阅读说明：本技术 一种过氧化物类***物的一步式快速比色检测方法 (One-step rapid colorimetric detection method for peroxide explosives ) 是由 李毓姝 曹洄鱼 窦新存 于 2019-10-26 设计创作，主要内容包括：本发明公开了一种过氧化物类爆炸物的一步式快速比色检测方法,该方法中所涉及的检测试剂是在室温下由钛盐、有机溶剂、质量分数为36%-98%的酸与蒸馏水的混合溶液配制而成,在检测中,从爆炸物可疑源中提取样品,将样品置于滤纸上,将检测试剂直接滴加到滤纸上提取的可疑物样品上,观察颜色变化,若含有过氧化物类爆炸物,滤纸上的可疑物样品会在5秒内由无色变为橘黄色。实现了现场搜爆及爆炸案中对过氧化物类爆炸物的快速检测,具有操作简单,反应灵敏,使用方便,成本低的特点,可为公安系统刑侦部门爆炸案的侦破提供有效技术手段。(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.)

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.

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.