from orange red when picric acid is detected, the solution changes from gentian blue when dinitrotoluene is detected, and the solution changes from moss green when sulfur is detected.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210166281.2A CN114527084B (en) | 2022-02-23 | 2022-02-23 | Reagent for rapidly detecting trinitrotoluene, tredrone, picric acid, dinitrotoluene and sulfur in explosive |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210166281.2A CN114527084B (en) | 2022-02-23 | 2022-02-23 | Reagent for rapidly detecting trinitrotoluene, tredrone, picric acid, dinitrotoluene and sulfur in explosive |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114527084A CN114527084A (en) | 2022-05-24 |
| CN114527084B true CN114527084B (en) | 2024-07-19 |
Family
ID=81625364
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210166281.2A Active CN114527084B (en) | 2022-02-23 | 2022-02-23 | Reagent for rapidly detecting trinitrotoluene, tredrone, picric acid, dinitrotoluene and sulfur in explosive |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114527084B (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110873713A (en) * | 2019-11-28 | 2020-03-10 | 中国科学院新疆理化技术研究所 | Method for rapidly detecting sulfur, dinitrotoluene, trinitrotoluene and potassium permanganate in explosive |
| CN111220606A (en) * | 2020-01-15 | 2020-06-02 | 中国科学院新疆理化技术研究所 | Preparation method and application of layered Steiner network structure fiber membrane |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016020939A1 (en) * | 2014-08-06 | 2016-02-11 | Council Of Scientific & Industrial Research | Para-aminobenzoic acid sensitized terbium doped laf3 nanoparticles for detection of explosive nitro compounds |
| CN111595840B (en) * | 2020-05-20 | 2022-07-05 | 中国科学院新疆理化技术研究所 | Preparation method and application of reagent permeation prevention paper-based array |
-
2022
- 2022-02-23 CN CN202210166281.2A patent/CN114527084B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110873713A (en) * | 2019-11-28 | 2020-03-10 | 中国科学院新疆理化技术研究所 | Method for rapidly detecting sulfur, dinitrotoluene, trinitrotoluene and potassium permanganate in explosive |
| CN111220606A (en) * | 2020-01-15 | 2020-06-02 | 中国科学院新疆理化技术研究所 | Preparation method and application of layered Steiner network structure fiber membrane |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114527084A (en) | 2022-05-24 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Nagarkar et al. | A fluorescent metal–organic framework for highly selective detection of nitro explosives in the aqueous phase | |
| US8377713B2 (en) | Detection of explosives through luminescence | |
| Taudte et al. | A portable explosive detector based on fluorescence quenching of pyrene deposited on coloured wax-printed μPADs | |
| Shahvar et al. | A portable smartphone-based colorimetric sensor for rapid determination of water content in ethanol | |
| Erçağ et al. | Selective spectrophotometric determination of TNT using a dicyclohexylamine-based colorimetric sensor | |
| CN102128908B (en) | On-site quick detection method for organic pollutants in water | |
| Pamula et al. | A droplet-based lab-on-a-chip for colorimetric detection of nitroaromatic explosives | |
| Aksuner | Development of a new fluorescent sensor based on a triazolo-thiadiazin derivative immobilized in polyvinyl chloride membrane for sensitive detection of lead (II) ions | |
| Erçağ et al. | Rapid detection of nitroaromatic and nitramine explosives on chromatographic paper and their reflectometric sensing on PVC tablets | |
| Zhang et al. | High-performance fluorescent and colorimetric dual-mode nitrite sensor boosted by a versatile coumarin probe equipped with diazotization-coupling reaction-sites | |
| WO2013165625A2 (en) | Explosives detection polymer comprising functionalized polyamine polymers and methods of using the same | |
| Ensafi et al. | Highly selective optical-sensing film for lead (II) determination in water samples | |
| Gowri et al. | Anthracene based AIEgen for picric acid detection in real water samples | |
| CN114527084B (en) | Reagent for rapidly detecting trinitrotoluene, tredrone, picric acid, dinitrotoluene and sulfur in explosive | |
| CN116217948B (en) | Luminescent metal organic frame material and preparation method and application thereof | |
| CN104251827A (en) | Method for determining concentration of mercury ions or silver ions in solution | |
| CN107402206B (en) | Mercury ion colorimetric sensor and preparation method and application thereof | |
| Şen et al. | A simple determination of trinitrotoluene (TNT) based on fluorescence quenching of rhodamine 110 with FRET mechanism | |
| CN110873713B (en) | Method for rapidly detecting sulfur, dinitrotoluene, trinitrotoluene and potassium permanganate in explosive | |
| CN113024468B (en) | Fluorescent molecular probe for detecting picric acid and preparation method and application thereof | |
| Jiao et al. | Conjugated carbazole dimer as fluorescence carrier for preparation of iodine-sensitive chemical sensor | |
| CN111208096B (en) | Method for detecting picric acid by using fluorescent sensor based on BODIPY derivative | |
| Ghobadi Seresht et al. | Determination of 2, 4, 6-Trinitrotoluene in Soil Samples Using a Paired Emitter-Detector Diode-Based Photometer | |
| Yang et al. | A selective PVC membrane for di-or trinitrophenol based on N, N-dibenzyl-3, 3′, 5, 5′-tetramethylbenzidine | |
| CN112964705B (en) | Reagent for detecting ethylenediamine by using dual modes of rapid colorimetric and fluorescent lighting |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |