CN114199824A - Preparation method for detecting pH value LPFG - Google Patents
Preparation method for detecting pH value LPFG Download PDFInfo
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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
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/41—Refractivity; Phase-affecting properties, e.g. optical path length
Abstract
The invention provides a preparation method for detecting a pH value LPFG, and belongs to the technical field of long-period fiber bragg grating detection. The specific method is that firstly, the sodium polystyrene sulfonate and the titanium dioxide film are assembled on the surface of the long-period grating, the LPFG is modulated to be in the optimal refractive index sensitivity area, and then the hyaluronic acid and the polyallylamine hydrochloride film are further assembled on the surface of the LPFG, so that the LPFG with good response to the pH value is prepared. The modification of the nano film greatly improves the distinguishing and identifying capability of LPFG on different pH values, can play a unique advantage in the pH value detection in severe environment, particularly in the environment where manual contact and operation are difficult, and is expected to be applied in various fields such as environment, biological engineering, chemistry, clinic and the like.
Description
Technical Field
The invention belongs to the technical field of long-period fiber grating detection, and particularly relates to a preparation method for detecting a pH value LPFG.
Background
The pH value is one of important physicochemical parameters of the aqueous solution and is the most important water chemistry inspection index. The pH value is required to be measured in various fields such as industry, agriculture, medicine, environmental protection, scientific research and the like, for example, the pH detection of meat can be used for judging the storage life and the meat property of meat; by measuring the pH value of the urine, whether the human body has the acidification tendency can be judged; in the water treatment process, the clarification and disinfection process can be optimized by controlling the pH value; the corrosion of the water distribution system to a pipe network can be reduced to the minimum degree by controlling the pH value; through the detection of the pH value of the paper, the quality of the printed matter can be judged in advance, and the pH value of the fountain solution can be adjusted. Therefore, the detection of the pH value has important significance.
Long Period Fiber Grating (LPFG) is a typical passive optical sensing device sensitive to environmental changes, and has the advantages of small fiber volume, electromagnetic interference resistance, capability of transmitting signals in a long distance, and the like, and also has the performance of being sensitive to the surrounding environment, so in recent years, LPFG has received wide attention and is widely applied to fiber communication and fiber sensing systems. For example, a simultaneous measurement sensor for refractive index and temperature of LPFG and coreless fiber cascade, published by photoelectron laser 2021.32(08), which is a joint work of ceramic force and river surpass, uses a long-period fiber grating for simultaneous measurement of refractive index and temperature; piezoelectric and acousto-optic 2021, published a long period fiber grating glucose sensor applied to human body environment, which is a treatise of zhang shi and jiangchao, and long period fiber grating is used for strain bending detection; the optical science newspaper 2020,40(18) discloses an immunosensor of graphene oxide coated gold nanoshell modified long-period optical grating, which is prepared by Shishenghi, Wudezhao and the like, and the long-period optical fiber grating is used for detecting avian influenza virus; optical Communications 2004.229(1-6) published journal Hin Chong, Ping Shum, et al, measurement of sensitive use of long-period grating, and long-period fiber grating was used for the measurement of ethylene glycol, sucrose, and salt concentrations (9.09% -23.08%).
The long-period grating is resistant to acid and alkali corrosion, and if the long-period grating is used for detecting the pH value of a solution, the long-period grating can play a unique advantage in a severe environment, particularly an environment which is not easy to contact and operate manually. However, bare long period gratings are generally insensitive to pH variations and it is difficult to distinguish between solutions of different pH values. Therefore, it is necessary to find a new method for detecting pH by using a long-period grating.
Disclosure of Invention
In view of the above, the present invention provides a preparation method for detecting the pH LPFG, which is low in operation cost, does not require harsh conditions, and is operable under room temperature and normal pressure environment conditions.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method for detecting a pH value LPFG comprises the following steps:
(1) respectively preparing a poly (diallyldimethylammonium chloride) solution, a sodium polystyrene sulfonate solution, a titanium dioxide solution, a hyaluronic acid solution and a poly (allylamine hydrochloride) solution for later use;
(2) straightening the long-period grating LPFG and fixing the long-period grating LPFG in a liquid pool by using a clamp;
(3) cleaning the long-period grating area;
(4) adding a poly (diallyldimethylammonium chloride) solution into a liquid pool, and assembling a poly (diallyldimethylammonium chloride) film on the surface of the long-period grating region;
(5) fully flushing the long-period grating area with distilled water, and drying by using nitrogen;
(6) adding a sodium polystyrene sulfonate solution into a liquid pool, and assembling a sodium polystyrene sulfonate film on the surface of the long-period grating area;
(7) fully flushing the long-period grating area with distilled water, and drying by using nitrogen;
(8) adding a titanium dioxide solution into a liquid pool, and assembling a titanium dioxide film on the surface of the long-period grating area;
(9) fully flushing the long-period grating area with distilled water, and drying by using nitrogen;
(10) repeating the operation steps from (6) to (9) until the long-period grating is in an optimal refractive index sensitive area;
(11) adding a hyaluronic acid solution into a liquid pool, and continuously assembling a hyaluronic acid film on the surface of the titanium dioxide film in the long-period grating area;
(12) fully flushing the long-period grating area with distilled water, and drying by using nitrogen;
(13) adding a hyaluronic acid solution into a liquid pool, and assembling a polyallylamine hydrochloride film on the surface of the long-period grating area;
(14) fully flushing the long-period grating area with distilled water, and drying by using nitrogen;
(15) and (4) repeating the operation steps from (11) to (14) and assembling to the required number of layers to obtain the long-period grating which can be used for detecting the pH value.
Preferably, the polydiallyldimethylammonium chloride solution is prepared by the following method: dissolving poly (diallyldimethylammonium chloride) in water, adding sodium chloride, and stirring to obtain the poly (diallyldimethylammonium chloride) solution; the molar concentration ratio of the poly (diallyldimethylammonium chloride) to the sodium chloride is 1: 0.001-30000.
Preferably, the sodium polystyrene sulfonate solution is prepared by the following method: dissolving sodium polystyrene sulfonate in water, adding sodium chloride, and stirring uniformly to obtain a sodium polystyrene sulfonate solution; the molar concentration ratio of the sodium polystyrene sulfonate to the sodium chloride is 1: 0.001-30000.
Preferably, the concentration of the titanium dioxide solution is 0.0001mg/mL-10 g/mL; the pH value of the titanium dioxide solution is 2.8-5.8; the particle size of the titanium dioxide in the titanium dioxide solution is 0.001-500 mu m.
Preferably, the concentrations of the hyaluronic acid solution and the polyallylamine hydrochloride solution are both 0.0001-0.1mol/L, and the pH values are both 3-10.
Preferably, the hyaluronic acid solution and the polyallylamine hydrochloride solution both contain sodium chloride with the concentration of 0-0.3 mol/L.
Preferably, the assembling on the surface of the long-period grating region in steps (4), (6), (8), (11) and (13) is specifically to perform assembling on the surface of the cladding of the long-period grating region after straightening and fixing.
Preferably, the time for assembling on the surface of the long-period grating region in steps (4), (6), (8), (11) and (13) is 1-30 min.
Preferably, the detection range of the long-period grating in the step (15) on the pH value is 3-10.
In the present invention, the long period grating is in the optimum refractive index sensitive region, which means that there is a very large shift in the resonance wavelength when a double-layer film is assembled.
Through the technical scheme, compared with the prior art, the invention has the following beneficial effects:
1. the long-period grating prepared by the invention improves the distinguishing and identifying capability of LPFG on different pH values;
2. the long-period grating prepared by the invention has the advantages of immunity to electromagnetic fields, tolerance to severe environments, safety of in-vivo pH measurement, long-distance sensing capability and the like, and can play a unique advantage in severe environments, particularly in pH value detection in environments where manual contact and operation are difficult;
3. the long-period grating prepared by the invention can be used for measuring the pH value of a solution in industries such as a power plant, a chemical industry, a fermentation industry, food, metallurgy, pharmacy, environmental protection, biochemistry and tap water, and is expected to be popularized and applied in the fields of environment, bioengineering, chemistry, clinic and the like.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
Fig. 1 is a schematic cross-sectional view of an LPFG fixture according to the present invention.
Wherein, in the figure:
1-long period grating fixing support; 2-a liquid pool; 3-a long period grating region; 4-fixing device screws; 5-optical fiber.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Straightening a long-period grating LPFG (Long period Grating) and fixing the long-period grating in a liquid pool by using a clamp, then cleaning a long-period grating area, further assembling a poly (diallyl dimethyl ammonium chloride) film on the surface of the long-period grating area, fully flushing the long-period grating area by using distilled water, and drying by using nitrogen; assembling a sodium polystyrene sulfonate film on the surface of the long-period grating area, fully flushing the long-period grating area with distilled water, and drying with nitrogen; then assembling a titanium dioxide film on the surface of the long-period grating area, fully flushing the long-period grating area with distilled water, and drying with nitrogen; the procedure of assembling the sodium polystyrene sulfonate/titanium dioxide film is repeated until the long-period grating is in the optimal refractive index sensitive area. Continuously assembling a hyaluronic acid film on the surface of the titanium dioxide film in the long-period grating area, fully washing the long-period grating area with distilled water, and drying with nitrogen; then assembling a polyallylamine hydrochloride film on the surface of the long-period grating area, fully flushing the long-period grating area with distilled water, and drying with nitrogen; and repeating the operation steps of assembling the hyaluronic acid/polyallylamine hydrochloride to the required number of layers to obtain the long-period grating for detecting the pH value.
Example 2
0.236g of polydiallyldimethylammonium chloride with molecular weight of 100000 is dissolved in 100ml of water, then 5.844g of sodium chloride is added, and the mixture is stirred uniformly, thus obtaining polydiallyldimethylammonium chloride solution. Then 0.287g of sodium polystyrene sulfonate with the molecular weight of 100000 is dissolved in 100ml of water, and then 5.844g of sodium chloride is added and stirred uniformly, thus obtaining the sodium polystyrene sulfonate solution. 0.3g of titanium dioxide having a particle size of 300 μm was dissolved in 300ml of water, and stirred uniformly to prepare a titanium dioxide solution. Polyallylamine hydrochloride solution was prepared by dissolving 18.71mg of polyallylamine hydrochloride in 100ml of water, followed by addition of 5.8mg of sodium chloride and stirring well. Hyaluronic acid solution was prepared by dissolving 80.66mg of hyaluronic acid in 100ml of water, followed by adding 6mg of sodium chloride, and stirring well. Adding the prepared poly (diallyldimethylammonium chloride) solution into a reaction tank with a fixed long-period grating, standing for 10 minutes, then fully washing with water, and drying with nitrogen. The prepared sodium polystyrene sulfonate solution was then added, allowed to stand for 10 minutes, then thoroughly rinsed with water and blown dry with nitrogen. Then adding the prepared titanium dioxide solution, standing for 10 minutes, then fully washing with water, and drying by using nitrogen. And (3) adding a sodium polystyrene sulfonate solution or a titanium dioxide solution in sequence according to the steps, and assembling to a sensitive area which enables the long-period grating to be in the best birefringence. The formulated hyaluronic acid solution was then added, allowed to stand for 10 minutes, then thoroughly rinsed with water and blown dry with nitrogen. The prepared polyallylamine hydrochloride solution is added again, the mixture is kept still for 10 minutes, and then the mixture is fully washed by water and dried by nitrogen. And repeating the steps, alternately and repeatedly adding the hyaluronic acid solution or the polyallylamine hydrochloride solution, and assembling 20 layers of hyaluronic acid/polyallylamine hydrochloride nano films to obtain the long-period grating with good response to pH.
Example 3
0.118g of poly (diallyldimethylammonium chloride) with the molecular weight of 100000 is dissolved in 100ml of water, then 1.461g of sodium chloride is added, and the mixture is stirred evenly, thus obtaining the poly (diallyldimethylammonium chloride) solution. Then 0.144g of polystyrene sodium sulfonate with the molecular weight of 100000 is dissolved in 100ml of water, and then 1.461g of sodium chloride is added and stirred evenly, thus obtaining the polystyrene sodium sulfonate solution. 0.4g of titanium dioxide with the particle size of 20nm is dissolved in 200ml of water and stirred uniformly to prepare a titanium dioxide solution. Polyallylamine hydrochloride solution was prepared by dissolving 400mg of polyallylamine hydrochloride in 200ml of water followed by addition of 20mg of sodium chloride and stirring well. 200mg of hyaluronic acid is dissolved in 200ml of water, and then 18mg of sodium chloride is added and stirred uniformly to prepare a hyaluronic acid solution. Adding the prepared poly (diallyldimethylammonium chloride) solution into a reaction tank with a fixed long-period grating, standing for 10 minutes, then fully washing with water, and drying with nitrogen. The prepared sodium polystyrene sulfonate solution was then added, allowed to stand for 20 minutes, then thoroughly rinsed with water and blown dry with nitrogen. Then adding the prepared titanium dioxide solution, standing for 20 minutes, then fully washing with water, and drying by using nitrogen. And (3) adding a sodium polystyrene sulfonate solution or a titanium dioxide solution in sequence according to the steps, and assembling to a sensitive area which enables the long-period grating to be in the best birefringence. The formulated hyaluronic acid solution was then added, allowed to stand for 20 minutes, then rinsed thoroughly with water and blown dry with nitrogen. The prepared polyallylamine hydrochloride solution is added again, the mixture is kept still for 20 minutes, and then the mixture is fully washed by water and dried by nitrogen. And repeating the steps, alternately and repeatedly adding the hyaluronic acid solution or the polyallylamine hydrochloride solution, and assembling 40 layers of the hyaluronic acid/polyallylamine hydrochloride nano films to obtain the long-period grating with good response to pH.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. The device disclosed by the embodiment corresponds to the method disclosed by the embodiment, so that the description is simple, and the relevant points can be referred to the method part for description.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to 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 (9)
1. A preparation method for detecting a pH value LPFG is characterized by comprising the following steps:
(1) respectively preparing a poly (diallyldimethylammonium chloride) solution, a sodium polystyrene sulfonate solution, a titanium dioxide solution, a hyaluronic acid solution and a poly (allylamine hydrochloride) solution for later use;
(2) straightening the long-period grating LPFG and fixing the long-period grating LPFG in a liquid pool by using a clamp;
(3) cleaning the long-period grating area;
(4) adding a poly (diallyldimethylammonium chloride) solution into a liquid pool, and assembling a poly (diallyldimethylammonium chloride) film on the surface of the long-period grating region;
(5) fully flushing the long-period grating area with distilled water, and drying by using nitrogen;
(6) adding a sodium polystyrene sulfonate solution into a liquid pool, and assembling a sodium polystyrene sulfonate film on the surface of the long-period grating area;
(7) fully flushing the long-period grating area with distilled water, and drying by using nitrogen;
(8) adding a titanium dioxide solution into a liquid pool, and assembling a titanium dioxide film on the surface of the long-period grating area;
(9) fully flushing the long-period grating area with distilled water, and drying by using nitrogen;
(10) repeating the operation steps from (6) to (9) until the long-period grating is in an optimal refractive index sensitive area;
(11) adding a hyaluronic acid solution into a liquid pool, and continuously assembling a hyaluronic acid film on the surface of the titanium dioxide film in the long-period grating area;
(12) fully flushing the long-period grating area with distilled water, and drying by using nitrogen;
(13) adding a hyaluronic acid solution into a liquid pool, and assembling a polyallylamine hydrochloride film on the surface of the long-period grating area;
(14) fully flushing the long-period grating area with distilled water, and drying by using nitrogen;
(15) and (4) repeating the operation steps from (11) to (14) and assembling to the required number of layers to obtain the long-period grating which can be used for detecting the pH value.
2. The preparation method for detecting the pH value LPFG according to claim 1, wherein the poly (diallyldimethylammonium chloride) solution is prepared by the following method: dissolving poly (diallyldimethylammonium chloride) in water, adding sodium chloride, and stirring to obtain the poly (diallyldimethylammonium chloride) solution; the molar concentration ratio of the poly (diallyldimethylammonium chloride) to the sodium chloride is 1: 0.001-30000.
3. The preparation method for detecting the pH value LPFG according to claim 1, wherein the sodium polystyrene sulfonate solution is prepared by the following method: dissolving sodium polystyrene sulfonate in water, adding sodium chloride, and stirring uniformly to obtain a sodium polystyrene sulfonate solution; the molar concentration ratio of the sodium polystyrene sulfonate to the sodium chloride is 1: 0.001-30000.
4. The preparation method for detecting the pH value LPFG according to claim 1, wherein the concentration of the titanium dioxide solution is 0.0001mg/mL-10 g/mL; the pH value of the titanium dioxide solution is 2.8-5.8; the particle size of the titanium dioxide in the titanium dioxide solution is 0.001-500 mu m.
5. The preparation method of claim 1, wherein the hyaluronic acid solution and the polyallylamine hydrochloride solution have a concentration of 0.0001-0.1mol/L and a pH of 3-10.
6. The preparation method of claim 5, wherein the hyaluronic acid solution and the polyallylamine hydrochloride solution both contain sodium chloride at a concentration of 0-0.3 mol/L.
7. The preparation method for detecting the pH value LPFG according to claim 1, wherein the assembly on the surface of the long-period grating region in steps (4), (6), (8), (11) and (13) is carried out on the surface of a long-period grating region cladding layer after straightening and fixing.
8. The preparation method for detecting the pH value LPFG according to claim 1, wherein the time for assembling on the surface of the long-period grating gate region in steps (4), (6), (8), (11) and (13) is 1-30 min.
9. The manufacturing method of claim 1, wherein the long period grating in step (15) has a pH value detection range of 3-10.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070025661A1 (en) * | 2005-04-04 | 2007-02-01 | Zhiyong Wang | Fiber-optic sensor or modulator using tuning of long period gratings with self-assembled layers |
| CN101003194A (en) * | 2006-01-19 | 2007-07-25 | 中国科学院化学研究所 | Humidity sensitive composite membrane of polymer, preparation method and application |
| CN213181234U (en) * | 2020-08-25 | 2021-05-11 | 深圳技术大学 | PH value monitoring device based on coating long-period fiber grating |
-
2021
- 2021-12-02 CN CN202111461487.XA patent/CN114199824A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070025661A1 (en) * | 2005-04-04 | 2007-02-01 | Zhiyong Wang | Fiber-optic sensor or modulator using tuning of long period gratings with self-assembled layers |
| CN101003194A (en) * | 2006-01-19 | 2007-07-25 | 中国科学院化学研究所 | Humidity sensitive composite membrane of polymer, preparation method and application |
| CN213181234U (en) * | 2020-08-25 | 2021-05-11 | 深圳技术大学 | PH value monitoring device based on coating long-period fiber grating |
Non-Patent Citations (1)
| Title |
|---|
| RUI-ZHU YANG, WEN-FEI DONG, XIANG MENG, ET AL: "Nanoporous TiO2/Polyion Thin-Film-Coated Long-Period Grating Sensors for the Direct Measurement of Low-Molecular-Weight Analytes", LANGMUIR, vol. 28, no. 23, pages 8815 - 8816 * |
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