阅读说明：本技术 一种快速检测***物中硫磺、二硝基甲苯、***和高锰酸钾的方法 (Method for rapidly detecting sulfur, dinitrotoluene, trinitrotoluene and potassium permanganate in explosive ) 是由 祖佰祎 刘勇 窦新存 于 2019-11-28 设计创作，主要内容包括：本发明涉及一种快速检测爆炸物中硫磺、二硝基甲苯、三硝基甲苯和高锰酸钾的方法,该方法基于化学比色法,由强碱、醇、二甲基亚砜、尿素、甲苯、吐温-20、吐温-40、吐温-60、吐温-80或TX-100混合溶液配制检测试剂,将试剂直接滴加到待测物上,根据变化后的颜色确定硫磺、二硝基甲苯、三硝基甲苯和高锰酸钾的存在。本发明所述的方法可用于爆炸案件和搜爆排爆现场中的爆炸物及其残留物中硫磺、二硝基甲苯、三硝基甲苯和高锰酸钾的快速定性检测。具有操作简单,现场快速准确,容易识别,灵敏度高,检测限低,可为安全部门现场检测分析爆炸物及其残留物提供有效的技术手段。(The invention relates to a method for rapidly detecting sulfur, dinitrotoluene, trinitrotoluene and potassium permanganate in explosives, which is based on a chemical colorimetric method, and comprises the steps of preparing a detection reagent by using a mixed solution of strong base, alcohol, dimethyl sulfoxide, urea, toluene, Tween-20, Tween-40, Tween-60, Tween-80 or TX-100, directly dripping the reagent on an object to be detected, and determining the existence of the sulfur, the dinitrotoluene, the trinitrotoluene and the potassium permanganate according to the changed color. The method can be used for the rapid qualitative detection of the sulfur, the dinitrotoluene, the trinitrotoluene and the potassium permanganate in the explosive and the residues thereof in the explosive cases, the explosive searching and removing sites. The method has the advantages of simple operation, fast and accurate field, easy identification, high sensitivity and low detection limit, and can provide an effective technical means for the field detection and analysis of explosives and residues thereof for safety departments.)

1. A method for rapidly detecting sulfur, dinitrotoluene, trinitrotoluene and potassium permanganate in explosives is characterized by comprising the following steps:

preparing a colorimetric reagent:

a. mixing 6.6-60% by volume of methanol, ethanol, isopropanol, n-butanol or tert-butanol with 15.6-41.4% by volume of dimethyl sulfoxide, 6.6-20% by volume of 600g/L urea aqueous solution, 8-20% by volume of toluene, 9.8-12% by volume of tween-20, tween-40, tween-60, tween-80 or TX-100, and stirring uniformly to obtain a mixed solvent;

b. b, adding potassium hydroxide, sodium hydroxide or quaternary ammonium hydroxide with the concentration of 20-100g/L into the mixed solvent obtained in the step a, uniformly stirring to obtain a colorimetric reagent for detecting sulfur, dinitrotoluene, trinitrotoluene and potassium permanganate in the explosive, filling the colorimetric reagent into a reagent bottle, and sealing and storing;

and (3) rapid detection:

c. b, extracting a sample from the explosive suspicious source by using a key slot or a sampling swab, then dropwise adding the colorimetric reagent obtained in the step b, and if the suspicious substance contains sulfur, showing a dark green color; if the suspicious substance contains dinitrotoluene, the suspicious substance presents dark blue; if the suspicious substance contains trinitrotoluene, the suspicious substance is reddish brown; if the suspicious substance contains potassium permanganate, the suspicious substance is green.

Technical Field

The invention relates to a method for rapidly detecting sulfur, dinitrotoluene, trinitrotoluene and potassium permanganate in explosives.

Background

The use of sulfur in China has a long history, and the invention of the gunpowder by our ancestors is as early as more than a thousand years ago. Because the sulfur is widely applied to the production life, including sulfur ores, craters, oil wells, brick kilns, sulfur soap or paste, traditional Chinese medicinal materials and match heads, the sulfur has the characteristics of active chemical property, flammability and large-amount gas generation. Dinitrotoluene and trinitrotoluene are one of the most common and widely used nitroaromatic explosives, have the characteristics of unstable chemical structure, explosion velocity, strong heat release capacity, toxicity and the like, are often used as main components of a plurality of known chemical explosives, but the saturated vapor pressure of the nitroaromatic explosives at room temperature is relatively low, so that great difficulty is caused in detection. Potassium permanganate, strong oxidant, mauve crystal, and is easily soluble in water, methanol, and acetone. Because of its strong oxidizing property, it is mixed with organic substances or inflammable substances such as cane sugar, glycol and glycerine, and can be easily produced strong combustion or explosion, and when it meets reducing agent, it can be extensively used in production and life, and can be mixed with cotton or aluminium powder, and can be used for illegal activity by extreme molecules. At present, researchers and their safety departments develop a lot of methods for detecting sulfur, dinitrotoluene, trinitrotoluene and potassium permanganate, and the laboratory is mainly used for detecting sulfur: thin layer chromatography (J.Chrokaeog,1968,35, 513-; the method for detecting dinitrotoluene and trinitrotoluene comprises the following steps: the X-ray imaging technology and the neutron technology or nuclear technology, the gas chromatography-mass spectrometer and the like are used for detecting the potassium permanganate: flow injection catalysis photometry (Microchemical Jouranl.1995,52,77-80), ultra-fiber optic sensors (Applied optics.2017,56, 224-. The method for detecting sulfur, dinitrotoluene, trinitrotoluene and potassium permanganate in explosives and explosive residues by a security department mainly comprises the following steps: the infrared spectrometer, the gas chromatograph, the ion mobility spectrometer and other large-scale instruments and equipment mostly have the problems of high price, complex operation, long detection time, high detection limit and the like, and cannot meet the requirement of rapid and accurate detection of explosive sites.

At present, sulfur, dinitrotoluene, trinitrotoluene and potassium permanganate detection products or equipment are developed in many fields, and the fields of chemical industry, environment, traditional Chinese medicine and the like are involved. The detection method or equipment of the sulfur comprises the following steps: the institute of chemical and physical research of the Chinese academy of sciences, a method for analyzing ion mobility spectrometry (201310039444.1), provides a method for detecting sulfur, and an ion consumption area is arranged between an ionization reaction area and a migration area of an ion migration tube. The ion consumption zone contains a specific organic reagent, so that not only can interference ions be selectively eliminated and the separation degree of target ions be improved, but also the influence on an ionization reaction zone and a migration zone is avoided. The 'device for rapidly detecting the sulfur component in the solid material' (201320268946.7) provides a device for rapidly detecting the sulfur component in the solid material, which irradiates a test sample with X-rays to obtain a mixed energy spectrum of characteristic X-rays and backscattered X-rays, and calculates the content of the sulfur component in the test sample by using the intensities of the characteristic X-rays of the sulfur element and the backscattered X-rays in the mixed energy spectrum. "a sulphur content detection equipment" (201410581965.4), provides an automatic sulphur content detection equipment, adds the sample to be detected into the tube furnace for high temperature heating, the gas produced enters the starch solution preset in the detection bottle through the air inlet device, the light detection device detects the color change of the starch solution, the control device controls the burette of the second liquid inlet device to titrate into the detection bottle according to the detection signal of the light detection device, when the detection signal returns to the initial starting point, the control device controls the second control valve to close, the titration is finished, the total sulphur content of the sample can be obtained through the consumed starch solution and the iodine potassium solution. Jiaxing Bei chemical polymer additive Co., Ltd, "a method for detecting sulfur masterbatch" (201510190365.X), provides a method for detecting sulfur masterbatch, which adopts a way of rolling and slicing masterbatch raw materials by an open mill to detect the dispersion uniformity of sulfur masterbatch particles. The detection device or method of dinitrotoluene and trinitrotoluene comprises the following steps: the invention discloses a functional monomer and a preparation method thereof, a fluorescent imprinted membrane and a preparation method thereof (201410624188.7) by the institute of chemical materials of China institute of engineering and physics, and develops the preparation of a fluorescent imprinted membrane material with a sensing function on dinitrotoluene and trinitrotoluene in an aqueous solution, the functional monomer for preparing the fluorescent imprinted membrane material and the preparation thereof. The Xinjiang physicochemical technology research institute of Chinese academy of sciences, "a preparation method and application of a Schottky junction explosive atmosphere sensing material" (201610344261.4), and improves the preparation method and application of the Schottky junction explosive atmosphere sensing material. Jilin university, "aggregation-induced emission organic fluorescent small molecule material and its application" (201810809888.1), provides an aggregation-induced emission organic fluorescent small molecule material and its application in the fluorescence detection of dinitrotoluene and trinitrotoluene gas. The invention relates to an AIE type fluorescent sensing material which takes 3,4, 5-triphenyl-4H-1, 2, 4-triazole as a structural center and is connected with tetraphenyl ethylene, triphenylamine or carbazole. Such materials exhibit weak fluorescence in dilute solutions, but exhibit strong fluorescence during aggregation or in the solid state. The tetraphenyl ethylene is used as a core construction unit of the fluorescent molecule, so that the material has AIE characteristics, meanwhile, a freely rotatable benzene ring of the tetraphenyl ethylene has a promotion effect on constructing a film with a porous structure, the formed film with a multi-cavity structure can form pi-pi accumulation with NACS explosives, and the fluorescent material is guaranteed to have extremely high selectivity and sensitivity and quick response to the detection of dinitrotoluene and trinitrotoluene. The detection of potassium permanganate mainly comprises the following steps: the invention provides a novel potassium permanganate solution concentration detection instrument (201310034926.8), which utilizes the fact that potassium permanganate solutions with different concentrations have different absorbances under a certain specific wavelength, and the light absorption and the concentration of the potassium permanganate solution form a linear relationship to realize the detection of the concentration of the potassium permanganate solution. Guangxi academy of academic, Guangxi, "a utilizes fluorescence quenching of graphene quantum dot to detect permanganate" (201410530777.9), provides a method for utilizing fluorescence quenching of graphene quantum dot to detect potassium permanganate, utilizes the graphene quantum dot probe as the fluorescence probe, and carries out the detection of highly sensitive potassium permanganate solution through the characteristic that the fluorescence intensity of the graphene quantum dot probe is weakened along with the increase of the concentration of the potassium permanganate solution. The university of Huaqiao, "a method for determining potassium permanganate index in water with DPD" (201710811615.6), provide a method for determining potassium permanganate index in water with DPD, the water sample to be measured is acidified with sulfuric acid, add excessive potassium permanganate standard solution, heat and react for a certain time, utilize residual potassium permanganate among them to oxidize N, N-diethyl-1, 4-phenylenediamine and produce red DPD free radical, then measure the absorbance value of DPD free radical in its characteristic wavelength 510nm or 551nm place through the visible spectrophotometer and is used for calculating the concentration of the above-mentioned residual potassium permanganate, calculate the consumption of the potassium permanganate according to the concentration of the above-mentioned residual permanganate, and then try to find the potassium permanganate index in the water sample to be measured.

In the prior art, the cost is high, the time consumption is high, the application field is narrow, the sensitivity is low, or only one type of substances are detected, and sulfur, dinitrotoluene, trinitrotoluene and potassium permanganate solid particles cannot be detected simultaneously; in order to solve the defects of the prior art, the invention aims to provide a method for rapidly detecting sulfur, dinitrotoluene, trinitrotoluene and potassium permanganate in explosives, which has the advantages of simple operation, rapid and accurate field, easy identification, high sensitivity and low detection limit, and can provide an effective technical means for the field detection and analysis of explosives and residues thereof by safety departments.

Disclosure of Invention

The invention aims to provide a method for rapidly detecting sulfur, dinitrotoluene, trinitrotoluene and potassium permanganate in explosives, which is based on a chemical colorimetric method, and comprises the steps of preparing a detection reagent by using strong base, alcohols, dimethyl sulfoxide, a urea solution, toluene, Tween-20 or Tween-40 or Tween-60 or Tween-80 or TX-100 mixed solution, directly dripping the detection reagent on an object to be detected to generate color change, and determining the existence of the sulfur, the dinitrotoluene, the trinitrotoluene and the potassium permanganate according to the changed color. If the object to be detected contains sulfur, the suspicious substance on the substrate can be blackish green; if the object to be detected contains dinitrotoluene, the suspicious substance on the substrate can be dark blue; if the object to be detected contains trinitrotoluene, the suspicious substance on the substrate is reddish brown; if the substance to be detected contains potassium permanganate, the suspicious substance on the substrate is green. The method can be used for the rapid qualitative detection of the sulfur, the dinitrotoluene, the trinitrotoluene and the potassium permanganate in the explosive and the residues thereof in the explosive cases, the explosive searching and removing sites. The method has the advantages of simple operation, fast and accurate field, easy identification, high sensitivity and low detection limit, and can provide an effective technical means for the field detection and analysis of explosives and residues thereof for safety departments.

The invention relates to a method for rapidly detecting sulfur, dinitrotoluene, trinitrotoluene and potassium permanganate in explosives, which comprises the following steps:

preparing a colorimetric reagent:

a. mixing 6.6-60% by volume of methanol, ethanol, isopropanol, n-butanol or tert-butanol with 15.6-41.4% by volume of dimethyl sulfoxide, 6.6-20% by volume of 600g/L urea aqueous solution, 8-20% by volume of toluene, 9.8-12% by volume of tween-20, tween-40, tween-60, tween-80 or TX-100, and stirring uniformly to obtain a mixed solvent;

b. b, adding potassium hydroxide, sodium hydroxide or quaternary ammonium hydroxide with the concentration of 20-100g/L into the mixed solvent obtained in the step a, uniformly stirring to obtain a colorimetric reagent for detecting sulfur, dinitrotoluene, trinitrotoluene and potassium permanganate in the explosive, filling the colorimetric reagent into a reagent bottle, and sealing and storing;

and (3) rapid detection:

c. b, extracting a sample from the explosive suspicious source by using a key slot or a sampling swab, then dropwise adding the colorimetric reagent obtained in the step b, and if the suspicious substance contains sulfur, showing a dark green color; if the suspicious substance contains dinitrotoluene, the suspicious substance presents dark blue; if the suspicious substance contains trinitrotoluene, the suspicious substance is reddish brown; if the suspicious substance contains potassium permanganate, the suspicious substance is green.

The invention relates to a method for rapidly detecting sulfur, dinitrotoluene, trinitrotoluene and potassium permanganate in explosives, which does not need to dissolve a suspicious sample, uses a mixed solution of alkoxide and dimethyl sulfoxide to prepare a colorimetric detection reagent at room temperature, and is directly used for detecting suspicious substances on a sampling substrate, if the suspicious substances contain sulfur, the suspicious substances on the substrate are changed into dark green within 2 seconds, so as to determine the existence of the sulfur; if the material contains dinitrotoluene, the suspicious material on the substrate becomes dark blue within 2 seconds, so as to determine the existence of the dinitrotoluene; if the suspicious substance contains trinitrotoluene, the suspicious substance on the substrate becomes reddish brown within 2 seconds, so as to determine the existence of trinitrotoluene; if the suspicious substance contains potassium permanganate, the suspicious substance on the substrate turns green within 2 seconds, so that the existence of the potassium permanganate is determined. The detection reagent can be used for rapid qualitative detection of black powder, industrial explosive and sulfur, dinitrotoluene, trinitrotoluene and potassium permanganate in explosives and residues thereof, and the detection limit of naked eyes can reach microgram level. The reagent has the advantages of simple operation, fast and accurate field, easy identification, high sensitivity and low detection limit, and can provide an effective technical means for the field detection and analysis of explosives and residues thereof for safety departments.

The method for rapidly detecting the sulfur, the dinitrotoluene, the trinitrotoluene and the potassium permanganate in the explosive disclosed by the invention has the advantages that the method shows extremely low detection limit (microgram level) and extremely high selectivity on the sulfur, so that the detection on the sulfur, the dinitrotoluene, the trinitrotoluene and the potassium permanganate in the explosive and residues thereof is ensured. The color of the product is changed immediately after the product is contacted with sulfur, dinitrotoluene, trinitrotoluene and potassium permanganate, and other auxiliary means are not needed for analysis, so that the low-cost and rapid detection of the sulfur, the dinitrotoluene, the trinitrotoluene and the potassium permanganate is realized. The reagent has the characteristics of simple operation, rapid and accurate site, easy identification, high sensitivity, low detection limit and the like. The method overcomes the defects of high cost, time consumption, narrow application field, low sensitivity, detection of only one type of substance and the like in the method for detecting the sulfur, the dinitrotoluene, the trinitrotoluene and the potassium permanganate in the explosives and the residues thereof in the prior art, and provides an effective technical means for detecting the explosives and the residues thereof.

Detailed Description