CN113203703A - Optical fiber sensor for detecting trivalent arsenic ions - Google Patents
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- CN113203703A CN113203703A CN202110473756.8A CN202110473756A CN113203703A CN 113203703 A CN113203703 A CN 113203703A CN 202110473756 A CN202110473756 A CN 202110473756A CN 113203703 A CN113203703 A CN 113203703A
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- 239000011651 chromium Substances 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 15
- 230000035945 sensitivity Effects 0.000 abstract description 9
- 238000001514 detection method Methods 0.000 abstract description 7
- 238000004873 anchoring Methods 0.000 abstract 1
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- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 description 2
- VHJLVAABSRFDPM-IMJSIDKUSA-N L-1,4-dithiothreitol Chemical compound SC[C@H](O)[C@@H](O)CS VHJLVAABSRFDPM-IMJSIDKUSA-N 0.000 description 1
- RWSXRVCMGQZWBV-PHDIDXHHSA-N L-Glutathione Natural products OC(=O)[C@H](N)CCC(=O)N[C@H](CS)C(=O)NCC(O)=O RWSXRVCMGQZWBV-PHDIDXHHSA-N 0.000 description 1
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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
-
- 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
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
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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
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
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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
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N2021/7769—Measurement method of reaction-produced change in sensor
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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
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Abstract
The invention relates to the field of optical fiber sensing, in particular to an optical fiber sensor for detecting trivalent arsenic ions in a water body. The fiber grating and the optical fiber with part of the cladding removed are utilized to couple light inside the fiber core to the cladding, a layer of metal nano film is deposited on the surface of the optical fiber, then chemical molecules capable of reacting with trivalent arsenic ions are modified, anchoring of the trivalent arsenic ions is realized, and chemically modified nano particles are further anchored to improve the sensitivity of the optical fiber sensor. The sensor can realize high-sensitivity detection of trivalent arsenic ions, and is simple in structure, low in price and easy to operate.
Description
Technical Field
The invention relates to the field of optical fiber sensing, in particular to an optical fiber sensor for detecting trivalent arsenic ions based on a chemically modified metal nano film.
Background
With the continuous development of industrialization, human beings discharge a plurality of pollutants into the environment, wherein heavy metal pollutants are representative of water body and soil pollutants and have huge toxicity. Arsenic ion is one of many heavy metal contaminants. Drinking water contaminated by arsenic ions poses a serious threat to human health. Statistically, about 1.4 million people worldwide drink drinking water contaminated with arsenic ions. The arsenic ion water body has a plurality of valence states, wherein the trivalent arsenic ion has the maximum toxicity, the strongest stability and the stronger mobility. Research shows that under the same conditions, the arsenic ion absorbing capacity of rice is about ten times that of other grains such as wheat, corn and the like, namely the rice has the capacity of enriching arsenic ions. While rice is the main food for human beings, and accounts for about half of the human ration. Excessive intake of arsenic ions can cause various organ diseases, and the content of arsenic ions in drinking water cannot exceed 10ppb by the world health organization due to extremely strong toxicity. Therefore, highly sensitive techniques are needed to detect ultra-low concentrations of arsenic ions.
The traditional heavy metal ion detection method comprises an atomic absorption spectrometry, a spectrophotometry, an inductively coupled plasma mass spectrometry, a chemiluminescence method and the like. The atomic absorption spectrometry and the inductively coupled plasma mass spectrometry are expensive, the sample pretreatment is complex, the operation is complex, and the detection time is long. The spectrophotometry cannot distinguish heavy metal ions with similar structures and radii, so that the detection selectivity is low. The chemiluminescence method has poor selectivity and is not suitable for detecting low-concentration samples. Therefore, it is necessary to develop a sensor which is easy to handle, small in size, and high in sensitivity. Although the optical fiber sensor has the characteristics of easy operation, miniaturization, high sensitivity and the like, the currently developed optical fiber sensor is less applied to detecting trivalent arsenic ions. And the influence of trivalent arsenic ions with trace concentration on the dielectric constant of an environmental medium is small, so that the high-sensitivity trivalent arsenic ion detection is difficult to realize. Therefore, there is a need to develop a new optical fiber sensor for detecting trivalent arsenic ions.
Disclosure of Invention
The invention aims to provide an optical fiber sensor with a layer of metal nano film deposited on the surface of an optical fiber, and the specific reaction of trivalent arsenic ions is realized on the surface of a metal film through chemical modification. And by introducing the chemically modified metal nanoparticles, the sensitivity of detecting trivalent arsenic ions is greatly improved.
In order to achieve the purpose, the invention adopts the following technical scheme:
an optical fiber sensor for detecting trivalent arsenic ions comprises an optical fiber, a metal nano film deposited on the surface of the optical fiber and chemically modified nano particles.
Wherein the metal nano film is deposited on the surface of the optical fiber, and the surface of the metal nano film is decorated with chemical molecules capable of reacting with trivalent arsenic ions.
Furthermore, the thickness of the metal nano film is 0.5nm-500 nm.
Furthermore, the metal nano-film comprises one or more of chromium, gold, silver, platinum and other metal films.
Further, the chemical molecule modified on the surface of the metal nano film is one of glutathione, dithiothreitol and cysteine.
Wherein the surface of the chemically modified nano-particle is modified with chemical molecules capable of reacting with trivalent arsenic ions. The diameter of the chemically modified nano-particles is 10-30 nm.
Further, the nano-particles are one of gold nano-particles, silver nano-particles and platinum nano-particles.
Further, the chemical molecule modified on the surface of the nanoparticle is any one of glutathione, dithiothreitol and cysteine.
The optical fiber comprises one or more of a fiber grating, an optical fiber with a partial cladding removed, and an optical fiber with a single-mode-multi-mode-single-mode structure.
The principle of the method of the invention is as follows:
the fiber grating, the fiber with a part of the cladding removed, and the fiber with a single-mode-multi-mode-single-mode structure can couple light inside the fiber core to the cladding, and when the refractive index of the environment medium near the surface changes, the transmitted light in the fiber changes, so that the change of the refractive index near the surface can be quantitatively reflected by measuring the spectral change. According to the invention, a layer of metal nano film is deposited on the surface of the optical fiber, and molecules which react with trivalent arsenic ions are modified on the surface of the optical fiber, so that the specificity of detecting the trivalent arsenic ions can be realized. To be able to further increase the detection sensitivity, chemically modified nanoparticles are used to enhance the refractive index of the ambient medium. The chemically modified nanoparticles can react with arsenic ions and are anchored on the surface of the optical fiber, so that the refractive index of the environment on the surface of the optical fiber can be greatly influenced.
From the above discussion, the optical fiber sensor for detecting trivalent arsenic ions has the advantages of integration, fast response, high sensitivity and the like.
Drawings
FIG. 1 is a schematic diagram of an optical fiber sensor for detecting trivalent arsenic ions;
FIG. 2 is a schematic illustration in the dashed box of FIG. 1;
FIG. 3 is an SEM photograph of a 20nm silver nano-film on the surface of an optical fiber;
FIG. 4 is an SEM photograph of the silver nano-film, trivalent arsenic ion and gold nanoparticles on the surface of the optical fiber;
in the figure: 1-fiber core, 2-metal nano film, 3-chemical modification molecule and trivalent arsenic ion, metal nano particle, 4-chemical molecule for metal nano film surface modification, 5-trivalent arsenic ion, 6-metal nano particle and 7-chemical molecule for metal nano particle surface modification;
FIG. 5 is a spectrum of arsenic ions of different concentrations measured using a fiber grating sensor; wherein the arsenic ion concentration is 0ppb,0.3ppb,0.6ppb,0.9ppb,1.2ppb,1.5ppb,1.8ppb and 3ppb according to the spectrum from bottom to top.
FIG. 6 shows the spectral peak intensities of arsenic ions of different concentrations measured with a fiber grating sensor.
Detailed Description
For further disclosure, but not limitation, the present invention is described in further detail below with reference to examples.
Example 1
Stripping the plastic on the surface of the commercial single-mode optical fiber by using a wire stripper for 3cm, and writing an optical fiber grating on the bare and leaky optical fiber by using a carbon dioxide laser, wherein the grating period is 500 microns, and the period number is 30. A layer of metal silver nano film is deposited on the surface of the fiber grating by a magnetron sputtering technology, and the thickness of the film is 20 nanometers. And then, immersing the fiber grating deposited with the silver nano film into a 1mmol/L glutathione solution, keeping for 2 hours, washing the surface of the optical fiber with deionized water, and washing away the unreacted glutathione on the surface of the optical fiber. Soaking the fiber grating into arsenic ion solutions with different concentrations, keeping for 2 hours, then washing the surface of the optical fiber with deionized water, and washing away the unreacted arsenic ions on the surface of the optical fiber.
On the other hand, glutathione-modified gold nanoparticles were prepared. First, 0.5mL of 20mmol/L chloroauric acid was added to 50mL deionized water at 80 ℃. Then, 1mL of a 1wt% sodium citrate solution was added to the above solution, and reacted for 10 minutes. After that, it was cooled to room temperature. The gold nanosol was centrifuged three times and re-dispersed in 50mL of deionized water. 15mL of gold nanosol was taken, and 40. mu.L of 10. mu. Mol glutathione solution was added and incubated at 25 ℃ for 12 hours.
And (3) welding the tail end of an optical fiber of a halogen tungsten lamp light source with one end of a fiber grating with arsenic ions anchored on the surface, connecting the other end of the fiber grating with a spectrum analyzer, and immersing the fiber grating into gold nano sol cultured by glutathione. The course of spectral change is collected.
The silver nano-film deposited on the surface of the optical fiber is shown in fig. 3, and it can be seen that the silver nano-film has a cracking phenomenon due to a thin thickness; after the nano-gold sol modified by glutathione, arsenic ion and glutathione is sequentially cultured, a large number of gold nanoparticles are deposited on the surface of the nano-silver, as shown in fig. 4. As shown in FIG. 5 and FIG. 6, the spectral absorption peak intensity shows a good linear change in the range of 0.3-1.8ppb arsenic ion:
(R2 = 0.93), where y is the intensity of the absorption peak and x is the concentration of arsenic ions, so that the sensitivity of the sensor can reach 0.22dB/ppb and the detection limit can reach 0.67 ppb.
Example 2
Stripping the plastic on the surface of the commercial single-mode optical fiber by using a wire stripper for 5cm, and polishing one side of the bare light leakage fiber by about 45 micrometers in a polishing and grinding mode. And depositing a layer of metal silver nano film on the polished surface of the optical fiber by a magnetron sputtering technology, wherein the thickness of the film is 40 nanometers. And then, soaking the fiber grating deposited with the silver nano film into 1mmol/L dithiothreitol solution, keeping for 2 hours, washing the surface of the optical fiber with deionized water, and washing away the unreacted dithiothreitol on the surface of the optical fiber. Soaking the fiber grating into arsenic ion solutions with different concentrations, keeping for 2 hours, then washing the surface of the optical fiber with deionized water, and washing away the unreacted arsenic ions on the surface of the optical fiber.
In another aspect, cysteine modified gold nanoparticles are prepared. First, 0.5mL of 20mmol/L chloroauric acid was added to 50mL deionized water at 80 ℃. Then, 1mL of a 1wt% sodium citrate solution was added to the above solution, and reacted for 10 minutes. After that, it was cooled to room temperature. The gold nanosol was centrifuged three times and re-dispersed in 50mL of deionized water. 15mL of gold nanosol was taken, and 40. mu.L of 10. mu. Mol cysteine solution was added and incubated at 25 ℃ for 12 hours.
And (3) welding the tail end of an optical fiber of a tungsten halogen lamp light source with one end of a fiber grating with arsenic ions anchored on the surface, connecting the other end of the fiber grating with a spectrum analyzer, and immersing the fiber grating into gold nano sol cultured by cysteine. The course of spectral change is collected. The spectrum result shows that the sensor can detect arsenic ions with the concentration as low as 0.5ppb, the position of a spectral absorption peak of the arsenic ions is in good linear change within the range of 0.5-10ppb, and the sensitivity can reach 0.14 nm/ppb.
Example 3
Stripping 5cm of plastic on the surface of the commercial single-mode optical fiber by using a wire stripper, cutting a section of plastic by using a cutting knife to realize a good cutting plane, welding a section of multimode optical fiber with the length of 2 cm, the core diameter of 65 microns and the outer diameter of 125 microns, and then welding a section of commercial single-mode optical fiber. A layer of metallic silver nano film is deposited on the surface of the multimode fiber by a magnetron sputtering technology, and the thickness of the film is 40 nanometers. And then, immersing the fiber grating deposited with the silver nano film into a cysteine solution of 1mmol/L, keeping for 2 hours, washing the surface of the optical fiber by deionized water, and washing away the unreacted cysteine on the surface of the optical fiber. Soaking the fiber grating into arsenic ion solutions with different concentrations, keeping for 2 hours, then washing the surface of the optical fiber with deionized water, and washing away the unreacted arsenic ions on the surface of the optical fiber.
On the other hand, glutathione-modified gold nanoparticles were prepared. First, 0.5mL of 20mmol/L chloroauric acid was added to 50mL deionized water at 80 ℃. Then, 1mL of a 1wt% sodium citrate solution was added to the above solution, and reacted for 10 minutes. After that, it was cooled to room temperature. The gold nanosol was centrifuged three times and re-dispersed in 50mL of deionized water. 15mL of gold nanosol was taken, and 40. mu.L of 10. mu. Mol glutathione solution was added and incubated at 25 ℃ for 12 hours.
And (3) welding the tail end of an optical fiber of a halogen tungsten lamp light source with one end of a fiber grating with arsenic ions anchored on the surface, connecting the other end of the fiber grating with a spectrum analyzer, and immersing the fiber grating into gold nano sol cultured by glutathione. The course of spectral change is collected. The spectrum result shows that the sensor can detect arsenic ions with the concentration as low as 0.3ppb, the spectrum absorption peak intensity shows good linear change within the range of 0.3-5ppb of the arsenic ions, and the sensitivity can reach 0.16 dB/ppb.
The above description is only a preferred embodiment of the present invention, and all equivalent changes and modifications made in accordance with the claims of the present invention should be covered by the present invention.
Claims (10)
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