CN114518349A - Method for nondestructive online detection of iodine vapor - Google Patents
Method for nondestructive online detection of iodine vapor Download PDFInfo
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- CN114518349A CN114518349A CN202210153728.2A CN202210153728A CN114518349A CN 114518349 A CN114518349 A CN 114518349A CN 202210153728 A CN202210153728 A CN 202210153728A CN 114518349 A CN114518349 A CN 114518349A
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- 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
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- G01N21/6402—Atomic fluorescence; Laser induced fluorescence
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Abstract
The invention relates to a method for nondestructive online detection of iodine vapor. The method is carried out by adopting an online optical detection system, a capillary tube containing a PIM-1 film is arranged on a scanning table, two ends of the capillary tube containing the PIM-1 film are connected with a gas path, the gas flow rate is adjusted by adjusting a peristaltic pump, clean air is firstly introduced into the gas path, the capillary tube is swept by the clean air, a high-intensity fluorescence signal reaches a stable baseline, then a gas port is switched to iodine steam, the iodine steam is introduced into the capillary tube, the fluorescence signal is rapidly quenched, the real-time fluorescence intensity of the PIM-1 film is obtained, and the nondestructive online detection of the iodine steam is realized. The method can detect the content of iodine vapor on line in real time, and has the advantages of high detection sensitivity, quick response time and high repeated utilization rate.
Description
Technical Field
The invention relates to a method for nondestructive online detection of iodine vapor, and belongs to the technical field of iodine detection.
Background
With the rapid increase of energy demand, nuclear power is receiving more and more attention and exploitation, but there is the generation and release of nuclear waste, of which iodine radioisotopes (129I and 131I) are one of the most likely released fission gases in nuclear fuel reprocessing plants, with great impact on human beings and the surrounding environment. One isotope 129I has a half-life of about 1700 ten thousand years and high fluidity, and can cause long-term pollution to the environment, and the other isotope 131I has a short half-life of about 8 days and high activity, can enter the human metabolic process through the food chain, influence the human metabolic process, and even cause cancers. Therefore, the research on the detection method of the iodine vapor is very important, so that early warning can be given in time, and the life and property safety of people can be guaranteed.
At present, some iodine vapor detection methods are developed, such as an iodine-starch color development method, the characteristic that iodine turns starch blue is utilized, the operation is simple, the reaction is sensitive, but the reproducibility is poor; a catalytic reaction method, which utilizes iodine to play a catalytic role in certain fading reactions, has good detection reproducibility and accurate measurement result, but has the problems of troublesome operation steps, incapability of recycling and the like; the electrochemical method is simple and accurate to operate, but the operation is long in time consumption and complicated; the plasma mass spectrometry is used for detecting the iodine vapor content according to the charge-to-mass ratio, has the advantages of low detection limit, high sensitivity and the like, but is difficult to operate and use on a large scale due to high cost.
The fluorescence detection utilizes iodine to enable the material with fluorescence property to generate a quenching mechanism, has the advantages of high sensitivity, good repeatability, small influence from the outside and the like, and can effectively detect the content of iodine vapor. For example, the document Dalton trans.2020,49,16623-16626 reports an MOF material used for iodine detection after preparation of MIL-53(Al) -TDC material, and the feasibility of fluorescence detection of iodine is proved by the drastic change of the fluorescence spectrum.
At present, after materials and iodine are mixed and reacted, a fluorescence spectrophotometer is used for measuring a fluorescence spectrum, the fluorescence intensity of the fluorescence spectrum is recorded, then the fluorescence detection is carried out, and the operation is complex, so that the online detection cannot be realized.
Therefore, there is a need to develop a method for nondestructive online detection of iodine vapor.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for nondestructively detecting iodine vapor on line. The method can detect the content of iodine vapor on line in real time, and has the advantages of high detection sensitivity, quick response time and high repeated utilization rate.
The invention is realized by the following technical scheme:
a method for nondestructive online detection of iodine vapor is carried out by adopting an online optical detection system and comprises the following steps:
(1) placing the PIM-1 membrane and excessive iodine solid in a closed system, contacting at room temperature, respectively testing fluorescence spectra of the PIM-1 membrane before and after iodine contact by using a fluorescence spectrophotometer, and determining the maximum excitation wavelength and the maximum fluorescence emission wavelength of the PIM-1 membrane by repeating excitation-emission operation;
(2) setting up an online optical detection system, which comprises:
the laser adopts a blue Light Emitting Diode (LED), and the emitted light is an excitation light source;
Reversely exciting the dichroic mirror;
the optical microscopic magnification objective lens is used for amplifying and imaging optical signals;
mirror oil for matching the refractive index of the high numerical aperture oil mirror;
a slide glass for absorbing the excitation light to generate a surface plasmon resonance phenomenon;
a scanning platform for placing a capillary tube containing a PIM-1 membrane;
n pieces of filter plates are arranged on the surface of the substrate,
a condenser lens and a photoelectric tube;
the light emitted by the laser irradiates the capillary tube containing the PIM-1 film through the reverse excitation dichroic beam splitter, the objective lens, the mirror oil and the glass slide, the reflected light of the sample to be detected in the capillary tube sequentially passes through the reverse excitation dichroic beam splitter, the N filters and the condenser lens to enter the photoelectric tube, and the photoelectric tube converts the optical signal into an electric signal and inputs the electric signal into the software processing module;
(3) placing the capillary tube containing the PIM-1 film on a scanning table, connecting two ends of the capillary tube containing the PIM-1 film with gas circuits, arranging peristaltic pumps on the gas circuits, adjusting the gas flow rate by adjusting the peristaltic pumps,
(4) firstly, introducing clean air into a gas path, blowing the capillary tube with the clean air to obtain a stable baseline of a high-intensity fluorescence signal, then switching a gas port to iodine steam, introducing the iodine steam into the capillary tube, rapidly quenching the fluorescence signal to obtain the real-time fluorescence intensity of the PIM-1 film, and realizing the nondestructive online detection of the iodine steam.
Preferably, in step (1), the PIM-1 membrane is prepared as follows:
under inert atmosphere, adding tetrafluoroterephthalonitrile (TFTPN), 5',6,6' -tetrahydroxy-3, 3,3',3' -tetramethyl-1, 1' -spirobiindane (TTSBI) into Dimethylacetamide (DMAC), and then adding potassium carbonate, toluene and crown ether to obtain a mixture; and (2) carrying out reflux reaction on the mixture at 160 ℃ to obtain a viscous solution, adding the viscous solution into methanol to obtain a yellow polymer, adding the yellow polymer into chloroform and methanol for purification, then carrying out reflux washing on the yellow polymer by deionized water, and carrying out vacuum drying to obtain self-micropore polymer powder: dissolving the polymer powder with micropores in chloroform, naturally volatilizing to form a membrane, soaking the membrane in methanol, and drying in vacuum to obtain the membrane-shaped polymer with micropores (PIM-1 membrane).
Further preferably, the molar ratio of tetrafluoroterephthalonitrile (TFTPN), 5',6,6' -tetrahydroxy-3, 3,3',3' -tetramethyl-1, 1' -spirobiindane (TTSBI), Dimethylacetamide (DMAC), potassium carbonate, toluene and crown ether is 1:1:19.3:3: 0.1: 0.05.
the drying of the potassium carbonate and the addition of the crown ether are beneficial to improving the molecular weight of the polymer with micropores, thereby being more beneficial to film formation.
Further preferably, the mass ratio of the polymer powder with micropores to the chloroform is 1: 50.
Preferably, in step (1), the PIM-1 membrane has a maximum excitation wavelength of 480nm and a maximum fluorescence emission wavelength of 520 nm.
Preferably, in step (1), the PIM-1 membrane is contacted with the excess iodine solid for a period of 4 to 8 min.
According to the invention, in the step (2), a hollowed hole is arranged on the scanning table, and the capillary tube containing the PIM-1 film is embedded in the hollowed hole.
Preferably, in step (2), the filter is a 488nm filter and a 532nm filter.
According to the invention, in the step (3), the capillary tube containing the PIM-1 film is prepared by the following method:
the glass capillary was washed with methanol and dried, and then filled with a PIM-1-chloroform solution, and the solvent was slowly evaporated at room temperature, so that the PIM-1 material was tightly attached to the inner surface of the capillary in the form of a thin film, resulting in a capillary containing a PIM-1 thin film.
More preferably, the PIM-1-chloroform solution is a mixture of a polymer powder having micropores and chloroform, and the mass ratio of the polymer powder having micropores to the chloroform is 1: 50.
Further preferably, the glass capillary has an inner diameter of 0.2 to 0.5mm and a length of 80 to 120 mm.
Preferably, according to the invention, in step (3), the peristaltic pump has a flow rate of 25 to 35 mL/min.
The invention has the technical characteristics and advantages that:
1. the method can detect the content of iodine vapor on line, and has the advantages of high detection sensitivity, quick response time and high repeated utilization rate.
2. The method has high sensitivity for detecting iodine vapor and quick response time, and the change value of the fluorescence intensity of the iodine vapor only contacts with the iodine for 5min at room temperature is more than 50 percent
3. The method has good repeatability and high utilization rate for iodine vapor fluorescence detection.
Drawings
FIG. 1 is a schematic representation of a PIM-1 film and a capillary tube comprising the PIM-1 film, a being the PIM-1 film and b being the capillary tube comprising the PIM-1 film;
FIG. 2 is a graph showing fluorescence spectra of a PIM-1 film before and after contact with iodine;
FIG. 3 is a schematic diagram of an on-line optical inspection system;
FIG. 4 is a pictorial view of an on-line optical inspection system;
FIG. 5 is a graph showing the on-line monitoring of iodine vapor cycle by capillary tube with PIM-1 film in the examples.
Detailed description of the preferred embodiments
The present invention will be further described with reference to the following detailed description of embodiments thereof, but not limited thereto, in conjunction with the accompanying drawings.
The raw materials used in the examples were all conventional commercially available products unless otherwise specified.
EXAMPLE 1 preparation of PIM-1 Material
Tetrafluoroterephthalonitrile (2.001g, 0.01mol) and 5,5',6,6' -tetrahydroxy-3, 3,3',3' -tetramethylspirobiindane (3.404g, 0.01mol), anhydrous potassium carbonate (4.14g, 0.03mol), dimethylacetamide (20mL), toluene (10mL) and a small amount of crown ether were added to a 100mL three-necked flask equipped with a magnetic stirrer, argon inlet and a water trap. The mixture was then refluxed at 160 ℃ for 40min, yielding a viscous solution, which was poured into methanol to yield a yellow, flexible linear polymer. The polymer product was dissolved in chloroform and precipitated from methanol for further purification, which was repeated three times, and finally the resulting polymer was refluxed with deionized water for 6h and vacuum dried at 100 ℃ for 48h to give PIM-1 powder.
EXAMPLE 2PIM-1 film preparation
0.1g of the PIM-1 powder obtained in example 1 and 5g of a chloroform solution were weighed, poured into a flat-bottomed polytetrafluoroethylene dish (diameter: 10cm), and naturally evaporated at room temperature to form a film, and after the solvent was completely evaporated, the obtained PIM-1 film was further immersed in methanol for 12 hours and then vacuum-dried at 100 ℃ for 24 hours to obtain a PIM-1 thin film. As shown in fig. 1 a.
EXAMPLE 3 capillary preparation of PIM-1-containing films
A glass capillary (inner diameter 0.3mm, length 100mm) was first washed with methanol and dried, then filled with a PIM-1/chloroform solution (2 wt%) by siphoning, and the solvent was slowly evaporated at room temperature to allow the PIM-1 material to adhere tightly to the inner surface of the capillary in the form of a thin film, as shown in FIG. 1 b.
EXAMPLE 4PIM-1 film off-line fluorescence detection of iodine vapor
The fluorescence spectrum of the PIM-1 membrane is tested by using a fluorescence spectrophotometer, and the maximum excitation wavelength and the maximum fluorescence emission wavelength of the fluorescence spectrum are determined to be 480nm and 520nm respectively through repeated excitation-emission operation, and the corresponding fluorescence intensity is 8.4 multiplied by 10^5, thereby proving that the PIM-1 has high self-fluorescence intensity. The PIM-1 membrane and excess iodine solid were placed in a closed system and kept at room temperature for 5min, and the fluorescence spectrum was measured using a fluorescence spectrophotometer, corresponding to a fluorescence intensity of 4.1X 10^4, as shown in FIG. 2. The PIM-1 film is contacted with iodine vapor for 5min, the fluorescence intensity is reduced to 48% of the initial intensity, and the advantages of quick response time and high sensitivity to the iodine vapor are shown.
Example 5 a method for non-destructive online detection of iodine vapor comprising the steps of:
(1) setting up an on-line optical detection system, which comprises:
the laser adopts a blue Light Emitting Diode (LED), and the emitted light is an excitation light source;
reversely exciting the dichroic beam splitter;
the optical microscopic magnification objective lens is used for amplifying and imaging optical signals;
mirror oil for matching the refractive index of the high numerical aperture oil mirror;
a slide glass for absorbing the excitation light to generate a surface plasmon resonance phenomenon;
A scanning table for placing a capillary tube containing a PIM-1 film;
n filter-plates are arranged on the substrate,
a condenser lens and a photoelectric tube;
the light emitted by the laser irradiates the capillary tube containing the PIM-1 film through the reverse excitation dichroic beam splitter, the objective lens, the mirror oil and the glass slide, the reflected light of the sample to be detected in the capillary tube sequentially passes through the reverse excitation dichroic beam splitter, the N filters and the condenser lens to enter the photoelectric tube, and the photoelectric tube converts the optical signal into an electric signal and inputs the electric signal into the software processing module;
(2) placing a capillary tube containing a PIM-1 film on a scanning table to be detected, connecting two ends of the capillary tube containing the PIM-1 film with gas paths, arranging a peristaltic pump on the gas paths, and adjusting the flow rate of gas by adjusting the peristaltic pump, wherein the flow rate of the peristaltic pump is 30 mL/min;
(3) the capillary was first purged with clean air to reach a stable baseline, and then the air port was switched to iodine vapor. As shown in fig. 5, when clean air passes through the duct at a flow rate of 30mL/min, a high intensity fluorescence signal is obtained, and when the passing gas is switched to iodine vapor, quenching of the fluorescence signal rapidly occurs after a 30s dead time. The fluorescence intensity continued to decrease at a rate of about 15% per minute for the first 3min, and after 4min with iodine-containing air, the fluorescence intensity decreased to 45% of the initial intensity. When the purge gas was switched back to clean air, desorption of iodine occurred and the PIM-1 film recovered the initial fluorescence intensity after 2 h. Although a decrease in fluorescence intensity was observed after two cycles, which may be due to degradation of the polymer under prolonged laser irradiation (burning spots can be seen on the film under prolonged intense laser irradiation), the capillary containing the PIM-1 film can be used for at least five cycles and has good reproducibility.
Claims (10)
1. A method for nondestructive online detection of iodine vapor is carried out by adopting an online optical detection system, and comprises the following steps:
(1) placing the PIM-1 membrane and excessive iodine solid in a closed system, contacting at room temperature, respectively testing fluorescence spectra of the PIM-1 membrane before and after iodine contact by using a fluorescence spectrophotometer, and determining the maximum excitation wavelength and the maximum fluorescence emission wavelength of the PIM-1 membrane by repeating excitation-emission operation;
(2) setting up an on-line optical detection system, which comprises:
the laser adopts a blue Light Emitting Diode (LED), and the emitted light is an excitation light source;
reversely exciting the dichroic mirror;
the optical microscopic objective lens is used for amplifying and imaging optical signals;
mirror oil for matching the refractive index of the high numerical aperture oil mirror;
a slide glass for absorbing the excitation light to generate a surface plasmon resonance phenomenon;
a scanning platform for placing a capillary tube containing a PIM-1 membrane;
n pieces of filter plates are arranged on the surface of the substrate,
a condenser lens and a photoelectric tube;
the light emitted by the laser irradiates the capillary tube containing the PIM-1 film through the reverse excitation dichroic beam splitter, the objective lens, the mirror oil and the glass slide, the reflected light of the sample to be detected in the capillary tube sequentially passes through the reverse excitation dichroic beam splitter, the N filters and the condenser lens to enter the photoelectric tube, and the photoelectric tube converts the optical signal into an electric signal and inputs the electric signal into the software processing module;
(3) Placing the capillary tube containing the PIM-1 film on a scanning table, connecting two ends of the capillary tube containing the PIM-1 film with gas circuits, arranging peristaltic pumps on the gas circuits, adjusting the gas flow rate by adjusting the peristaltic pumps,
(4) firstly, introducing clean air into a gas path, blowing the capillary tube with the clean air to obtain a stable baseline of a high-intensity fluorescence signal, then switching a gas port to iodine steam, introducing the iodine steam into the capillary tube, rapidly quenching the fluorescence signal to obtain the real-time fluorescence intensity of the PIM-1 film, and realizing the nondestructive online detection of the iodine steam.
2. The method according to claim 1, wherein in step (1), the PIM-1 membrane is prepared as follows:
under inert atmosphere, adding tetrafluoroterephthalonitrile (TFTPN), 5',6,6' -tetrahydroxy-3, 3,3',3' -tetramethyl-1, 1' -spirobiindane (TTSBI) into Dimethylacetamide (DMAC), and then adding potassium carbonate, toluene and crown ether to obtain a mixture; and (2) carrying out reflux reaction on the mixture at 160 ℃ to obtain a viscous solution, adding the viscous solution into methanol to obtain a yellow polymer, adding the yellow polymer into chloroform and methanol for purification, then carrying out reflux washing on the yellow polymer by deionized water, and carrying out vacuum drying to obtain self-micropore polymer powder: dissolving the polymer powder with micropores in chloroform, naturally volatilizing to form a membrane, soaking the membrane in methanol, and drying in vacuum to obtain the membrane-shaped polymer with micropores (PIM-1 membrane).
3. The process of claim 2, wherein the molar ratio of tetrafluoroterephthalonitrile (TFTPN), 5',6,6' -tetrahydroxy-3, 3,3',3' -tetramethyl-1, 1' -spirobiindane (TTSBI), Dimethylacetamide (DMAC), potassium carbonate, toluene and crown ether is 1:1:19.3:3: 0.1: 0.05, and the mass ratio of the polymer powder with micropores to chloroform is 1: 50.
4. The method according to claim 1, wherein in step (1), the PIM-1 membrane has a maximum excitation wavelength of 480nm and a maximum fluorescence emission wavelength of 520 nm.
5. The method of claim 1, wherein in step (1), the PIM-1 membrane is contacted with the excess iodine solid for a period of 4 to 8 min.
6. The method of claim 1, wherein in step (2), the scanning platform is provided with a hollow hole, and the capillary tube containing the PIM-1 film is embedded in the hollow hole.
7. The method of claim 1, wherein in step (2), the filters are 488nm filter and 532nm filter.
8. The method according to claim 1, wherein in step (3), the capillary tube containing the PIM-1 film is prepared by the following method:
the glass capillary was washed with methanol and dried, and then filled with a PIM-1-chloroform solution, and the solvent was slowly evaporated at room temperature, so that the PIM-1 material was tightly attached to the inner surface of the capillary in the form of a thin film, resulting in a capillary containing a PIM-1 thin film.
9. The method according to claim 1, wherein the PIM-1-chloroform solution is a mixture of a polymer powder having fine pores and chloroform, the mass ratio of the polymer powder having fine pores to the chloroform is 1:50, the inner diameter of the glass capillary is 0.2 to 0.5mm, and the length thereof is 80 to 120 mm.
10. The method according to claim 1, wherein in the step (3), the flow rate of the peristaltic pump is 25 to 35 mL/min.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115096960A (en) * | 2022-06-24 | 2022-09-23 | 山东大学 | High-selectivity and high-sensitivity iodine vapor electrochemical impedance sensor and construction method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115096960A (en) * | 2022-06-24 | 2022-09-23 | 山东大学 | High-selectivity and high-sensitivity iodine vapor electrochemical impedance sensor and construction method thereof |
| CN115096960B (en) * | 2022-06-24 | 2023-08-11 | 山东大学 | High-selectivity high-sensitivity iodine vapor electrochemical impedance sensor and construction method thereof |
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