CN110749592A - One-step rapid colorimetric detection method for peroxide explosives - Google Patents
One-step rapid colorimetric detection method for peroxide explosives Download PDFInfo
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- CN110749592A CN110749592A CN201911026553.3A CN201911026553A CN110749592A CN 110749592 A CN110749592 A CN 110749592A CN 201911026553 A CN201911026553 A CN 201911026553A CN 110749592 A CN110749592 A CN 110749592A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/22—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators
- G01N31/228—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators for peroxides
Abstract
The invention discloses a one-step rapid colorimetric detection method of peroxide explosives, wherein a detection reagent is prepared from a mixed solution of titanium salt, an organic solvent, 36-98% acid and distilled water at room temperature, during detection, a sample is extracted from an explosive suspicious source, the sample is placed on filter paper, the detection reagent is directly dripped onto a suspicious sample extracted from the filter paper, color change is observed, and if the peroxide explosives are contained, the suspicious sample on the filter paper is changed from colorless to orange within 5 seconds. The method realizes the rapid detection of peroxide explosives in field search and explosion cases, has the characteristics of simple operation, sensitive reaction, convenient use and low cost, and can provide an effective technical means for the detection of explosion cases in public security system criminal investigation departments.
Description
Technical Field
The invention belongs to the technical field of explosive detection, and particularly relates to a one-step rapid colorimetric detection method for peroxide explosives.
Background
Peroxide explosives have the characteristics of great explosive power, simple synthesis steps, easily available raw materials, difficult detection of a conventional detector and the like, and become the first choice of terrorists. Peroxide explosives generally include: triacetoneperoxide (TATP), cyclohexyltriperoxydiamine (HMTD), diproponeperoxide (DADP), and Tetramethylenediperoxycarboxamide (TMDD). Common peroxide explosives detection methods include: electrochemical methods, indirect fluorescence methods, mass spectrometry, ion mobility spectrometry and the like, and products or equipment for rapidly detecting peroxide explosives are developed at present.
The invention patent, Kadun Luoyang Intelligent science and technology Limited, a TATP detection device, patent number 201610526682.9 provides a TATP qualitative detection device, which uses a laser controller to control a laser to alternately emit laser light with a first wavelength capable of being absorbed by the TATP and laser light with a second wavelength incapable of being absorbed by the TATP at a preset frequency, then, a part of laser light of the first wavelength laser or the second wavelength laser is split into a first photoelectric detector through a light splitting plate to output a reference signal, the other part of laser light is split into a collimator of a laser to be collimated and then emitted, the collimated light beam passes through a TATP detection area and then irradiates to the target, the reflected light is reflected to the auxiliary mirror by the primary mirror in the telescope after being reflected by the target, and then is converged to the second photoelectric detector through the auxiliary mirror to output a detectivity signal, the presence or absence of TATP can be detected by the difference in the detected signals on the first wavelength laser and the second wavelength laser.
The invention relates to a method for rapidly and sensitively detecting peroxide explosive HMTD, which is designed by the application (201410587879.4) of reagent molecules in the ion mobility spectrometry detection of the peroxide explosive HMTD, and belongs to the institute of chemical and physical, which is connected with the academy of Chinese sciences. An ion mobility spectrometry technology with a vacuum ultraviolet lamp (VUV lamp) as an ionization source is used as a basic detection technology, and a method for detecting HMTD is established by adding reagent molecules into carrier gas in a positive ion mode. The reagent molecules are added, and new reagent ions are generated by ionization of the VUV lamp in an ion mobility spectrometry positive ion mode, so that the selectivity and the sensitivity of HMTD detection are improved.
The invention patent, Beijing university of Physician technology, preparation method and detection method (201210004174.6) of the hydrogen peroxide compound provide a detection method for qualitatively detecting TATP by adopting the chemochromic law, under the acidic condition, the concentrated potassium permanganate solution is directly titrated into the liquid sample containing a trace of hydrogen peroxide compound, the potassium permanganate solution fades, which indicates that the hydrogen peroxide possibly exists in the sample. In order to further confirm whether the TATP exists, a reduction method is adopted again, namely a detected liquid sample is taken, excessive potassium iodide is added in a dilute sulfuric acid acidic environment, if the colorless transparent bottle does not develop color, the sample to be detected does not contain the TATP, and if the color development is yellow, the sample contains the TATP.
The methods either need complicated instruments or meters, or have long detection time, or have high detection cost and complex operation, and in order to solve the defects of the prior art, the invention provides a one-step rapid colorimetric detection reagent and a detection method for peroxide explosives, which have simple operation and sensitive reaction.
Disclosure of Invention
The invention aims to provide a one-step rapid colorimetric detection method for peroxide explosives, wherein a detection reagent involved in the method is prepared from a mixed solution of titanium salt, an organic solvent, 36-98% by mass of acid and distilled water at room temperature, in the detection process, a sample is extracted from an explosive suspicious source, the sample is placed on filter paper, the detection reagent is directly dripped onto a suspicious sample extracted from the filter paper, the color change is observed, and if the peroxide explosives are contained, the suspicious sample on the filter paper is changed from colorless to orange within 5 seconds. The method realizes the rapid detection of peroxide explosives in field search and explosion cases, has the characteristics of simple operation, sensitive reaction, convenient use and low cost, and can provide an effective technical means for the detection of explosion cases in public security system criminal investigation departments.
The one-step rapid colorimetric detection method for peroxide explosives, disclosed by the invention, is carried out according to the following steps:
preparing a detection reagent:
a. adding titanium salt such as titanium trichloride, titanium tetrachloride, titanium sulfate, titanyl sulfate, titanic acid or titanium potassium oxalate into a container for preparing a detection reagent at room temperature, adding distilled water, stirring until the solid is completely dissolved, sequentially adding one or three of methanol, ethanol, isopropanol, dimethyl sulfoxide, acetonitrile and acetone and acid hydrochloric acid, nitric acid or sulfuric acid with the mass fraction of 36-98% into the container for containing the detection reagent, continuously stirring, and cooling to room temperature to obtain the detection reagent;
the detection method comprises the following steps:
b. using a medicine spoon to extract a sample from an explosive suspicious source, placing the sample on a filter paper, directly dripping the detection reagent obtained in the step a onto the suspicious sample extracted from the filter paper, observing the color change, and if the suspicious sample contains peroxide explosives, changing the color of the suspicious sample on the filter paper from colorless to orange within 5 seconds.
The peroxide explosive is triacetoneperoxide, cyclohexane-triperoxydiamine, dipropionylperoxide or tetramethylene-diperoxyamide.
Compared with the prior art, the invention has the advantages that:
(1) the invention has simple operation and convenient use, and realizes the real one-step detection of the peroxide explosives. The traditional colorimetric detection of peroxide explosives requires two steps: the first step needs to pretreat a sample suspected of containing peroxide explosives to generate hydrogen peroxide, the second step utilizes the redox performance of the hydrogen peroxide to realize a color reaction, and the two steps of reactions are usually carried out separately, so that the operation is complex and the field use is not facilitated. The invention integrates the decomposition reaction and the color reaction, thereby realizing the one-step detection of the peroxide explosives.
(2) The invention has short detection time and visual and accurate result through colorimetric analysis.
Drawings
FIG. 1 is a color photograph of a detection reagent of the present invention added with TATP solutions of different concentrations;
FIG. 2 is a diagram of the UV absorption spectrum of TATP added to a detection reagent according to the present invention, wherein the solid line is the detection reagent and the dotted line is TATP + detection reagent.
Detailed Description
The following description is only exemplary of the present invention and should not be construed as limiting the present invention.
Example 1
Preparing a detection reagent:
a. at room temperature, adding 0.001g of titanium trichloride into a container for preparing a detection reagent, adding 5g of distilled water, stirring until the titanium trichloride is completely dissolved, sequentially adding 10mL of a mixed solvent of methanol, isopropanol and acetone in a volume ratio of 1:1:1 and 0.02mL of hydrochloric acid with a mass fraction of 36% into the container for containing the detection reagent, continuously stirring, and cooling to room temperature to obtain the detection reagent;
the detection method comprises the following steps:
b. and (b) using a medicine spoon, extracting a 0.5mg tripipropylone peroxide (TATP) sample, placing the sample on a filter paper, directly dripping the detection reagent obtained in the step a onto the tripipropylone peroxide (TATP) sample extracted on the filter paper, observing the color change, changing the color of the sample from colorless to orange within 5 seconds, and determining that the sample contains the peroxide explosive.
Example 2
Preparing a detection reagent:
a. at room temperature, adding 1g of titanium tetrachloride into a container for preparing a detection reagent, adding 5g of distilled water, stirring until the titanium tetrachloride is completely dissolved, sequentially adding 10mL of methanol and 5mL of hydrochloric acid with the mass fraction of 36% into the container containing the titanium tetrachloride, continuously stirring, and cooling to room temperature to obtain the detection reagent;
the detection method comprises the following steps:
b. and (c) extracting a 0.5mg sample of the cyclohexanediamine triperoxyide (HMTD) by using a medicine spoon, placing the sample on a filter paper, directly dripping the detection reagent obtained in the step a onto the sample of the cyclohexanediamine triperoxyide (HMTD) extracted from the filter paper, observing the color change, changing the color of the sample from colorless to orange within 5 seconds, and determining that the sample contains the peroxide explosives.
Example 3
Preparing a detection reagent:
a. at room temperature, adding 0.001g of titanium potassium oxalate into a container for preparing a detection reagent, adding 5g of distilled water, stirring until the titanium oxalate is completely dissolved, sequentially adding 10mL of ethanol and 10mL of nitric acid with the mass fraction of 69% into the container containing the titanium oxalate, continuously stirring, and cooling to room temperature to obtain the detection reagent;
the detection method comprises the following steps:
b. and (b) extracting a 0.2mg diproprione diperoxide (DADP) sample by using a medicine spoon, placing the sample on a filter paper, directly dripping the detection reagent obtained in the step (a) onto the diproprione diperoxide (DADP) sample extracted on the filter paper, observing the color change, and determining that the sample is changed from colorless to orange within 5 seconds to determine that the sample contains the peroxide explosives.
Example 4
Preparing a detection reagent:
a. at room temperature, adding 0.5g of titanic acid into a container for preparing a detection reagent, adding 5g of distilled water, stirring until the titanic acid is completely dissolved, sequentially adding 10mL of isopropanol and 5mL of nitric acid with the mass fraction of 69% into the container containing the titanic acid, continuously stirring, and cooling to room temperature to obtain the detection reagent;
the detection method comprises the following steps:
b. using a medicine spoon, extracting a 0.2mg sample of tetramethylene-bis-peroxycarbnamide (TMDD) and placing the sample on a filter paper, directly dripping the detection reagent obtained in the step a on the TMDD sample extracted on the filter paper, observing the color change, changing the color of the sample from colorless to orange within 5 seconds, and determining that the sample contains the peroxide explosives.
Example 5
Preparing a detection reagent:
a. at room temperature, adding 0.7g of titanyl sulfate into a container for preparing a detection reagent, adding 5g of distilled water, stirring until the titanyl sulfate is completely dissolved, sequentially adding 35mL of dimethyl sulfoxide and 5mL of sulfuric acid with the mass fraction of 98% into the container containing the titanyl sulfate, continuously stirring, and cooling to room temperature to obtain the detection reagent;
b. the detection method comprises the following steps: and (b) using a medicine spoon, extracting a 0.1mg tripipropylone peroxide (TATP) sample, placing the sample on a filter paper, directly dripping the detection reagent obtained in the step a onto the tripipropylone peroxide (TATP) sample extracted on the filter paper, observing the color change, changing the color of the sample from colorless to orange within 5 seconds, and determining that the sample contains the peroxide explosive.
Example 6
Preparing a detection reagent:
a. at room temperature, adding 0.7g of titanyl sulfate into a container for preparing a detection reagent, adding 5g of distilled water, stirring until the titanyl sulfate is completely dissolved, sequentially adding 35mL of acetonitrile and 5mL of sulfuric acid with the mass fraction of 98% into the container containing the titanyl sulfate, continuously stirring, and cooling to room temperature to obtain the detection reagent;
the detection method comprises the following steps:
b. using a medicine spoon, extracting 0.1mg of tripropionone peroxide (TATP) and 0.1mg of cyclohexane tripropanediamine peroxide (HMTD) samples and placing the samples on a filter paper, directly dripping the detection reagent obtained in the step a onto the tripropionone peroxide (TATP) and cyclohexane tripropanediamine peroxide (HMTD) samples extracted on the filter paper, observing the color change, changing the color of the samples from colorless to orange within 5 seconds, and determining that the samples contain peroxide explosives.
Example 7
Preparing a detection reagent:
a. at room temperature, adding 0.7g of titanium potassium oxalate into a container for preparing a detection reagent, adding 5g of distilled water, stirring until the titanium potassium oxalate is completely dissolved, sequentially adding 35mL of acetone and 5mL of sulfuric acid with the mass fraction of 98% into the container containing the titanium potassium oxalate, continuously stirring, and cooling to room temperature to obtain the detection reagent;
the detection method comprises the following steps:
b. using a medicine spoon, extracting 0.1m triproperoxytriacetone (TATP) and 0.1mg cyclohexane triperoxydiamine (HMTD) samples and placing the samples on filter paper, directly dripping the detection reagent obtained in the step a onto the triproperoxytriacetone (TATP) and cyclohexane triperoxydiamine (HMTD) samples extracted from the filter paper, observing the color change, changing the color of the samples from colorless to orange within 5 seconds, and determining that the samples contain peroxide explosives.
Example 8 (control)
a. At room temperature, adding 1g of titanium sulfate into a container for preparing a detection reagent, adding 5g of distilled water, stirring until the titanium sulfate is completely dissolved, sequentially adding 35mL of a mixed solvent of ethanol and acetone with a volume ratio of 3:1 and 5mL of nitric acid with a mass fraction of 69% into the container containing the titanium sulfate, continuously stirring, and cooling to room temperature to obtain the detection reagent;
b. 0.2mg of easy-explosion raw material potassium perchlorate is extracted by using a medicine spoon, a sample is placed on a filter paper, and a detection reagent is directly dripped on the filter paper containing the sample, so that the sample does not have any color change, and the sample does not contain peroxide explosives.
The one-step rapid colorimetric detection method for peroxide explosives can rapidly and accurately detect the peroxide explosives, saves cost and improves detection efficiency and accuracy.
Claims (2)
1. A one-step rapid colorimetric detection method for peroxide explosives is characterized by comprising the following steps:
preparing a detection reagent:
a. adding titanium salt such as titanium trichloride, titanium tetrachloride, titanium sulfate, titanyl sulfate, titanic acid or titanium potassium oxalate into a container for preparing a detection reagent at room temperature, adding distilled water, stirring until the solid is completely dissolved, sequentially adding one or three of methanol, ethanol, isopropanol, dimethyl sulfoxide, acetonitrile and acetone and acid hydrochloric acid, nitric acid or sulfuric acid with the mass fraction of 36-98% into the container for containing the detection reagent, continuously stirring, and cooling to room temperature to obtain the detection reagent;
the detection method comprises the following steps:
b. using a medicine spoon to extract a sample from an explosive suspicious source, placing the sample on a filter paper, directly dripping the detection reagent obtained in the step a onto the suspicious sample extracted from the filter paper, observing the color change, and if the suspicious sample contains peroxide explosives, changing the color of the suspicious sample on the filter paper from colorless to orange within 5 seconds.
2. The method for the one-step rapid colorimetric detection of peroxide explosives in accordance with claim 1, wherein the peroxide explosives are triproperoxytriacetone, cyclohexyltriperoxydiamine, dipropionylperoxydiacetone or tetramethylene-diperoxycarbonylamine.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112964686A (en) * | 2021-02-07 | 2021-06-15 | 中国科学院新疆理化技术研究所 | Peroxide fluorescence colorimetric dual-mode detection method based on carbon dot fluorescence internal filtering effect |
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| US4908323A (en) * | 1983-03-05 | 1990-03-13 | Merck Patent Gesellschaft Mit Beschrankter Haftung | Method for the determination of organic peroxides in organic solutions |
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| EP2646794A1 (en) * | 2010-11-29 | 2013-10-09 | Commissariat à l'Énergie Atomique et aux Énergies Alternatives | Method for detecting in situ the presence of explosives in a gaseous medium |
| CN103472054A (en) * | 2013-09-18 | 2013-12-25 | 杭州天迈生物科技有限公司 | Quick detection effervescent tablet for hydrogen peroxide residues in food |
| CN205720000U (en) * | 2016-06-21 | 2016-11-23 | 上海瑞鑫科技仪器有限公司 | Hydrogen peroxide Test paper in food |
| CN109115759A (en) * | 2018-08-23 | 2019-01-01 | 智锐达仪器科技南通有限公司 | Hydrogen peroxide quick detection reagent, kit and detection method in a kind of food |
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2019
- 2019-10-26 CN CN201911026553.3A patent/CN110749592A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4908323A (en) * | 1983-03-05 | 1990-03-13 | Merck Patent Gesellschaft Mit Beschrankter Haftung | Method for the determination of organic peroxides in organic solutions |
| CN102612649A (en) * | 2009-11-20 | 2012-07-25 | 犹他大学研究基金会 | Sensors and methods for detecting peroxide based explosives |
| EP2646794A1 (en) * | 2010-11-29 | 2013-10-09 | Commissariat à l'Énergie Atomique et aux Énergies Alternatives | Method for detecting in situ the presence of explosives in a gaseous medium |
| CN103472054A (en) * | 2013-09-18 | 2013-12-25 | 杭州天迈生物科技有限公司 | Quick detection effervescent tablet for hydrogen peroxide residues in food |
| CN205720000U (en) * | 2016-06-21 | 2016-11-23 | 上海瑞鑫科技仪器有限公司 | Hydrogen peroxide Test paper in food |
| CN109115759A (en) * | 2018-08-23 | 2019-01-01 | 智锐达仪器科技南通有限公司 | Hydrogen peroxide quick detection reagent, kit and detection method in a kind of food |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112964686A (en) * | 2021-02-07 | 2021-06-15 | 中国科学院新疆理化技术研究所 | Peroxide fluorescence colorimetric dual-mode detection method based on carbon dot fluorescence internal filtering effect |
| CN112964686B (en) * | 2021-02-07 | 2022-05-10 | 中国科学院新疆理化技术研究所 | Peroxide fluorescence colorimetric dual-mode detection method based on carbon dot fluorescence internal filtering effect |
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