CN109900662A - A kind of highly sensitive smooth miniflow explosive detector - Google Patents

A kind of highly sensitive smooth miniflow explosive detector Download PDF

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Publication number
CN109900662A
CN109900662A CN201910171658.1A CN201910171658A CN109900662A CN 109900662 A CN109900662 A CN 109900662A CN 201910171658 A CN201910171658 A CN 201910171658A CN 109900662 A CN109900662 A CN 109900662A
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China
Prior art keywords
miniflow
laser
dnt
smooth
organic luminescent
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CN201910171658.1A
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Chinese (zh)
Inventor
范茂雯
王艳琼
龚朝阳
杨熙
龚元
吴杰云
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University of Electronic Science and Technology of China
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University of Electronic Science and Technology of China
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Priority to CN201910171658.1A priority Critical patent/CN109900662A/en
Publication of CN109900662A publication Critical patent/CN109900662A/en
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Abstract

The invention discloses a kind of highly sensitive smooth miniflow explosive detectors, belong to field of sensing technologies.The specific method is as follows for it: solution to be measured being mixed with organic luminescent dyes, is sucked fluid sample in the microchannel in Fabry-Perot cavity using sampling pump, under pulse pump light action, resonant cavity provides light feedback, realizes the output of miniflow laser.Relationship between first Calibration of Laser intensity and DNT concentration, then laser intensity is exported by spectrometer measurement, in conjunction with calibration curve, realize DNT detection.The present invention combines organic luminescent dyes with light miniflow laser, has a clear superiority than traditional fluorescence sense.Meanwhile smooth miniflow explosive detector provided by the invention is easy to operate, low in cost, measurement sensitivity is high, and dynamic range is big, suitable for the real-time detection inside micro-fluidic chip.

Description

A kind of highly sensitive smooth miniflow explosive detector
Technical field
The invention belongs to sensor technical fields, and in particular to a kind of highly sensitive smooth miniflow explosive detector.
Background technique
Explosive constitutes safely grave danger to state and society, and explosive and its reactant are water-soluble or organic molten Agent, it is toxic to plant, it is also harmful to human health.Therefore, explosive detection is heavy to preventing security threat and environmental pollution to have Want meaning.Common explosive usually contains the compound dinitro of nitro-aromatic, 1-3 trinitrotoluene (TNT) and its degradation Toluene (DNT).So the explosive detection towards safety and environmental protection is test object mainly for TNT and DNT.
Fluorescent organic dyes are because of its quick response, low cost and the advantages of being readily synthesized and by pass in explosive sensing Note.Organic dyestuff can be used for specific determinand identification and sensing by design synthesis.Nitroaromatic explosive is electron deficient , fluorescent quenching is generated when it interacts with the fluorescent organic dyes rich in electronics.Up to the present, a variety of tools have been synthesized There is the fluorescent dye of electron rich conjugated backbone, and is used for realizing the chemical sensor of Nitroaromatic explosive detection.Overcome The sensitivity of traditional fluorescence explosives sensor is lower, and dynamic range is small, and Monitoring lower-cut is high, is not able to satisfy highly sensitive detection The problem of demand.
On the other hand, light microfluidic technology develops into a kind of novel highly sensitive biochemical sensitive technology in recent years, at present Until, not light-exposed microfluidic technology is used for explosive detection.
Summary of the invention
The present invention on the basis of in the introduction, designs and has made a kind of smooth miniflow explosive detector.The sensing Device has the characteristics that of simple structure and low cost, measurement sensitivity is high, dynamic range is big.
A kind of smooth miniflow explosive detector, including sample detection part and signal collection part;Sample detection part packet It includes: pulse laser (1), convergent lens (3), reflecting mirror (4), microchannel (6), Fabry-Perot cavity (7), injection Device (8), sampling pump (9).
The pulse laser (1) provides pump energy, exports pulse pump light, concentrated lens and reflecting mirror are radiated at On Fabry-Perot cavity.The Fabry-Perot cavity (7) includes upper and lower two pieces of reflecting mirrors disposed in parallel and two Support construction between reflecting mirror.The microchannel includes the round plastic hose of rectangular capillary and its two sides, rectangular hair Tubule is set in resonant cavity, and resonant cavity provides light feedback for miniflow laser, and makes miniflow laser more back and forth in resonant cavity Secondary reflection improves sensing sensitivity.The syringe (8) and sampling pump (9) are at the uniform velocity to convey organic luminescent dyes and to be measured molten The mixed liquor of liquid passes in and out microchannel.After the pulse pump light is incident in method amber resonant cavity, organic luminescent dyes molecule is inhaled Pulse pump light energy is received, stimulated radiation occurs, generates the output of laser sensing signal.
Signal collection processing unit point includes: gathering element (5), optical fiber (10), spectrometer (11), computer (12).It is described The laser sensing signal being collected into is coupled in optical fiber (10) by gathering element (5), and laser sensing signal is transmitted along optical fiber (10) To spectrometer, spectrometer (11) handles laser signal, and processing result is output to computer (12).
Its specifically used method is: solution to be measured mixed with organic luminescent dyes, it is using sampling pump (9) that mixed liquor is defeated Enter in the microchannel in Fabry-Perot cavity (7), under pumping laser effect, resonant cavity provides light feedback, realizes micro- Flow laser output.Relationship between preparatory Calibration of Laser intensity and DNT concentration, then the miniflow laser exported by spectrometer measurement Intensity realizes DNT detection in conjunction with calibration curve.
Donor-acceptor-donor (DAD) organic luminescent dyes of synthesis prepare simple convenient, the gain as miniflow laser Medium forms laser output, while reacting with DNT to be measured causes laser to be quenched, and is quenched by Fabry-Perot cavity (7) amplification It goes out effect, to improve detection sensitivity.
The Fabry-Perot cavity (7) can be made of two panels reflecting mirror disposed in parallel and support construction, reflecting mirror Between clamp microchannel.Compact method cloth can also be realized by plating reflection type medium film in rectangular capillary (6) outer surface In-Perot resonator cavity (7), as shown in Figure 2.
The gathering element (5) includes convergent lens, filter plate, space diaphragm, and light sensing signal is filtered out through space diaphragm Then fluorescence background is focused by convergent lens, through filter plate filtering pump light, then coupled into optical fibres.
The mixed liquor that the sampling pump (9) conveys solution and organic luminescent dyes to be measured passes in and out microchannel, and precision is high, behaviour Make simply, and can be effectively controlled the amount of test sample.
Beneficial effects of the present invention: advanced luminescent material is applied to light miniflow laser, compared with traditional fluorescence sense With apparent advantage.Firstly, since the Fabry-Perot resonance structure in laser, miniflow laser is more than fluorescence detection method It is sensitive.Secondly, laser signal has narrower line width and better directionality, can be filtered by space when so collecting detection light The methods of wave, optical electivity filter out the interference of fluorescence background well.Third, the intensity of light miniflow laser are higher than fluorescence intensity several A order of magnitude is, it can be achieved that bigger detection range.Meanwhile the highly sensitive smooth miniflow explosive detector of the present invention is integrated with luminous increasing Beneficial material, optical resonantor and microchannel realize the on piece explosives sensor of small size.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of smooth miniflow explosive detector provided by the invention.
Fig. 2 is the sectional view of the different Fabry-Perot cavities of smooth miniflow explosive detector provided by the invention.
Fig. 3 is the organic luminescent dyes molecular structure of smooth miniflow explosive detector provided by the invention.
Fig. 4 is the miniflow laser threshold curve of smooth miniflow explosive detector provided by the invention.
Fig. 5 is the sensing curve about explosive DNT of smooth miniflow explosive detector provided by the invention.
Wherein, (1): pulse laser, (2): transmissibility of adjustable attenuation piece, (3): convergent lens, (4): (5): reflecting mirror collects member Part, (6): rectangular capillary, (7): Fabry-Perot cavity, (8): syringe, (9): micro-sampling pump, (10): optical fiber, (11): spectroanalysis instrument, (12): computer.
Specific embodiment
Embodiment 1:
The present embodiment provides a kind of smooth miniflow explosive detectors, including two portions in sample detection part and signal collection Point.The sample detection part includes: pulse laser (1), transmissibility of adjustable attenuation piece (2), convergent lens (3), rectangular capillary (6), Fabry-Perot cavity (7), syringe (8), sampling pump (9).It is connected to by rectangular capillary (6) and two sides Round plastic hose forms microchannel, then rectangular capillary is put into the method amber of two panels reflecting mirror composition together with support construction Between resonant cavity (7), the position of method amber resonant cavity (7) is then adjusted, so that the pulse pump light assembled is incident on method amber resonance It is intracavitary.The signal collection processing unit point includes: gathering element (5), optical fiber (10), spectrometer (11), computer (12).It will receive The laser sensing signal collected is coupled in optical fiber (10), and is transferred in spectrometer along optical fiber (10), records its spectrum.
A kind of production and application method of smooth miniflow explosive detector, specifically includes the following steps:
Step 1: building Fabry-Perot cavity (7)
Two plastic flexible pipes are connected to rectangular capillary (6) both ends, gap ultraviolet glue is filled and solidified, and miniflow is formed Channel.Mechanics amber resonant cavity is arranged by support construction in two panels reflecting mirror, and rectangular capillary is placed in method amber resonant cavity.It can also Compact Fabry-Perot cavity (7) are realized by plating reflection type medium film in rectangular capillary (6) outer surface, such as Fig. 2 It is shown
Step 2: weighing the powder of 5mg organic luminescent dyes, alcohol is added, be uniformly mixed, prepare 0.5mM organic light emission dye Expect alcoholic solution.
Step 3: plastic flexible pipe one being connected empty syringe, other end is submerged equipped with 0.5mM organic luminescent dyes In the centrifuge tube of alcoholic solution.Micro-sampling pump parameter: sucking 20 μ L/min of rate is set again.
Step 4: opening pulse laser, adjust transmissibility of adjustable attenuation piece, the energy of the pulse pump light of control pulse output exists 4.5μJ。
Step 5: opening spectrometer and computer, record the shoot laser spectrum of organic luminescent dyes.
Step 6: increasing the energy of pulse pump light, repeat experimental procedure 8-12 times of above-mentioned 4-5.
Step 7: will be removed equipped with the syringe of waste liquid after spectra re-recorded, changing another, to fill spirituous syringe past It is passed through alcohol in microchannel about 4~5 minutes, guarantees the clean of channel.The spectrum of record is handled again, demarcates organic hair The threshold curve of photoinitiator dye, as shown in Figure 4.
Embodiment 2:
This implementation further limits on the basis of embodiment 1, provides the DNT calibration curve measurement method of detection.
DNT detection calibration curve measurement method specifically includes the following steps:
Step 1: plastic flexible pipe one being connected empty syringe, other end is submerged equipped with DNT to be measured and organic light emission dye In the centrifuge tube of the mixed liquor of material.Sampling pump parameter is set again: sucking 20 μ L/min of rate.
Step 2: opening pump laser, adjust transmissibility of adjustable attenuation piece, keep the pulse pump light energy of output constant, be to have The energy of the best luminous intensity out of machine luminescent dye.
Step 3: opening spectroanalysis instrument and computer, record the shoot laser spectrum of mixed liquor.
Step 4: will be removed equipped with the syringe of waste liquid after spectra re-recorded, changing another, to fill spirituous syringe past It is passed through alcohol in microchannel about 4~5 minutes, guarantees the clean of channel.
Step 5: changing the concentration of DNT in mixed liquor, repeat experimental procedure 8-12 times of above-mentioned 1-4, then remember to spectrometer The spectrum of record is integrated, and integrated intensity is calculated, and draws the calibration curve of DNT detection, as shown in Figure 5.
Embodiment 3:
This implementation further limits on the basis of embodiment 2, provides DNT concentration measuring method in actual sample.
DNT concentration measuring method in actual sample specifically includes the following steps:
Step 1: plastic flexible pipe one being connected empty syringe, other end is submerged equipped with DNT to be measured and organic light emission dye In the centrifuge tube of the mixed liquor of material.Sampling pump parameter is set: sucking 20 μ L/min of rate.
Step 2: opening pump laser, adjust transmissibility of adjustable attenuation piece, make the pulse pump light energy measurement DNT mark of output Determine energy when curve.
Step 3: opening spectroanalysis instrument and computer, record the shoot laser spectrum of mixed liquor.
Step 4: will be removed equipped with the syringe of waste liquid after spectra re-recorded, changing another, to fill spirituous syringe past It is passed through alcohol in microchannel about 4~5 minutes, guarantees the clean of channel.
Step 5: the spectrum of spectrometer record being integrated, integrated intensity, and the calibration curve phase with DNT detection are calculated Compare, the specific concentration of practical DNT solution can be obtained.

Claims (8)

1. a kind of smooth miniflow explosive detector, including sample detection part and signal collection part;
Sample detection part includes: pulse laser (1), convergent lens (3), reflecting mirror (4), microchannel (6), Fabry- Perot resonator cavity (7), syringe (8), sampling pump (9);
The pulse laser (1) provides pump energy, exports pulse pump light, concentrated lens and reflecting mirror are radiated at method cloth In-Perot resonator cavity on;
The Fabry-Perot cavity (7) includes upper and lower two pieces of reflecting mirrors disposed in parallel, and resonant cavity is that miniflow laser mentions It is fed back for light, and makes miniflow laser multiple reflections back and forth in resonant cavity;
The microchannel includes the round plastic hose of rectangular capillary and its two sides, wherein rectangular capillary is placed in humorous It shakes intracavitary;
The syringe (8) and sampling pump (9) pass in and out miniflow with the mixed liquor at the uniform velocity conveying organic luminescent dyes and solution to be measured Channel;
After the pulse pump light is incident in method amber resonant cavity, organic luminescent dyes molecule absorption pulse pump light energy, hair Raw stimulated radiation generates the output of laser sensing signal;
Signal collection processing unit point includes: gathering element (5), optical fiber (10), spectrometer (11), computer (12);
The laser sensing signal being collected into is coupled in optical fiber (10) by the gathering element (5), and laser sensing signal is along optical fiber (10) it is transferred to spectrometer, spectrometer (11) handles laser signal, and processing result is output to computer (12).
2. a kind of smooth miniflow explosive detector as described in claim 1, it is characterised in that: Fabry-Perot cavity (7) Two reflecting mirrors between be provided with support construction.
3. a kind of smooth miniflow explosive detector as described in claim 1, it is characterised in that: the Fabry-Perot resonance Chamber (7) is realized by plating reflection type medium film in rectangular capillary (6) outer surface.
4. a kind of smooth miniflow explosive detector as described in claim 1, it is characterised in that: the gathering element (5) includes Convergent lens, filter plate, space diaphragm, laser sensing signal filter out fluorescence background through space diaphragm, are then gathered by convergent lens Coke, through filter plate filtering pump light, then coupled into optical fibres.
5. a kind of smooth miniflow explosive detector as described in claim 1, it is characterised in that: the pulse laser (1) with It is provided with transmissibility of adjustable attenuation piece between convergent lens (3), adjusts pulse pump light output energy.
6. a kind of smooth miniflow explosive detector as claimed in claim 5, it is characterised in that: it demarcates organic luminescent dyes Threshold curve method includes following steps:
Step 1: weighing the powder of organic luminescent dyes, alcohol is added, be uniformly mixed, prepare organic luminescent dyes alcoholic solution;
Step 2: plastic flexible pipe one is connected empty syringe, other end submerge equipped with organic luminescent dyes alcoholic solution from In heart pipe;Micro-sampling is set and pumps parameter: sucking 20 μ L/min of rate;
Step 3: opening pulse laser, adjust transmissibility of adjustable attenuation piece, the energy of the pulse pump light of control pulse output is in 4.5 μ J;
Step 4: opening spectrometer and computer, record the shoot laser spectrum of organic luminescent dyes;
Step 5: increasing the energy of pulse pump light, repeat experimental procedure 8-12 times of above-mentioned 3-4;
Step 6: the spectrum of record being handled, the threshold curve of organic luminescent dyes is demarcated.
7. a kind of smooth miniflow explosive detector as claimed in claim 6, it is characterised in that: the calibration of the DNT detection is bent Line measurement method the following steps are included:
Step 1: plastic flexible pipe one being connected empty syringe, other end is submerged equipped with DNT to be measured and organic luminescent dyes In the centrifuge tube of mixed liquor;Sampling pump parameter is set: sucking 20 μ L/min of rate;
Step 2: opening pump laser, adjust transmissibility of adjustable attenuation piece, keeping the pulse pump light energy of output is organic light emission dye The energy of the best luminous intensity out of material;
Step 3: opening spectroanalysis instrument and computer, record the shoot laser spectrum of mixed liquor;
Step 4: the syringe equipped with waste liquid being removed after spectra re-recorded, another is changed and fills spirituous syringe toward miniflow It is passed through alcohol in channel about 4~5 minutes, guarantees the clean of channel;
Step 5: changing the concentration of DNT in mixed liquor, repeat experimental procedure 8-12 times of above-mentioned 1-4, then to spectrometer record Spectrum is integrated, and integrated intensity is calculated, and draws the calibration curve of DNT detection.
8. a kind of smooth miniflow explosive detector as claimed in claim 6, it is characterised in that: DNT is dense in the actual sample Spend measurement method specifically includes the following steps:
Step 1: plastic flexible pipe one being connected empty syringe, other end is submerged equipped with DNT to be measured and organic luminescent dyes In the centrifuge tube of mixed liquor;Sampling pump parameter is set: sucking 20 μ L/min of rate;
Step 2: opening pump laser, adjust transmissibility of adjustable attenuation piece, keep the pulse pump light energy measurement DNT calibration of output bent Energy when line;
Step 3: opening spectroanalysis instrument and computer, record the shoot laser spectrum of mixed liquor;
Step 4: the syringe equipped with waste liquid being removed after spectra re-recorded, another is changed and fills spirituous syringe toward miniflow It is passed through alcohol in channel about 4~5 minutes, guarantees the clean of channel;
Step 5: the spectrum of spectrometer record being integrated, calculates integrated intensity, and compared with the calibration curve of DNT detection Compared with to get the specific concentration for arriving DNT solution.
CN201910171658.1A 2019-03-07 2019-03-07 A kind of highly sensitive smooth miniflow explosive detector Pending CN109900662A (en)

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Publication number Priority date Publication date Assignee Title
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