CN112763471A - Trace explosive detection method - Google Patents
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- CN112763471A CN112763471A CN202011593460.1A CN202011593460A CN112763471A CN 112763471 A CN112763471 A CN 112763471A CN 202011593460 A CN202011593460 A CN 202011593460A CN 112763471 A CN112763471 A CN 112763471A
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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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
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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
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
- G01N21/64—Fluorescence; Phosphorescence
- G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
- G01N2021/6432—Quenching
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Abstract
The invention relates to a trace explosive detection method, and belongs to the technical field of chemical detection. The detection method of the explosive substance comprises the following steps: s1: providing an acidic wiping sheet, and contacting the acidic wiping sheet with the surface of a sample to be detected to attach a trace of detected substance to the acidic wiping sheet; s2: heating the acidic wiping sheet obtained in the step S1 to enable the acidic wiping sheet to react with the substance to be detected to generate gaseous substances; s3: and (4) sending the gaseous substance obtained in the step S2 to a detector by adopting a fluorescent agent based on a fluorescence quenching principle, quenching the luminescence of the fluorescent agent, and detecting the ammonium nitrate in the sample by fluorescence spectrum analysis. The invention solves the qualitative judgment and analysis of trace ammonium nitrate in the tested sample, and leads the detection sensitivity of ammonium nitrate explosives to be 0.1ng, which is improved by 1-2 orders of magnitude compared with the sensitivity in the prior art; the method can solve the limitation problem of rapidly measuring the trace ammonium nitrate in the explosive under the condition of not changing detection equipment and sensitive materials.
Description
Technical Field
The invention relates to the technical field of chemical detection, in particular to a trace explosive detection method.
Background
Since the invention of the safety explosive, the explosive plays an extremely important role in the recent social development, particularly in the military field, the aerospace field, the infrastructure construction field and some industrial fields. However, with the expansion of the application range of explosives, the appearance of new varieties of trace explosives and the technical invention of new explosives, the problem of safety management of trace explosives becomes more and more important. Ammonium nitrate dangerous chemical substances, such as ammonium nitrate, and the like, are used as main components of common chemical fertilizers, industrial raw materials and energetic materials (such as explosives, solid propellants and the like), are widely applied to the fields of China industry, agriculture, national defense and the like, and the safe production, transportation, storage and use of the ammonium nitrate dangerous chemical substances are directly related to the stable development of national production and economy. Since the 20 th century, a lot of heavy and extra-large ammonium nitrate explosion accidents occur worldwide, causing numerous casualties and huge economic losses. Therefore, the method has important theoretical and practical significance for maintaining public safety of places such as flammable and explosive hazardous chemical industrial parks and the like and guaranteeing the safety of people and national property by researching and quickly detecting trace ammonium nitrate chemical substances.
Since the last 90 s, fluorescence detection technology based on polymer materials for trace explosives has received increasing attention and research and has been successfully commercialized, representing products of FIDO series from FLIR corporation in the United states. These polymeric materials have energy level structures that match trace explosives (e.g., TNT) and that may interact with each other, such as charge transfer, chemical reactions, etc. Therefore, whether trace explosives exist can be judged by observing the change trend and the amplitude of the fluorescence of the sensitive material in the fluorescence sensor.
The traditional ion mobility spectrometry technology can also detect explosives, but the resolving power for the mixture is weak, and common explosives generally exist in the form of the mixture when in use, so that some false alarm problems can occur in practical use. Compared with the traditional ion mobility spectrometry, the fluorescence sensing technology of the nano fluorescence sensing material for trace explosives has the characteristics of high sensitivity, high selectivity, quick response, portability, no radioactive source, high environmental interference resistance and the like
In the existing method, explosive components are volatilized by a heating means, and then a fluorescence quenching detection method is adopted for detection, specifically, the volatilization of the explosive is promoted by heating, so that the explosive volatilizes and acts with a fluorescent molecule with an electron-rich group, the fluorescent molecule transfers electrons to the explosive molecule in an excited state, and the fluorescence of the fluorescent molecule is quenched, so that the effect of weakening the fluorescence is achieved. The presence of explosives can therefore be determined by detecting the decay of fluorescence. However, compared with other explosives such as TNT and S, which have strong electron-gaining capability, ammonium nitrate explosives have a weak charge transfer capability, and detection sensitivity is generally much weaker than that of TNT and S. Therefore, the invention provides a wiping sheet for improving the detection of trace ammonium nitrate explosives, a preparation method thereof and a detection method for improving the sensitivity of trace ammonium nitrate explosives, aiming at the problem of detection limitation of trace ammonium nitrate.
Disclosure of Invention
The invention provides a method for detecting explosives, which aims to solve the technical problems and adopts an acidic wiping sheet with strong acid groups attached to the surface, so that trace ammonium nitrate in the explosives can be quickly measured, and the detection sensitivity of the ammonium nitrate is lower than 0.1 ng.
The invention provides a trace explosive detection method for qualitatively analyzing trace ammonium nitrate components in an explosive sample.
The technical scheme for solving the technical problems is as follows:
s1: providing an acid wiping sheet, and contacting the acid wiping sheet with the surface of an explosive sample to be detected to attach the explosive sample to the acid wiping sheet;
s2: heating the acidic wiping sheet obtained in the step S1 until the acidic wiping sheet reacts with the sample of the explosive to be tested to generate gaseous substances;
s3: and (5) marking the gaseous substance obtained in the step (S2) with a fluorescent agent, sending the gaseous substance into a detector, quenching fluorescence, and qualitatively analyzing the ammonium nitrate component in the explosive sample to be detected through fluorescence spectroscopy.
The principle of detecting ammonium nitrate in an explosive sample according to the invention is as follows: the method comprises the steps of coating fluorescent materials on the inner wall of a quartz tube and the position corresponding to a detector, opening an excitation light source to enable the fluorescent materials to emit light, placing a wiping sheet attached with explosives to be detected in a clamping sheet of the detector, setting the clamping sheet at a temperature for detecting heat treatment in advance, enabling the explosives to be detected attached to the wiping sheet to react with sulfonic acid groups on the surface of the wiping sheet to generate volatile nitric acid (TNT, S and the like do not participate in reaction, enabling ammonium nitrate to react with strongly acidic sulfonic acid groups to generate nitric acid, and enabling volatile nitric acid to contain volatile nitric acid), pumping the volatile nitric acid into the quartz tube, enabling the volatile nitric acid to act with fluorescent molecules in an excited state, quenching the light emission of the fluorescent molecules, enabling a fluorescence spectrometer in the detector to detect the weakening of fluorescence.
The detection method of the explosive has the beneficial effects that:
the invention solves the problem of low detection sensitivity of ammonium nitrate in explosive materials, and can analyze the ammonium nitrate in the explosive materials in trace quantity under the conditions of not changing fluorescent sensor materials and not interfering the detection of other explosives.
On the basis of the technical scheme, the invention can be further improved as follows.
Further, in step S1, the acidic wiping sheet is formed by introducing sulfonic acid groups on the surface of the glass fiber sheet by a physicochemical method.
Further, the acidic wiping sheet is prepared by the following steps:
s11: providing a glass fiber sheet, and cleaning the surface of the glass fiber sheet;
s12: soaking the glass fiber sheet treated in the step S11 in a mixed solution of concentrated sulfuric acid and hydrogen peroxide, heating for 0.5-1h under the condition of micro boiling, taking out, and washing with high-purity water;
s13: soaking the glass fiber sheet treated in the step S12 in a toluene solution of octadecyl trichlorosilane, reacting for 10-30min, taking out, washing with acetone, and drying;
s14: carrying out surface oxidation reaction on the glass fiber sheet treated in the step S13 for 1-5 min;
s15: soaking the glass fiber sheet treated in the step S14 in high-purity water, adding excessive isethionic acid (after the sulfonation reaction is finished, the presence of isethionic acid components in the high-purity water indicates that excessive isethionic acid is added, or calculating the number of droplets of isethionic acid to participate in the reaction according to the surface area of the glass fiber sheet and the area of one droplet of isethionic acid attached to the glass fiber sheet, and then multiplying the number of droplets by the volume of isethionic acid obtained by converting 1.5, i.e., indicating that excessive isethionic acid is added), taking out after the sulfonation reaction is carried out for 2-4h, washing twice by turns with high-purity water and ethanol, and drying to obtain the acidic wiping sheet.
The principle of introducing sulfonic acid groups to the glass fiber sheet to obtain the acid wiping sheet is as follows:
after being cleaned, the glass fiber sheet reacts with a mixed solution of concentrated sulfuric acid and hydrogen peroxide, carboxyl is introduced through surface carboxylation reaction of the glass fiber sheet, long-chain silane is introduced through alkylation reaction of the carboxyl and alkyl trichlorosilane, then carbon base at the base end of the long-chain silane is oxidized into carboxyl in an oxygen plasma cavity, the generated carboxyl is subjected to sulfonation reaction with hydrocarbon ethyl sulfonic acid, sulfonic acid groups are introduced on the surface of the glass fiber sheet, the sulfonic acid groups are strongly acidic and can react with ammonium nitrate under a heating condition to generate volatile nitric acid, the volatile nitric acid or nitrogen dioxide which is a further decomposition product of the volatile nitric acid is sent to a detector, quenching fluorescence is weakened, and whether an explosive sample contains ammonium nitrate or not can be qualitatively judged. That is, the wiping sheet obtained by the present invention has- (-O-) on the surface thereof3Si-R-COO-CH2-SO3H group (wherein R represents 10-20 carbon atoms, and alkyl trichlorosilane is octadecyl trichlorosilane, so that R represents alkyl with 17 carbon atoms), the group has strong acidity due to sulfo group, can react with ammonium nitrate to generate volatile nitric acid, or can be decomposed into nitrogen dioxide by irradiation of an ultraviolet decomposition light source, the fluorescence intensity of the fluorescence indicator can be quenched to be weakened, the ammonium nitrate in explosive samples can be qualitatively analyzed, and the problem of low detection sensitivity of the ammonium nitrate in explosive materials is solved.
The beneficial effect of adopting the further scheme is that: the method solves the problem of introduction of sulfonic acid groups on the surface of the glass fiber sheet, and simultaneously introduces long-chain alkyl to be grafted on the surface of the glass fiber sheet through trichlorosilane, so that the long-chain alkyl can better react with ammonium nitrate in an explosive sample to be detected to generate nitric acid, the problem of low detection sensitivity of the ammonium nitrate in an explosive material is solved, the preparation is convenient and rapid, and the problem of limitation of a fluorescent indicator to the ammonium nitrate in explosive detection is solved.
Further, in step S11, the specific method of cleaning includes: washing the glass fiber sheet with high-purity water, soaking in detergent for 24h, taking out, soaking in acetone solution, washing with ultrasonic wave for 10min, taking out, soaking in ethanol solution, and washing with ultrasonic wave for 10 min.
The beneficial effect of adopting the further scheme is that: by adopting the cleaning method, the glass fiber sheet can be better cleaned, and the interference of impurities attached to the surface of the glass fiber sheet on chemical reaction is effectively reduced.
Further, in step S12, the mixed solution of the concentrated sulfuric acid and the hydrogen peroxide is prepared from the concentrated sulfuric acid with a mass fraction of 98% and the hydrogen peroxide with a mass fraction of 30% according to a volume ratio of 3:1 to 7: 3.
Further, in step S13, in the toluene solution of octadecyltrichlorosilane, the volume fraction of octadecyltrichlorosilane is 0.5% -1%; the drying is drying by nitrogen at normal temperature.
Further, in step S14, the temperature of the surface oxidation reaction is 20 to 30 ℃.
Further, in step S15, the temperature of the sulfonation reaction is 150-200 ℃; the drying is drying by nitrogen at normal temperature.
Further, in step S2, the heating temperature is 100 ℃ to 200 ℃, and if the explosive sample liquid is attached to the surface of the acidic wiping sheet, the acidic wiping sheet needs to be dried before heating.
Further, in step S3, the gaseous substance is irradiated by the ultraviolet decomposition light source to be decomposed into gaseous decomposition products before being sent to the detector, and then the gaseous decomposition products are sent to the detector again. Nitric acid in the gaseous substance is decomposed into nitrogen dioxide gaseous decomposition products under the irradiation of an ultraviolet decomposition light source, the nitric acid and the nitrogen dioxide gaseous decomposition products in the gaseous substance can quench fluorescence luminescence, and ammonium nitrate in the explosive sample is qualitatively analyzed through fluorescence spectroscopy.
Compared with the prior art, the detection method of the explosives provided by the invention has the following advantages:
1. the qualitative analysis of trace ammonium nitrate in the explosive is solved, the detection sensitivity of the ammonium nitrate explosive is increased by 1-2 orders of magnitude, and the detection sensitivity can realize the qualitative analysis of 0.1 ng.
2. The acid wiping sheet prepared by the invention is convenient and quick to sample and detect, and can quickly measure trace ammonium nitrate in explosives under the condition of not changing detection equipment.
3. The preparation method of the acidic wiping sheet is simple and easy to obtain, and is beneficial to large-scale production.
4. The invention solves the problem of limitation of ammonium nitrate in detection of explosives by fluorescent indicators.
Drawings
FIG. 1 is a schematic flow chart of the present invention for detecting ammonium nitrate in explosives
FIG. 2 is a flow chart of the preparation principle of introducing sulfonic acid groups onto an acidic wiping sheet according to the present invention;
FIG. 3 is a graph showing a fluorescence test curve obtained in example 1 of the present invention;
FIG. 4 is a graph showing a fluorescence test curve obtained in example 2 of the present invention;
FIG. 5 is a graph showing the fluorescence test curve obtained in comparative example 1 of the present invention;
FIG. 6 is a graph showing the fluorescence test curve obtained in comparative example 2 of the present invention;
FIG. 7 is a graph showing the fluorescence test curve obtained in comparative example 3 of the present invention;
FIG. 8 is a graph showing the fluorescence test curve obtained in comparative example 4 of the present invention.
Detailed Description
The principles and features of this invention are described below in conjunction with the following drawings, which are set forth by way of illustration only and are not intended to limit the scope of the invention.
Example 1
The embodiment provides a method for detecting explosives, which specifically includes the following steps:
preparing materials: octadecyltrichlorosilane, with a purity of > 95%, purchased from tianjin Xiangyu science and technology trade; toluene with purity > 99.9%, purchased from Shanghai chemical reagent III works; the hydroxyethyl sulfonic acid, the acetone and the absolute ethyl alcohol are analytically pure; ultrapure water is self-made in laboratories.
Preparing equipment: PDC-MG type inductive type radio frequency plasma cleaner; USB4000 spectrometer.
Preparation of acidic wiping sheets:
according to the attached figure 1, the specific operation steps are as follows:
washing a glass fiber sheet containing silicon dioxide with the size of 70 mm by 20mm by using high-purity water, soaking the glass fiber sheet in soap water for 24 hours, then placing the glass fiber sheet in an acetone solution, ultrasonically shaking and cleaning for 10 minutes, taking out the glass fiber sheet, repeatedly washing the glass fiber sheet by using the high-purity water for multiple times, then placing the glass fiber sheet in an ethanol solution, ultrasonically shaking and cleaning for 10 minutes, taking out the glass fiber sheet, repeatedly washing the glass fiber sheet by using the high-purity water, finally placing the glass fiber sheet in the high-purity water, ultrasonically shaking and cleaning;
putting a glass fiber sheet into a mixed solution prepared by concentrated sulfuric acid with the mass fraction of 98% and hydrogen peroxide with the mass fraction of 30% according to the volume ratio of 7:3, heating for 1 hour under the condition of micro boiling, taking out, washing with high-purity water, observing the amount of liquid attached to the surface of the glass sheet before washing to prevent the glass fiber wiping sheet from being damaged by heat generated by mixing the concentrated sulfuric acid with the high-purity water, and drying with nitrogen for later use after washing;
putting the glass fiber sheet into a mixed solution of octadecyltrichlorosilane and toluene, wherein the mass fraction of the octadecyltrichlorosilane in the toluene solution is 1%, reacting for 15min at normal temperature, taking out, repeatedly washing with acetone, and drying with nitrogen for later use (if the glass fiber sheet is not used for a long time, the glass fiber sheet needs to be stored in a dry container);
putting the glass fiber sheet into a PDC-MG type inductive radio frequency plasma cleaning machine, carrying out oxidation reaction for 5min, and taking out;
putting the glass fiber sheet into high-purity water, transferring the glass fiber sheet into a stainless steel high-pressure kettle with a polytetrafluoroethylene lining, adding excessive hydroxyethyl sulfonic acid, sealing, putting the high-pressure kettle into a drying oven, performing sulfonation reaction at 200 ℃ for 4 hours, taking out the glass fiber sheet, drying and cooling the glass fiber sheet, repeatedly washing the glass fiber sheet with the high-purity water and ethanol for multiple times, drying the glass fiber sheet with nitrogen, and sealing and storing the glass fiber sheet to obtain the acidic wiping sheet.
The wiping sheet prepared by the preparation method has sulfonic acid groups on the surface, so that the surface of the wiping sheet is strongly acidic and is an acidic wiping sheet.
A method for detecting explosives using an acidic wiper blade, according to figure 2, comprising the steps of:
1. dripping 1 mu L of ammonium nitrate aqueous solution to-be-detected sample on the upper surface of the acid wiping sheet, and naturally airing (if the surface of the acid wiping sheet is attached with a solid explosive sample, airing is not needed);
2. coating a fluorescent material on the inner wall of the quartz tube at a position corresponding to a detector of the explosive detector, placing the quartz tube in a dark environment, starting an excitation light source to enable the fluorescent material to emit light, setting the temperature of a clamping piece of the detector to be 180 ℃ of the temperature required by heat treatment, and keeping;
3. and placing the acidic wiping sheet on a clamping sheet of an explosive detector, pumping gaseous substances generated by heat treatment into a quartz tube to enable the gaseous substances to contact with the fluorescent agent and quench the luminescence of the fluorescent agent, detecting by using a fluorescence spectrometer to obtain a fluorescence spectrum curve, and qualitatively analyzing the ammonium nitrate in the explosive sample by using the fluorescence spectrum curve.
The obtained fluorescence spectrum curve is shown in FIG. 3, and the test result is: the lower limit of the sensitivity detection of ammonium nitrate is 0.1-0.5 ng.
Example 2
This example is the same as the detection method of example 1, except that: the wiping sheet is an untreated common glass fiber sheet (when in use, the surface of the glass fiber sheet needs to be cleaned). The method comprises the steps of washing with high-purity water, soaking in soap water for 24 hours, then sequentially placing in an ultrasonic oscillator in acetone and ethanol, oscillating and cleaning for 10min, repeatedly washing the glass sheet with a large amount of high-purity water after each oscillating and cleaning, finally placing in the ultrasonic oscillator in high-purity water, cleaning for 10min, and drying for later use.
The obtained fluorescence spectrum curve is shown in FIG. 4, and the test result is: the lower limit of the sensitivity detection of the ammonium nitrate is 2-5 ng.
Comparative example 1
This example is the same as the detection method of example 1, except that: a1 ng/. mu.L aqueous TNT solution was used as the sample to be probed.
The obtained fluorescence spectrum curve is shown in FIG. 5, and the test result is: the lower limit of detection sensitivity is less than 0.1 ng.
Comparative example 2
This example is the same as the detection method of example 1, except that: 1. taking 1 ng/mu L TNT aqueous solution as a sample to be detected; 2. the wiping sheet is an untreated common glass fiber sheet (when in use, the surface of the glass fiber sheet needs to be cleaned). The method comprises the steps of washing with high-purity water, soaking in soap water for 24 hours, then sequentially placing in an ultrasonic oscillator in acetone and ethanol, oscillating and cleaning for 10min, repeatedly washing the glass sheet with a large amount of high-purity water after each oscillating and cleaning, finally placing in the ultrasonic oscillator in high-purity water, cleaning for 10min, and drying for later use.
The obtained fluorescence spectrum curve is shown in FIG. 6, and the test result is: the lower limit of detection sensitivity is less than 0.1 ng.
Comparative example 3
This example is the same as the detection method of example 1, except that: as a sample to be detected, 1 ng/. mu.L of an aqueous S (elemental sulfur) solution was used.
The obtained fluorescence spectrum curve is shown in FIG. 7, and the test result is: the lower limit of detection sensitivity is less than 0.1 ng.
Comparative example 4
This example is the same as the detection method of example 1, except that: 1. 1 ng/mu L of S (elemental sulfur) aqueous solution is adopted; 2. the wiping sheet is an untreated common glass fiber sheet (when in use, the surface of the glass fiber sheet needs to be cleaned). The method comprises the steps of washing with high-purity water, soaking in soap water for 24 hours, then sequentially placing in an ultrasonic oscillator in acetone and ethanol, oscillating and cleaning for 10min, repeatedly washing the glass sheet with a large amount of high-purity water after each oscillating and cleaning, finally placing in the ultrasonic oscillator in high-purity water, cleaning for 10min, and drying for later use.
The obtained fluorescence spectrum curve is shown in FIG. 8, and the test result is: the lower limit of detection sensitivity is less than 0.1 ng.
The experimental conclusion proves that: 1. the lower limit of the sensitivity of detecting ammonium nitrate in explosives by adopting the acid wiping sheet is lower than that of detecting ammonium nitrate in explosives without adopting the acid wiping sheet, so that the trace amount of ammonium nitrate in the explosives can be qualitatively analyzed, the detection sensitivity of the trace amount of ammonium nitrate can be improved by 1-2 orders of magnitude by adopting the wiping sheet prepared by the preparation method of the wiping sheet, and the detection sensitivity of the ammonium nitrate in the explosives can reach 0.1 ng; 2. according to the examples and comparative examples, the acid wiper blade was not sensitive to TNT, S explosives detection.
The term "wiping sheet" used herein generally refers to a sheet-like structure that an object is wiped with cloth or the like to clean the object, and the wiping sheet prepared and applied herein is a sheet-like structure that an explosive to be detected is attached to the surface thereof by wiping, contacting or the like, and is generally made square for the convenience of collecting the explosive to be detected, and the wiping sheet used herein is 70 × 20 mm; in addition, the expression "contacting the wiping sheet with the explosive sample to be detected" is understood to mean that the explosive sample is naturally attached to the surface of the wiping sheet by means of wiping, contacting and the like in actual use, and the method is used for qualitatively analyzing trace ammonium nitrate with weak charge transfer capability in the explosive sample, so that the thickness of the explosive sample attached to the wiping sheet and the concentration requirement of the ammonium nitrate in the explosive do not need to be set deliberately.
The term "trace amount" as used herein in the field of applied science means that the content of a certain substance is below one part per million, and the trace amount of ammonium nitrate in an explosive sample herein means that the mass fraction of ammonium nitrate in the explosive sample is less than or equal to one part per million.
The term "qualitative analysis" as used herein, which is the detection of trace ammonium nitrate species components in explosives samples by fluorescence spectroscopy, is the identification and characterization of which elements, radicals, functional groups or compounds the species consists of.
The term "slight boiling" as used herein generally refers to a state of a liquid just before boiling, and since the glass fiber pieces are reacted in a mixed solution of concentrated sulfuric acid and hydrogen peroxide, the glass fiber pieces are reacted under slight boiling conditions in order to avoid the danger of boiling and splashing of the concentrated sulfuric acid.
As used herein, a "detergent" is an agent such as a washing powder, soapy water, or a detergent that is capable of cleaning the surface of the fiberglass sheet, and is not further limited herein.
In the description of the present invention, "a plurality" means at least two, e.g., two, three, etc., unless specifically limited otherwise.
In the description of the present specification, reference to the description of the terms "embodiment 1", "this embodiment", "example", "specific example", or "some examples", etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. A method for trace explosive detection, comprising the steps of:
s1: providing an acid wiping sheet, and contacting the acid wiping sheet with the surface of an explosive sample to be detected to attach the explosive sample to the acid wiping sheet;
s2: heating the acidic wiping sheet obtained in the step S1 until the acidic wiping sheet reacts with the sample of the explosive to be tested to generate gaseous substances;
s3: and (5) marking the gaseous substance obtained in the step (S2) with a fluorescent agent, sending the gaseous substance into a detector, quenching fluorescence, and qualitatively analyzing the ammonium nitrate component in the explosive sample to be detected through fluorescence spectroscopy.
2. The method for detecting a trace explosive according to claim 1, wherein in step S1, the acidic wiping sheet is formed by introducing strong acidic groups to the surface of the wiping sheet by a physicochemical method.
3. The trace explosive detection method according to claim 1, wherein the acidic wiping sheet is prepared by the steps of:
s11: providing a glass fiber sheet, and cleaning the surface of the glass fiber sheet;
s12: soaking the glass fiber sheet treated in the step S11 in a mixed solution of concentrated sulfuric acid and hydrogen peroxide, heating for 0.5-1h under the condition of micro boiling, taking out, and washing with high-purity water;
s13: soaking the glass fiber sheet treated in the step S12 in a toluene solution of octadecyl trichlorosilane, reacting for 10-30min, taking out, washing with acetone, and drying;
s14: carrying out surface oxidation reaction on the glass fiber sheet treated in the step S13 for 1-5 min;
s15: and (4) soaking the glass fiber sheet treated in the step (S14) in high-purity water, adding excessive hydroxyethyl sulfonic acid, performing sulfonation reaction for 2-4h, taking out, washing twice by using high-purity water and ethanol in turn, and drying to obtain the acidic wiping sheet.
4. The method for detecting trace explosives in claim 3, wherein in the step S11, the specific method for cleaning is as follows: washing the glass fiber sheet with high-purity water, soaking in detergent for 24h, taking out, soaking in acetone solution, washing with ultrasonic wave for 10min, taking out, soaking in ethanol solution, and washing with ultrasonic wave for 10 min.
5. The method for detecting a trace explosive according to claim 3, wherein in step S12, the mixed solution of concentrated sulfuric acid and hydrogen peroxide is prepared from 98% by mass of concentrated sulfuric acid and 30% by mass of hydrogen peroxide in a volume ratio of 3:1 to 7: 3.
6. The method for detecting a trace explosive according to claim 3, wherein in step S13, the volume fraction of octadecyltrichlorosilane in the toluene solution of octadecyltrichlorosilane is 0.5% -1%; the drying is drying by nitrogen at normal temperature.
7. The method for detecting a trace explosive according to claim 3, wherein the temperature of the surface oxidation reaction in step S14 is 20-30 ℃.
8. The trace explosive detection method according to claim 3, wherein the temperature of the sulfonation reaction is 150 ℃ to 200 ℃ in step S15; the drying is drying by nitrogen at normal temperature.
9. The method for detecting a trace explosive according to claim 1, wherein the heating temperature is 100 ℃ to 200 ℃ in step S2.
10. The method for detecting a trace explosive according to any one of claims 1 to 8, wherein in step S3, said gaseous substance is decomposed into gaseous decomposed substances by irradiation with an ultraviolet decomposition light source before being sent to the detector, and then said gaseous decomposed substances are sent to the detector again.
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| CN115791730A (en) * | 2022-11-30 | 2023-03-14 | 中船重工安谱（湖北）仪器有限公司 | Optical detection module for detecting trace drugs and explosives |
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