CN111208097A - Device and method for detecting RDX fluorescence of explosive - Google Patents

Device and method for detecting RDX fluorescence of explosive Download PDF

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CN111208097A
CN111208097A CN201811388785.9A CN201811388785A CN111208097A CN 111208097 A CN111208097 A CN 111208097A CN 201811388785 A CN201811388785 A CN 201811388785A CN 111208097 A CN111208097 A CN 111208097A
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rdx
light source
fluorescence
explosives
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CN111208097B (en
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冯亮
高建梅
王昱
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Dalian Institute of Chemical Physics of CAS
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    • 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
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    • G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"

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Abstract

The invention provides a device for detecting explosive RDX fluorescence and a detection method thereof, the device integrates an explosive RDX decomposition light source and an excitation light source, wherein a short-wavelength ultraviolet lamp bead is used as the decomposition light source of the RDX, a longer-wavelength ultraviolet lamp bead is used as the excitation light source of the RDX, the RDX after photolysis of the decomposition light source interacts with a fluorescence indicator to be excited by the excitation light source, emitted light passes through a lens and a light filter, a photomultiplier is used as a fluorescence signal detector, and finally, a signal is output by the voltage of a universal meter. The device simple structure, convenient to carry, the practicality is strong, can realize detecting on the spot of explosive RDX, has good application prospect in RDX's fluorescence detection.

Description

Device and method for detecting RDX fluorescence of explosive
Technical Field
The invention belongs to the technical field of analytical instruments, and particularly relates to a device and a method for detecting explosive RDX fluorescence.
Background
As is known, along with the increasing and rampant terrorism and complex composition in China and China, various explosives with huge power are utilized by terrorists, which brings serious harm to national safety and ecological environment, thereby having great significance for detecting explosives all the time. The cyclotrimethylenetrinitramine (RDX) is an important explosive, the application range of the cyclotrimethylenetrinitramine is second to trinitrotoluene (TNT), but compared with TNT, due to the fact that the lowest unoccupied orbital level of the TNT is higher, the electron receiving capacity of the TNT is weaker, and the RDX is more difficult to detect by using a conventional detection method. In recent years, the detection of explosives RDX has relied on large instrumentation such as gas/liquid chromatography, mass spectrometry, ion mobility spectrometry, etc. Although these large instruments can meet practical requirements in terms of sensitivity and detection limits, operating these large instruments often requires experienced technicians and many still have difficulty in real-time on-line detection in the field, thus requiring a simpler method for detecting explosive RDX.
In recent years, fluorescent materials with great potential have received wide attention due to the characteristics of diverse synthetic methods, low cost, high sensitivity and good selectivity. At present, many documents report that the qualitative and quantitative detection of explosive RDX by using fluorescent probe molecules is realized. However, some problems still need to be solved, for example, although the generation of fluorescence can be identified by naked eyes after being irradiated by an ultraviolet lamp, the fluorescence intensity needs to be scanned by a fluorescence spectrometer for accurate quantification, and the fluorescence spectrometer is also inconvenient to carry and difficult to realize the requirement of field detection, so that the fluorescence spectrometer is changed into a small instrument which is convenient to operate on the premise of not losing sensitivity, and the defect that the existing fluorescence spectrometer is large in size and difficult to carry is overcome while the high-sensitivity detection of explosives RDX is met.
Disclosure of Invention
The invention aims to make up for the defects of the existing instrument and provides an explosive RDX fluorescence detection device and a detection method thereof, which can meet the requirements of on-site fluorescence quantitative detection of the explosive RDX.
The technical scheme of the invention is as follows:
a device for detecting explosive RDX fluorescence comprises a fluorescent molecular probe of hydrazine group substituted BODIPY derivative and a fluorescence detection device, wherein the detection device consists of an RDX decomposition light source, an excitation light source, a sample measuring position, a light path system, a detector and a base. Placing the fluorescent molecular probe in a quartz cuvette to be placed at a sample measuring position after reacting with the RDX photolysis product;
the decomposition light source, the excitation light source, the sample measuring position and the optical path system are all fixed on the base;
the photolysis light source is positioned at the bottom of the sample measuring position, and the excitation light source is positioned at the side of the sample measuring position;
the light of the decomposition light source enters a sample measuring position, formaldehyde and active free radicals are generated through decomposition for a period of time, after the formaldehyde and the active free radicals react with the fluorescent indicator, an excitation light source is opened, and fluorescence emitted by a product enters a detector through a light path system in the vertical direction.
The structural formula of the fluorescence sensor of the hydrazine-substituted BODIPY derivative is as follows:
Figure BDA0001873564630000021
the wavelength range of the decomposition light source (1) is 254nm-265nm, and the wavelength range of the excitation light source (2) is 340-370 nm.
The optical path system consists of two lenses and a long-wave pass filter, wherein the lens is a phi 12.7K9 plano-convex lens coated with MgF2An antireflection film and a long-wave pass filter are arranged between the two lenses, and the interception wavelength is 400 nm.
The detector (5) is a photomultiplier and is connected with a universal meter, signals are converted into voltage signals through the universal meter and are output, when fluorescence is enhanced, the voltage signals are increased, and when the fluorescence is weakened, the voltage signals are reduced.
The decomposition time of the decomposition light source is 1-20 minutes.
A method for detecting explosive RDX fluorescence, which adopts the device for detecting explosive RDX fluorescence; the specific operation steps of detection are as follows:
(1) adding an explosive RDX solution to be detected into a quartz cuvette, and turning on a decomposition light source;
(2) after photolysis for a period of time, turning off a decomposition light source, and adding a certain amount of fluorescent indicator;
(3) after being mixed uniformly, the mixture reacts for a period of time, and an excitation light source is turned on;
(4) and reading the voltage signal through a multimeter, and substituting the voltage signal into the standard curve to calculate the concentration of the explosive.
The specification of the quartz cuvette in the operation step (1) is 1 multiplied by 1 cm;
in the operation step (1), solvents of RDX are methanol, acetonitrile and ethanol;
the adding volume of the fluorescent indicator in the operation step (2) is 500-;
the reaction time after mixing in the operation step (3) is 10-60 s.
The invention has the following advantages:
1. the device has small volume, lower cost and convenient carrying, and can realize the field detection of the explosive RDX;
2. the device integrates the RDX decomposition light source and the exciting light source, and is more convenient and faster to use;
3. the device has high sensitivity, and can detect 0.1 mu M of RDX;
4. the device has good linear relation to RDX fluorescence response, and can realize accurate quantification of RDX.
Drawings
FIG. 1 is a schematic view of a fluorescence detection device for explosive RDX;
FIG. 2 is a linear relationship of fluorescence detection device for explosive RDX to RDX.
Wherein, 1 is an RDX decomposition light source, 2 excitation light sources, 3 sample measuring positions, 4 optical path systems, 5 detectors and 6 bases.
Detailed Description
The following examples further illustrate the invention but are not intended to limit it.
Example 1
As shown in fig. 1, the device for detecting RDX fluorescence of an explosive consists of an RDX decomposition light source 1, an excitation light source 2, a sample measurement part 3, an optical path system 4, a detector 5 and a base 6. The photolysis light source 1 is positioned at the bottom of the sample measuring position 3, and the excitation light source 2 is positioned at the side of the sample measuring position 3; the decomposition light source 1 is a short-wavelength ultraviolet lamp bead with the wavelength of 265nm, the excitation light source 2 is a longer-wavelength ultraviolet lamp bead with the wavelength of 365 nm; the optical path system comprises two lenses and a long wave pass filter, wherein the lens is a phi 12.7K9 plano-convex lens coated with MgF2An antireflection film and a long-wave pass filter are arranged between the two lenses, and the interception wavelength is 400 nm; the decomposition light source 1, the excitation light source 2, the sample measuring position 3 and the optical path system 4 are all fixed on the base 6. The detector 5 is photoelectricIncrease the pipe, link to each other with the universal meter, the signal passes through the universal meter and turns into voltage signal output, and when fluorescence reinforcing, voltage signal increases, and when fluorescence weakens, voltage signal reduces.
Example 2
And (3) preparing a standard curve:
the device for the fluorescence detection of explosive RDX described in example 1 was used in the preparation of a standard curve for standard RDX. 0.5mg of the fluorescence sensor was weighed out and dissolved in 20ml of acetonitrile to prepare 10. mu.L of 1X 10-5M，5×10-5M，1×10-4M，5×10-4M，1×10-3M，2×10-3M，4×10-3And (3) placing the RDX standard solution of M in a quartz cuvette, opening a 265nm ultraviolet lamp for photolysis for 3 minutes, closing the 265nm ultraviolet lamp, adding a 990 mu L fluorescence sensor, immediately opening a 365nm ultraviolet lamp after 10 seconds, reading a voltage value output by the multimeter, and drawing a standard curve by taking the voltage value as a vertical coordinate and the RDX concentration as a horizontal coordinate, wherein the standard curve is shown in figure 2.
Example 3
Determination of unknown concentrations of RDX:
the device for detecting the RDX of the explosive in the embodiment 1 is used for measuring the RDX with unknown concentration, 0.5mg of a fluorescence sensor is weighed and dissolved in 20ml of acetonitrile, 10 mu L of RDX solution with certain concentration is prepared and placed in a quartz cuvette, a 265nm ultraviolet lamp is opened for photolysis for 3 minutes, a 990 mu L fluorescence sensor is added after the 265nm ultraviolet lamp is closed, a 365nm ultraviolet lamp is immediately opened after 10 seconds, the voltage value output by a universal meter is read, and the voltage value is substituted into a standard curve to obtain the concentration value of the RDX, wherein the concentration value is consistent with the result of a laboratory fluorescence detector.
Example 4
Determination of unknown concentrations of RDX:
the device for detecting the RDX of the explosive in the embodiment 1 is used for measuring the RDX with unknown concentration, 0.5mg of a fluorescence sensor is weighed and dissolved in 20ml of acetonitrile, 10 mu L of RDX solution with certain concentration is prepared and placed in a quartz cuvette, a 265nm ultraviolet lamp is opened for photolysis for 5 minutes, a 990 mu L fluorescence sensor is added after the 265nm ultraviolet lamp is closed, a 365nm ultraviolet lamp is immediately opened after 10 seconds, the voltage value output by a universal meter is read, and the voltage value is substituted into a standard curve to obtain the concentration value of the RDX, wherein the concentration value is consistent with the result of a laboratory fluorescence detector.
Example 5
Determination of unknown concentrations of RDX:
the device for detecting the RDX of the explosive in example 1 is used for detecting RDX with unknown concentration, 0.5mg of a fluorescence sensor is weighed and dissolved in 20ml of acetonitrile, 10 mul of RDX solution with certain concentration is prepared and placed in a quartz cuvette, a 265nm ultraviolet lamp is opened for photolysis for 5 minutes, a 1490 mul fluorescence sensor is added after the 265nm ultraviolet lamp is closed, a 365nm ultraviolet lamp is immediately opened after 10 seconds, the voltage value output by a multimeter is read, and the voltage value is substituted into a standard curve to obtain the concentration value of RDX, wherein the concentration value is consistent with the result of a laboratory fluorescence detector.

Claims (11)

1. An apparatus for RDX fluorescence detection of explosives, characterized in that the apparatus: the detection device consists of an RDX decomposition light source (1), an excitation light source (2), a sample measuring part (3), a light path system (4), a detector (5) and a base (6), wherein the fluorescent molecular probe is placed at the sample measuring part after reacting with an RDX photolysis product in a quartz cuvette;
the decomposition light source (1), the excitation light source (2), the sample measuring position (3) and the optical path system (4) are all fixed on the base (6);
the photolysis light source (1) is positioned at the bottom of the sample measuring position (3), and the excitation light source (2) is positioned on the side of the sample measuring position (3);
light rays of the decomposition light source (1) enter a sample measuring position (3), are decomposed for a period of time to generate formaldehyde and active free radicals, and after the formaldehyde and the active free radicals react with a fluorescent indicator, an excitation light source (2) is turned on, and fluorescence emitted by a product enters a detector (5) through a light path system (4) in the vertical direction.
2. An apparatus for RDX fluorescence detection of explosives in accordance with claim 1, wherein: the structural formula of the fluorescence sensor of the hydrazine-substituted BODIPY derivative is as follows:
Figure FDA0001873564620000011
3. an apparatus for RDX fluorescence detection of explosives in accordance with claim 1, wherein: the wavelength range of the decomposition light source (1) is 254nm-265nm, and the wavelength range of the excitation light source (2) is 340-370 nm.
4. An apparatus for RDX fluorescence detection of explosives in accordance with claim 1, wherein: the optical path system consists of two lenses and a long-wave pass filter, wherein the lens is a phi 12.7K9 plano-convex lens coated with MgF2An antireflection film and a long-wave pass filter are arranged between the two lenses, and the interception wavelength is 400 nm.
5. An apparatus for RDX fluorescence detection of explosives in accordance with claim 1, wherein: the detector (5) is a photomultiplier and is connected with a universal meter, signals are converted into voltage signals through the universal meter and are output, when fluorescence is enhanced, the voltage signals are increased, and when the fluorescence is weakened, the voltage signals are reduced.
6. An apparatus for RDX fluorescence detection of explosives in accordance with claim 1, wherein: the decomposition time of the decomposition light source is 1-20 minutes.
7. A method for RDX fluorescence detection of explosives, characterized by: the device for the RDX fluorescence detection of explosives in accordance with claim 1 is used, and the specific operation steps are as follows:
(1) adding an explosive RDX solution to be detected into a quartz cuvette at a sample detection position, and turning on a decomposition light source;
(2) after photolysis for a period of time, turning off a decomposition light source, and adding a certain amount of fluorescent indicator;
(3) after being mixed uniformly, the mixture reacts for a period of time, and an excitation light source is turned on;
(4) and reading the voltage signal through a multimeter, and substituting the voltage signal into the standard curve to calculate the concentration of the explosive.
8. The RDX fluorescence detection method for explosives in accordance with claim 7, characterized in that: the specification of the quartz cuvette in the operation step (1) is 1X 1 cm.
9. Method for RDX fluorescence detection of explosives in accordance with claim 7, characterized in that: the solvent of RDX in the operation step (1) is methanol, acetonitrile and ethanol.
10. Method for RDX fluorescence detection of explosives in accordance with claim 7, characterized in that: the fluorescence indicator in the operation step (2) is a fluorescent molecular probe of hydrazine group substituted BODIPY derivative, and the addition volume is 500-.
11. Method for RDX fluorescence detection of explosives in accordance with claim 7, characterized in that: the reaction time after mixing in the operation step (3) is 10-60 s.
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20150056711A1 (en) * 2012-03-21 2015-02-26 University Of Connecticut Explosive Detection Polymer Comprising Functionalized Polyamine Polymers and Methods of Using the Same
CN108473862A (en) * 2015-11-16 2018-08-31 弗尔斯特博士研究院有限责任两合公司 For detecting in air, in solution and from wipe samples based on NOxExplosive fluorescent dye film

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20150056711A1 (en) * 2012-03-21 2015-02-26 University Of Connecticut Explosive Detection Polymer Comprising Functionalized Polyamine Polymers and Methods of Using the Same
CN108473862A (en) * 2015-11-16 2018-08-31 弗尔斯特博士研究院有限责任两合公司 For detecting in air, in solution and from wipe samples based on NOxExplosive fluorescent dye film

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
J.HAWRI,ET AL: "Photodegradation of RDX in Aqueous Solution:A Mechanistic Probe for Biodegradation with Rhodococcus sp", 《ENVIRON.SCI.TECHNOL.》 *
赵军伟: "基于BODIPY的次氯酸根荧光探针及pH和光双控药物传输纳米硅球的合成与应用研究", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 *

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