CN211505175U - Device for improving detection sensitivity of long-period grating in non-film coating mode - Google Patents

Device for improving detection sensitivity of long-period grating in non-film coating mode Download PDF

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CN211505175U
CN211505175U CN201922299750.4U CN201922299750U CN211505175U CN 211505175 U CN211505175 U CN 211505175U CN 201922299750 U CN201922299750 U CN 201922299750U CN 211505175 U CN211505175 U CN 211505175U
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long
liquid
period grating
pool
peristaltic pump
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李秋顺
史建国
杨艳
孟庆军
蔡雷
刘庆艾
王丙莲
马耀宏
杨俊慧
朱思荣
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Biology Institute of Shandong Academy of Sciences
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Biology Institute of Shandong Academy of Sciences
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Abstract

The utility model discloses a device for improving the detection sensitivity of a long-period grating in a non-film coating mode, which comprises a liquid mixing pool, a testing pool, a fiber laser and a spectrum analyzer; the liquid mixing pool is provided with a liquid sample inlet to be detected and a high-refractive-index liquid sample inlet; the testing pool can be communicated with the liquid mixing pool; a temperature control device and a long-period grating are arranged in the test pool; the optical signal sent by the fiber laser is transmitted into the long-period grating through the optical fiber and is transmitted to the spectrum analyzer through the long-period grating. The utility model can directly realize the high-sensitivity detection of low-concentration substances without modifying the surface of the long-period grating, greatly simplify the detection process and the operation process, save the detection cost, and avoid the trouble that the residual liquid to be detected is difficult to wash caused by modifying the film; is suitable for popularization and application in the detection of low-concentration substances.

Description

Device for improving detection sensitivity of long-period grating in non-film coating mode
Technical Field
The utility model relates to an analysis sensing technology field, more specifically the device that says so relates to a non-film formula improves long period grating detectivity.
Background
The concentration of a substance in a solution is an important biochemical parameter in a liquid. By improving the sensitivity of detecting the concentration of the substances in the liquid to be detected, the content of the substances in the liquid can be accurately mastered, so that better guidance is provided for industrial and agricultural production. Therefore, the improvement of the detection sensitivity of the concentration of the substance in the solution to be detected has important significance in the fields of industrial production, environmental monitoring, food detection, clinical examination, drug screening, metallurgical scientific research and the like.
The long-period fiber grating is a passive optical device which is relatively sensitive to the ambient refractive index, and has been directly used for measuring the concentration of substances such as glycerol, sodium chloride, calcium chloride, ethylene glycol, sugar and the like in a solution. The sensitivity of the bare Long-Period grating is limited generally, therefore, some researchers modify the Long-Period grating with nano materials to improve the sensitivity of the Long-Period grating to the environmental medium, for example, the document "Optimization of sensitivity in Long Period Fiber grating deployment" improves the sensitivity of the Long-Period grating to the environmental medium by modifying PDDA +/Poly S-119-film on the surface of the grating, "Enhanced sensitivity of Long Period grating deployment of Long Period grating by selecting-assisted polymer membranes" improves the sensitivity of the Long-Period grating to sucrose solution by modifying PAH/PSS film on the surface of the Long-Period grating, the document "modified sensitivity of Long Period grating deployment of Long Period grating to sucrose solution by modifying PAH/PSS film on the surface of the Long-Period grating," Improved sensitivity of Long Period grating deployment of large Period Fiber grating deployment of polymer membranes "improves the sensitivity of Long Period grating to methanol film on the surface of the PSS film, the document "High-sensitivity optical chemically modulated on-surface-periodic gratings for sub-ppm chemical detection in water" improves the sensitivity of the long-period grating to the chloroform concentration by modifying a thin film on the surface of the grating to modify a polystyrene thin film.
Although the above methods of surface coating with nano-thin films can improve the sensitivity of long-period gratings, these methods have some disadvantages: (1) the coated nano film is easily influenced by factors such as environmental temperature, solution pH value, solvent type, solvent solubility, solvent concentration and the like; (2) the operation process of coating and preparing the nano film is complicated; (3) the film can produce certain adsorption to the determinand, cause the determinand to remain on the film surface, cause the subsequent cleaning to be comparatively difficult, and then influence long period grating to the detection of follow-up material, influence long period grating to repeatability and the stability of material detection. It is therefore necessary to find new means for improving the sensitivity of long period gratings to detect substances.
SUMMERY OF THE UTILITY MODEL
In view of this, the utility model provides a device that long period grating detectivity was improved to non-coating formula need not to decorate the film at long period grating surface, can directly realize detecting the high sensitivity of low concentration material.
In order to achieve the above purpose, the utility model adopts the following technical scheme:
a device for improving the detection sensitivity of a long-period grating in a non-coating mode comprises a liquid mixing pool, a testing pool, a fiber laser and a spectrum analyzer;
the liquid mixing pool is provided with a liquid sample inlet to be detected and a high-refractive-index liquid sample inlet;
the testing pool can be communicated with the liquid mixing pool; a temperature control device and a long-period grating are arranged in the test pool;
the optical signal sent by the fiber laser is transmitted into the long-period grating through the optical fiber and is transmitted to the spectrum analyzer through the long-period grating.
The liquid mixing pool is used for uniformly mixing the liquid to be detected and the high-refractive-index liquid; the testing pool can be communicated with the liquid mixing pool through closeable components such as a pump, a valve and the like, and then the mixed liquid is directly transferred into the testing pool after the liquid is uniformly mixed. The testing pool is internally provided with a long-period grating which is connected between the fiber laser and the spectrum analyzer, the fiber laser is used for providing a light source signal, the long-period grating is used for sensing the physical property change of the mixed liquid, the spectrum analyzer is used for receiving and displaying a spectrum signal, and the detection of the concentration of a substance in the liquid to be detected is realized by analyzing according to spectrum data. Be provided with temperature control device in the test tank, can be used to keep mixed liquid constant temperature, and then make the detection state more stable.
Preferably, a stirring device is arranged in the liquid mixing tank, so that the liquid to be detected and the high-refractive-index liquid are further uniformly mixed.
Preferably, the stirring device is a magnetic stirrer.
Preferably, a first peristaltic pump, a second peristaltic pump and a third peristaltic pump are also included;
pumping the liquid to be detected into a liquid mixing pool through a liquid sample inlet to be detected by a first peristaltic pump;
pumping the high-refractive-index liquid into a liquid mixing pool through a high-refractive-index liquid sample inlet by a second peristaltic pump;
and the third peristaltic pump pumps the mixed liquid in the liquid mixing pool into the testing pool or pumps the tested mixed liquid out of the testing pool.
The peristaltic pump is arranged to automate the detection process and enable the liquid to be detected and the liquid with high refractive index to be mixed more sufficiently and accurately.
Preferably, the temperature control device comprises a thermostatic control device with a temperature sensor, and the temperature of the mixed liquid in the test pool is detected and simultaneously adjusted according to a preset temperature.
According to the technical scheme, the utility model can directly realize the high-sensitivity detection of low-concentration substances without modifying a film on the surface of the long-period grating, thereby greatly simplifying the detection process and the operation process, saving the detection cost and avoiding the trouble that the residual liquid to be detected is difficult to wash due to the modification of the film; is suitable for popularization and application in the detection of low-concentration substances.
Drawings
FIG. 1 is a schematic structural view of the non-film-coated device for improving the detection sensitivity of the long-period grating according to the present invention;
in the figure: 1. the device comprises a first peristaltic pump, a second peristaltic pump, a liquid sample inlet to be detected, a liquid sample inlet with a high refractive index, a liquid mixing pool, a magnetic stirrer, a third peristaltic pump, a fiber laser, a testing pool, a temperature control device, a long-period grating, a fiber analyzer and a liquid sample inlet with a high refractive index, and a fiber laser, wherein the liquid mixing pool comprises 6, a magnetic stirrer, 7, the third peristaltic pump, 8, a fiber laser, 9, the testing pool, 10, a temperature control device.
FIG. 2 shows the response spectrum of a long period grating to a sodium chloride solution before the addition of a high refractive index liquid;
FIG. 3 shows the response spectrum of a long period grating to a sodium chloride solution after addition of 1.42044 of a high refractive index liquid;
FIG. 4 shows the response spectrum of a long period grating to a sodium chloride solution after addition of 1.42789 of a high refractive index liquid;
FIG. 5 shows the response spectrum of a long period grating to a sodium chloride solution after addition of 1.43534 of a high refractive index liquid.
Detailed Description
The technical solutions in the embodiments of the present invention are described below clearly and completely, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention.
Example 1
As shown in figure 1, the device for improving the detection sensitivity of the long-period grating in a non-coating mode comprises a first peristaltic pump 1, a second peristaltic pump 2, a liquid mixing pool 5, a third peristaltic pump 7, a testing pool 9, a fiber laser 8 and a spectrum analyzer 12.
The liquid mixing pool 5 is 10cm long and is provided with a liquid sample inlet 3 to be detected and a high-refractive-index liquid sample inlet 4;
a first peristaltic pump 1 pumps a liquid to be detected into a liquid mixing pool 5 from a liquid sample inlet 3 to be detected;
the second peristaltic pump 2 pumps the high-refractive-index liquid into a liquid mixing pool 5 through a high-refractive-index liquid sample inlet 4;
the third peristaltic pump 7 pumps the mixed liquid in the liquid mixing tank 5 into the testing tank 9 or pumps the tested mixed liquid out of the testing tank 9.
A magnetic stirrer 6 is arranged in the liquid mixing pool 5.
The test cell 9 is provided with a temperature control device 10 and a long-period grating 11.
The temperature control device 10 is used for detecting the temperature of the mixed liquid in the test pool 9 and adjusting the temperature of the mixed liquid according to a preset temperature.
The long-period grating 11 is connected between the fiber laser 8 and the spectrum analyzer 12, and an optical signal emitted by the fiber laser 8 is transmitted into the long-period grating 11 through an optical fiber and is transmitted to the spectrum analyzer 12 through the long-period grating 11.
The refractive index of the high refractive index liquid is equal to or greater than 1.41.
Preferably, the refractive index of the mixed solution of the liquid to be measured and the high refractive index liquid is not less than 1.400 and not more than 1.461. The mixture of the liquid to be detected and the high-refractive-index liquid is physical mixture without chemical reaction.
The detection is carried out by using the device, and the method comprises the following steps:
(1) straightening and fixing the long-period grating 11 in the test pool 9, and cleaning the long-period grating 11;
(2) respectively introducing a liquid to be detected and a high-refractive-index liquid into a liquid mixing pool 5 through a liquid sample inlet to be detected and a high-refractive-index liquid sample inlet by using a first peristaltic pump 1 and a second peristaltic pump 2; under the action of the magnetic stirrer 6, the liquid to be detected and the liquid with high refractive index are fully mixed;
(3) transferring the mixed liquid obtained in the step (2) into a testing pool 9 by using a third peristaltic pump 7, and keeping the mixed liquid at a constant temperature by using a temperature control device in the testing process;
(4) transmitting an optical signal sent by an optical fiber laser 8 into a long-period grating 11 through an optical fiber, receiving and displaying a spectral signal of the long-period grating 11 responding to the liquid to be detected in real time by using an optical spectrum analyzer 12, and analyzing the liquid to be detected according to the spectral signal;
(5) after the test is finished, the mixed liquid is removed from the test pool 9 by using a third peristaltic pump 7;
(6) fully washing the liquid mixing tank 5, the testing tank 9 and the long-period grating 11 arranged in the testing tank 9 by using deionized water through the driving of the first peristaltic pump 1, the second peristaltic pump 2 and the third peristaltic pump 7, and drying by using nitrogen after washing;
(7) and (4) testing the next sample according to the steps (2), (3) and (4).
Example 2
The sodium chloride solution was tested using the apparatus of example 1:
(1) washing the liquid mixing tank, the long-period grating and the testing tank with acetone, ethanol and water in sequence, and cleaning;
(2) under the action of a first peristaltic pump and a second peristaltic pump, 0.1mL of 4% sodium chloride solution and 5mL of 1.42044-refractivity high-refractivity liquid (65% glycerol solution) are injected into a liquid mixing pool, and the two liquids are uniformly mixed in the liquid mixing pool through stirring of a magnetic stirrer;
(3) under the action of a third peristaltic pump, transferring the mixed liquid uniformly mixed in the liquid mixing pool into a testing pool for testing, and keeping the temperature of the mixed liquid at 20 +/-0.1 ℃ in the testing process;
(4) reading and recording the spectrum signal of the long-period grating to the mixed liquid consisting of high-refractive-index liquid with the refractive index of 5mL 1.42044 and 0.1mL sodium chloride solution with the concentration of 4%;
(5) fully washing the liquid mixing tank, the testing tank and the long-period grating by using deionized water, and drying by using nitrogen;
(6) sequentially changing a 4% sodium chloride solution into 8%, 12%, 16%, 20% and 24% sodium chloride solution and water (namely, the concentration of sodium chloride is 0%), and sequentially testing according to the steps (2) to (5);
(7) and (3) processing and analyzing the data: the resonance wavelength shifted within the range of 0-24% sodium chloride concentration is compared to the resonance wavelength shifted before the addition of the high refractive index liquid to obtain the multiple of the increase in detection sensitivity.
Through the spectral data analysis of the sodium chloride mixed liquid with different concentrations, with the aid of the high-refractive-index liquid with the refractive index of 1.42044, when the concentration of sodium chloride is increased from 0% to 24%, the resonant wavelength of the long-period grating is shifted by 16.07nm, as shown in fig. 3. Compared with the method before adding no high-refractive-index liquid (directly using sodium chloride solutions with different concentrations for detection, and the resonance wavelength of the long-period grating is shifted by 7.82nm, as shown in figure 2), the sensitivity of the long-period grating to the sodium chloride solution is improved by 2.05 times.
Example 3
The sodium chloride solution was tested using the apparatus of example 1:
(1) washing the liquid mixing tank, the long-period grating and the testing tank with acetone, ethanol and water in sequence, and cleaning;
(2) under the action of a first peristaltic pump and a second peristaltic pump, 0.1mL of 4% sodium chloride solution and 5mL of 1.42789-refractivity high-refractivity liquid (70% glycerol solution) are injected into a liquid mixing pool, and the two liquids are uniformly mixed in the liquid mixing pool through stirring of a magnetic stirrer;
(3) under the action of a third peristaltic pump, transferring the mixed liquid uniformly mixed in the liquid mixing pool into a testing pool for testing, and keeping the temperature of the mixed liquid at 20 +/-0.1 ℃ in the testing process;
(4) reading and recording the spectrum signal of the long-period grating to the mixed liquid consisting of high-refractive-index liquid with the refractive index of 5mL 1.42789 and 0.1mL sodium chloride solution with the concentration of 4%;
(5) fully washing the liquid mixing tank, the testing tank and the long-period grating by using deionized water, and drying by using nitrogen;
(6) sequentially changing a 4% sodium chloride solution into 8%, 12%, 16%, 20% and 24% sodium chloride solution and water (namely, the concentration of sodium chloride is 0%), and sequentially testing according to the steps (2) to (5);
(7) the data were processed and analyzed in the same manner as in example 2.
Through the spectral data analysis of the sodium chloride mixed liquid with different concentrations, with the aid of the high-refractive-index liquid with the refractive index of 1.42789, when the concentration of sodium chloride is increased from 0% to 24%, the resonant wavelength of the long-period grating is shifted by 28.47nm, as shown in fig. 4. The sensitivity of the long period grating to sodium chloride solution was increased by a factor of 3.64 compared to that before the addition of the high refractive index liquid.
Example 4
The sodium chloride solution was tested using the apparatus of example 1:
(1) washing the liquid mixing tank, the long-period grating and the testing tank with acetone, ethanol and water in sequence, and cleaning;
(2) under the action of a first peristaltic pump and a second peristaltic pump, 0.1mL of 4% sodium chloride solution and 5mL of 1.43534-refractivity high-refractivity liquid (75% glycerol solution) are injected into a liquid mixing pool, and the two liquids are uniformly mixed in the liquid mixing pool through stirring of a magnetic stirrer;
(3) under the action of a third peristaltic pump, transferring the mixed liquid uniformly mixed in the liquid mixing pool into a testing pool for testing, and keeping the temperature of the mixed liquid at 20 +/-0.1 ℃ in the testing process;
(4) reading and recording the spectrum signal of the long-period grating to the mixed liquid consisting of high-refractive-index liquid with the refractive index of 5mL1.43534 and 0.1mL of sodium chloride solution with the concentration of 4%;
(5) fully washing the liquid mixing tank, the testing tank and the long-period grating by using deionized water, and drying by using nitrogen;
(6) changing a 4% sodium chloride solution into 8%, 12%, 16%, 20% and 24% sodium chloride solution and water (namely, the concentration of sodium chloride is 0%), and sequentially testing the mixed liquid of the sodium chloride with the concentration according to the steps (2) to (5);
(7) the data were processed and analyzed in the same manner as in example 2.
Through the spectral data analysis of the sodium chloride mixed liquid with different concentrations, with the aid of the high-refractive-index liquid with the refractive index of 1.43534, when the concentration of sodium chloride is increased from 0% to 24%, the resonance wavelength of the long-period grating is shifted by 60.36nm, and as shown in fig. 5, the sensitivity of the long-period grating to the sodium chloride solution is improved by 7.72 times compared with that before the high-refractive-index liquid is not added.
The general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.

Claims (5)

1. A device for improving the detection sensitivity of a long-period grating in a non-coating mode is characterized by comprising a liquid mixing pool, a testing pool, a fiber laser and a spectrum analyzer;
the liquid mixing pool is provided with a liquid sample inlet to be detected and a high-refractive-index liquid sample inlet;
the testing tank can be communicated with the liquid mixing tank; a temperature control device and a long-period grating are arranged in the test pool;
and optical signals sent by the optical fiber laser are transmitted into the long-period grating through optical fibers and are transmitted to the spectrum analyzer through the long-period grating.
2. The device for improving the detection sensitivity of the long-period grating in the non-coating mode according to claim 1, wherein a stirring device is installed in the liquid mixing tank.
3. The device for improving the detection sensitivity of a long-period grating in an uncoated mode according to claim 2, wherein the stirring device is a magnetic stirrer.
4. The device for improving the detection sensitivity of the long-period grating in the non-film coating mode according to claim 1, further comprising a first peristaltic pump, a second peristaltic pump and a third peristaltic pump;
the first peristaltic pump pumps the liquid to be detected into the liquid mixing pool through the liquid sample inlet to be detected;
the second peristaltic pump pumps the high-refractive-index liquid into the liquid mixing pool through the high-refractive-index liquid sample inlet;
the third peristaltic pump pumps the mixed liquid in the liquid mixing pool into the testing pool or pumps the tested mixed liquid out of the testing pool.
5. The apparatus according to claim 1, wherein the temperature control means comprises a thermostat control means having a temperature sensor.
CN201922299750.4U 2019-12-19 2019-12-19 Device for improving detection sensitivity of long-period grating in non-film coating mode Active CN211505175U (en)

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