CN102288593A - System for detecting melamine and detecting method thereof - Google Patents
System for detecting melamine and detecting method thereof Download PDFInfo
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- CN102288593A CN102288593A CN2011102043436A CN201110204343A CN102288593A CN 102288593 A CN102288593 A CN 102288593A CN 2011102043436 A CN2011102043436 A CN 2011102043436A CN 201110204343 A CN201110204343 A CN 201110204343A CN 102288593 A CN102288593 A CN 102288593A
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Abstract
The invention discloses a system for detecting melamine and detecting method thereof, relating to the fields of fiber sensing and fiber gas detection. The method comprises the following steps of: filling the fiber core holes of a photonic crystal fiber with silver nanoparticles, outputting light of 785 nanometers emitted by a semiconductor laser by using a fiber in the semiconductor laser, coupling the emitted light into the photonic crystal fiber under the collimating and focusing actions of a first non-spherical lens and a second non-spherical lens to excite the generation of a surface-enhanced Raman scattering signal, and focusing the surface-enhanced Raman scattering signal with a third non-spherical lens; and filtering the surface-enhanced Raman scattering signal with a wave trapping sheet to obtain a filtered surface-enhanced Raman scattering signal, and inputting the filtered surface-enhanced Raman scattering signal into a spectrometer to realize detection of melamine. Qualitative detection of melamine in a liquid sample is realized by adopting the photonic crystal fiber based on surface enhancement Raman scattering. Surface-enhanced Raman scattering signals are acquired in an equidirectional way, so that the acquisition degree of signals is increased.
Description
Technical field
The present invention relates to Fibre Optical Sensor and fiber-optic fiber gas detection range, particularly a kind of system and detection method thereof that detects melamine.
Background technology
Melamine formal name used at school three ammonia triazines are the very high organic chemical industry's materials of a kind of nitrogen atom.Because of its high nitrogen content makes the lawless person carry out incorrect utilization to it, be entrained in the materials such as milk, feed to cause the illusion of protein content virtual height, therefrom to the human and next serious health hazard of other lead for animals.At present the melamine detection method is mainly comprised: Solid-Phase Extraction-ion-exchange chromatography, fluorescent spectrometry, Solid-Phase Extraction-capillary electrophoresis, nano-modified silk electro-chemistry immunity method and pressurization capillary electric chromatogram method etc.
Shortcoming and defect below the inventor finds to exist at least in the prior art in realizing process of the present invention:
Above-mentioned these methods all have certain shortcoming, as growing analysis time, being not suitable for on-site measurement and environmental baseline restriction etc., have dwindled range of application, can't satisfy the multiple needs in the practical application.
Summary of the invention
In order to reduce analysis time, enlarge range of application, the invention provides a kind of system and detection method thereof that detects melamine, see for details hereinafter and describe:
A kind of system that detects melamine, described system comprises: semiconductor laser, first non-spherical lens, second non-spherical lens, the 3rd non-spherical lens, photonic crystal fiber, trap sheet and spectrometer,
Be filled with silver nano-grain in the fibre core hole of described photonic crystal fiber, the optical fiber output of the light of the 785nm that described semiconductor laser sends in described semiconductor laser, collimation focusing by described first non-spherical lens and described second non-spherical lens is coupled into described photonic crystal fiber, excite and produce the Surface enhanced raman spectroscopy signal, by described the 3rd non-spherical lens described Surface enhanced raman spectroscopy signal is focused on then, described trap sheet filters described Surface enhanced raman spectroscopy signal, Surface enhanced raman spectroscopy signal after obtaining filtering, Surface enhanced raman spectroscopy signal after the described filtration is input in the described spectrometer, realizes melamine detection.
Described semiconductor laser is a FC-D-785A N-type semiconductor N laser instrument.
Described non-spherical lens model is 354120 and 354430, and plates the anti-reflection film of 785nm.
Described photonic crystal fiber model is an Air-6-800 type hollow-core photonic crystal fiber.
Described trap sheet model is NF03-785E-25, and its notch bandwidth is 39nm.
A kind of method that detects melamine said method comprising the steps of:
(1) adopt optical fiber splicer to draw the awl mode that photonic crystal fiber is drawn awl;
(2) silver nano-grain is filled in the fibre core hole of described photonic crystal fiber;
(3) the optical fiber output of the light of the 785nm that sends of semiconductor laser in described semiconductor laser, collimation focusing by first non-spherical lens and second non-spherical lens is coupled into described photonic crystal fiber, excite to produce the Surface enhanced raman spectroscopy signal, the 3rd non-spherical lens focuses on described Surface enhanced raman spectroscopy signal;
(4) the trap sheet filters described Surface enhanced raman spectroscopy signal, the Surface enhanced raman spectroscopy signal after obtaining filtering;
(5) the Surface enhanced raman spectroscopy signal after the described filtration is input in the spectrometer, realizes melamine detection by described spectrometer.
Described employing optical fiber splicer in the step (1) draws the awl mode to draw awl to be specially to photonic crystal fiber:
At first photonic crystal fiber is cut into about 15cm several sections, remove its coat, utilize described optical fiber splicer to draw awl then at every section center section;
Set the spacing d of electrode and described photonic crystal fiber, discharge time and discharge current realize that the covering airport of described photonic crystal fiber subsides, and keep the fibre core hole constant.
The radius of described silver nano-grain is that the spacing between 38nm, the particle is 0.7nm.
The beneficial effect of technical scheme provided by the invention is:
The invention provides a kind of system and detection method thereof that detects melamine, the present invention has adopted based on the photonic crystal fiber of Surface enhanced raman spectroscopy and has realized qualitative detection to the melamine in the fluid sample, collect the Surface enhanced raman spectroscopy signal in the same way owing to adopt, thereby increased the collection dynamics of signal, for reverse collection, reduced the decay of signal; The present invention draws the selectivity of awl technology realization photonic crystal fiber to fill owing to adopting, thereby guarantees better still to have photon band gap behind the photonic crystal fiber filling liquid, thereby makes exciting light accurate single mode transport in fibre core; Owing to adopt silver nano-grain to be suspended in the testing liquid sample, thereby realize the preparation of Surface enhanced raman spectroscopy substrate, for fibre core hole inwall prepares substrate, have bigger enhancer, thereby can realize that super low concentration detects.
Description of drawings
Fig. 1 is a kind of structural drawing that detects the system of melamine provided by the invention;
Fig. 2-a is a photonic crystals optical fiber structure synoptic diagram provided by the invention;
Fig. 2-b is the transmission spectrum line chart of photonic crystal fiber provided by the invention;
Fig. 3-a and Fig. 3-b are the pattern analysis figure of photonic crystal fiber provided by the invention;
Fig. 4 draws the awl principle schematic for photonic crystal fiber provided by the invention;
Fig. 5 draws the awl design sketch for photonic crystal fiber provided by the invention;
Fig. 6 is a kind of process flow diagram that detects the method for melamine provided by the invention.
Shown in components listed is listed as follows in the accompanying drawing:
1: semiconductor laser; 2: the first non-spherical lenses;
3: photonic crystal fiber; 4: the trap sheet;
5: spectrometer; 6: the second non-spherical lenses;
7: the three non-spherical lenses.
Embodiment
For making the purpose, technical solutions and advantages of the present invention clearer, embodiment of the present invention is described further in detail below in conjunction with accompanying drawing.
In order to reduce analysis time, enlarge range of application, the embodiment of the invention provides a kind of system and detection method thereof that detects melamine, sees for details hereinafter to describe:
PCF (Photonic Crystal Fiber, photonic crystal fiber) is also referred to as microstructured optical fibers or porous optical fiber.After first PCF in 1996 occurred, along with it is furtherd investigate, the PCF of various forms structure occurred in succession.Because the above-mentioned special performance that the periodic structure of PCF is brought further enlarges the application of optical fiber, especially at sensory field of optic fibre.Utilize the correlation properties of PCF, can make polytype sensor.The PCF sensor has characteristics such as high stability, wide wavelength coverage work, and can work under extreme temperature.
The Surface enhanced raman spectroscopy technology has just fully been paid attention to since being found and is utilized, and has incomparable advantage in super low concentration sample or even Single Molecule Detection.Unique cyclic array structure of photonic crystal fiber obtains fast development as a new type ideal platform of Surface enhanced raman spectroscopy SERS sensor, and further widens the application of Surface enhanced raman spectroscopy sensor.The peculiar property of PCF combines with the SERS sensor, has constituted novel sensor---SERS PCF sensor, and in chemistry, biology and environment measuring, be widely used.
A kind of system that detects melamine referring to Fig. 1, comprising: semiconductor laser 1, first non-spherical lens 2, second non-spherical lens 6, the 3rd non-spherical lens 7, photonic crystal fiber 3, trap sheet 4 and spectrometer 5,
Wherein, be filled with silver nano-grain in the fibre core hole of photonic crystal fiber 3, the optical fiber output of the light of the 785nm that semiconductor laser 1 sends in semiconductor laser 1, collimation focusing by first non-spherical lens 2, second non-spherical lens 6 is coupled into photonic crystal fiber 3, excite to produce the Surface enhanced raman spectroscopy signal, focus on by 7 pairs of Surface enhanced raman spectroscopy signals of the 3rd non-spherical lens then; 4 pairs of Surface enhanced raman spectroscopy signals of trap sheet filter, the Surface enhanced raman spectroscopy signal after obtaining filtering, and the Surface enhanced raman spectroscopy signal after the filtration is input in the spectrometer 5, realizes melamine detection.
Wherein, silver nano-grain is filled into the fibre core hole of photonic crystal fiber 3 as the Surface enhanced raman spectroscopy substrate, utilize the Surface enhanced raman spectroscopy principle, produce the Surface enhanced raman spectroscopy signal thereby in the fibre core hole, utilize the Surface enhanced raman spectroscopy substrate to excite, and the Surface enhanced raman spectroscopy signal after filtering is collected in employing in the same way, Surface enhanced raman spectroscopy signal after the filtration is input in the spectrometer 5, realizes the melamine testing goal.
Further, in order to improve the stability of testing result, semiconductor laser 1 in the embodiment of the invention is preferably the FC-D-785A N-type semiconductor N laser instrument of Changchun new industry photoelectricity company, its output wavelength is 785 ± 0.3nm, line width is less than 0.2, and what this light source adopted is optical fiber output, and Optical Fiber Numerical Aperture is 0.22, output power after the optical fiber coupling is 300mW, and stability is in 3%.
Further, in order to cooperate the optical fiber output of light source, non-spherical lens adopts the non-spherical lens of LightPath production, and the non-spherical lens model is 354120 and 354430, and plates the anti-reflection film of 785nm.
Further, in order better to transmit the exciting light of 785nm, and for exciting light and test substance provide bigger contact area, the Air-6-800 type hollow-core photonic crystal fiber that photonic crystal fiber 3 adopts Denmark NKT Photonics company to produce is referring to Fig. 2-a, Fig. 2-b, Fig. 3-a, Fig. 3-b.Wherein Fig. 2-a is geometry synoptic diagram and the transmission spectrum line chart of Air-6-800, and its structure centre is that big airport, covering is 9 layers of little airport, and test substance and exciting light interact in big airport, with Raman emission.Fig. 2-b is its transmission spectrum line chart, has figure as seen very little in the loss of 785nm place photonic crystal fiber, promptly can the low-loss transmission exciting light.Fig. 3-a and 3-b adopt COMSOL software Air-6-800 to be carried out the three dimensional field distribution plan and the equipotential field pattern of numerical simulation gained.
Further,, and eliminate having a strong impact on of exciting light for the Raman signal that will excite generation better outputs to spectrometer 5, the NF03-785E-25 that trap sheet 4 adopts U.S. Semrock to produce, its notch bandwidth is 39nm.
A kind of method that detects melamine, this method may further comprise the steps:
101: adopt optical fiber splicer to draw the awl mode that photonic crystal fiber 3 is drawn awl;
Wherein, adopt optical fiber splicer to draw the awl mode that the covering airport of photonic crystal fiber 3 is subsided, keep the fibre core hole constant, thereby realize the filling of silver nano-grain, be that silver nano-grain only is filled in the fibre core hole of photonic crystal fiber 3, and the covering airport is still realized the selectivity filling for air, and specific implementation process is as follows:
1, at first photonic crystal fiber is cut into about 15cm several sections, remove its coat, utilize optical fiber splicer to draw awl then at every section center section;
Wherein, the model of the optical fiber splicer that the embodiment of the invention adopts is Ericsson FSU-925, during specific implementation, can also adopt the optical fiber splicer of other models, for example: Ericsson FSU-975-A and SCS4000 etc., the embodiment of the invention does not limit this.
2, set the spacing d of electrode and photonic crystal fiber 3, discharge time and discharge current realize that the covering airport of photonic crystal fiber 3 subsides, and keep the fibre core hole constant;
Wherein, draw the covering airport of the photonic crystal fiber 3 that only subsides when boring and keep constant discharge current, pulling force and the material heat transfer effect of depending on fully in fibre core hole, the spacing d of needs setting electrode and photonic crystal fiber 3, discharge time and discharge current.Electric current between the electrode can be expressed as
σ(z)＝σ
0(1+z
2)
-1/3
In the formula, I
0Be by to whole r (radius of a circle in the cylindrical coordinate, r
2=x
2+ y
2) total current that integration obtains, σ (z) is Gauss's width at z place, σ
0It is Gauss's width at electrode mid point z=0 place.Space temperature is directly proportional with current density, promptly
T(r，z)∝i
2(r，z)
This shows that temperature is the highest at the eletrode tip place, equally also can find in the surface of photonic crystal fiber 3 temperature the highlyest that fibre core place temperature is minimum.The thermal conductivity of solid silicon can be slowed down gradually to fibre core by covering because of the existence of air in the photonic crystal fiber 3, and work as the rate of heat addition is
The time covering airport can subside.In the formula, γ is a surface tension, and η is the viscosity of silicon.Because viscosity can descend rapidly along with the increase of temperature,, the covering airport of photonic crystal fiber 3 was subsided before the fibre core hole so that the airport of high-temperature region subsides is faster.If select the suitable awl parameter of drawing, just can realize that the covering airport of photonic crystal fiber 3 subsides, keep intact in the fibre core hole.
102: silver nano-grain is filled in the fibre core hole of photonic crystal fiber 3;
According to the enhanced mechanism of Surface enhanced raman spectroscopy, when the polarity of scattered light was identical with incident light, the Raman signal electromagnetism of expection strengthened and can be expressed as
In the formula, E
(r, ω)Be at the total electric field in r place, E
Inc (ω)It is the incident electromagnetic wave electric field.
Further, in order to strengthen the Surface enhanced raman spectroscopy signal, by numerical simulation, when drawing radius when silver nano-grain and be spacing between 38nm, the particle and being 0.7nm, have best enhancing effect, be specially: in preparation process, suitably add surfactant in the solution, silver nano-grain is suspended in liquid, and the concentration of control silver nano-grain in solution changes the distance between the silver nano-grain, thereby can more effectively excite the SERS signal.The silver nano-grain of 38nm evenly is suspended in the testing liquid sample under the effect of surfactant, then mixing material is filled in the fibre core hole of photonic crystal fiber 3, make silver nano-grain in the fibre core hole of photonic crystal fiber 3, evenly distribute, rather than only attached to fibre core hole inwall, thereby produce stronger Surface enhanced raman spectroscopy signal.
103: the optical fiber output of the light of the 785nm that semiconductor laser 1 sends in semiconductor laser 1, collimation focusing by first non-spherical lens 2, second non-spherical lens 6 is coupled into photonic crystal fiber 3, excite to produce the Surface enhanced raman spectroscopy signal, focus on by 7 pairs of Surface enhanced raman spectroscopy signals of the 3rd non-spherical lens then;
104: 4 pairs of Surface enhanced raman spectroscopy signals of trap sheet filter, the Surface enhanced raman spectroscopy signal after obtaining filtering;
105: the Surface enhanced raman spectroscopy signal after will filtering is input in the spectrometer 5, realizes melamine detection by spectrometer 5.
In sum, the embodiment of the invention provides a kind of system and detection method thereof that detects melamine, the embodiment of the invention has adopted based on the photonic crystal fiber of Surface enhanced raman spectroscopy and has realized qualitative detection to the melamine in the fluid sample, collect the Surface enhanced raman spectroscopy signal in the same way owing to adopt, thereby increased the collection dynamics of signal, for reverse collection, reduced the decay of signal; The embodiment of the invention draws the selectivity of awl technology realization photonic crystal fiber to fill owing to adopting, thereby guarantees better still to have photon band gap behind the photonic crystal fiber filling liquid, thereby makes exciting light accurate single mode transport in fibre core; Owing to adopt silver nano-grain to be suspended in the testing liquid sample, thereby realize the preparation of Surface enhanced raman spectroscopy substrate, for fibre core hole inwall prepares substrate, have bigger enhancer, thereby can realize that super low concentration detects.
It will be appreciated by those skilled in the art that accompanying drawing is the synoptic diagram of a preferred embodiment, the invention described above embodiment sequence number is not represented the quality of embodiment just to description.
The above only is preferred embodiment of the present invention, and is in order to restriction the present invention, within the spirit and principles in the present invention not all, any modification of being done, is equal to replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (8)
1. a system that detects melamine is characterized in that, described system comprises: semiconductor laser, first non-spherical lens, second non-spherical lens, the 3rd non-spherical lens, photonic crystal fiber, trap sheet and spectrometer,
Be filled with silver nano-grain in the fibre core hole of described photonic crystal fiber, the optical fiber output of the light of the 785nm that described semiconductor laser sends in described semiconductor laser, collimation focusing by described first non-spherical lens and described second non-spherical lens is coupled into described photonic crystal fiber, excite and produce the Surface enhanced raman spectroscopy signal, by described the 3rd non-spherical lens described Surface enhanced raman spectroscopy signal is focused on then, described trap sheet filters described Surface enhanced raman spectroscopy signal, Surface enhanced raman spectroscopy signal after obtaining filtering, Surface enhanced raman spectroscopy signal after the described filtration is input in the described spectrometer, realizes melamine detection.
2. a kind of system that detects melamine according to claim 1 is characterized in that, described semiconductor laser is a FC-D-785A N-type semiconductor N laser instrument.
3. a kind of system that detects melamine according to claim 1 is characterized in that described non-spherical lens model is 354120 and 354430, and plates the anti-reflection film of 785nm.
4. a kind of system that detects melamine according to claim 1 is characterized in that, described photonic crystal fiber model is an Air-6-800 type hollow-core photonic crystal fiber.
5. a kind of system that detects melamine according to claim 1 is characterized in that, described trap sheet model is NF03-785E-25, and its notch bandwidth is 39nm.
6. a method that detects melamine is characterized in that, said method comprising the steps of:
(1) adopt optical fiber splicer to draw the awl mode that photonic crystal fiber is drawn awl;
(2) silver nano-grain is filled in the fibre core hole of described photonic crystal fiber;
(3) the optical fiber output of the light of the 785nm that sends of semiconductor laser in described semiconductor laser, collimation focusing by first non-spherical lens and second non-spherical lens is coupled into described photonic crystal fiber, excite to produce the Surface enhanced raman spectroscopy signal, the 3rd non-spherical lens focuses on described Surface enhanced raman spectroscopy signal;
(4) the trap sheet filters described Surface enhanced raman spectroscopy signal, the Surface enhanced raman spectroscopy signal after obtaining filtering;
(5) the Surface enhanced raman spectroscopy signal after the described filtration is input in the spectrometer, realizes melamine detection by described spectrometer.
7. a kind of method that detects melamine according to claim 6 is characterized in that, the described employing optical fiber splicer in the step (1) draws the awl mode to draw awl to be specially to photonic crystal fiber:
At first photonic crystal fiber is cut into about 15cm several sections, remove its coat, utilize described optical fiber splicer to draw awl then at every section center section;
Set the spacing d of electrode and described photonic crystal fiber, discharge time and discharge current realize that the covering airport of described photonic crystal fiber subsides, and keep the fibre core hole constant.
8. a kind of method that detects melamine according to claim 6 is characterized in that, the radius of described silver nano-grain is that the spacing between 38nm, the particle is 0.7nm.
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Cited By (4)
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| CN103257134A (en) * | 2013-04-18 | 2013-08-21 | 东南大学 | Method for preparing surface-enhanced Raman scattering (SERS) substrate based on capillary tube |
| CN104807805A (en) * | 2015-05-04 | 2015-07-29 | 华北电力大学 | Detection device for gas dissolved in transformer oil based on Raman spectrum |
| CN106290896A (en) * | 2016-07-27 | 2017-01-04 | 东北师范大学 | A kind of photonic crystal fiber immunosensor and application thereof |
| CN110567934A (en) * | 2019-08-16 | 2019-12-13 | 北京工业大学 | Raman test auxiliary adjustment coupling real-time imaging system and testing method based on micro-structure optical fiber |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103257134A (en) * | 2013-04-18 | 2013-08-21 | 东南大学 | Method for preparing surface-enhanced Raman scattering (SERS) substrate based on capillary tube |
| CN104807805A (en) * | 2015-05-04 | 2015-07-29 | 华北电力大学 | Detection device for gas dissolved in transformer oil based on Raman spectrum |
| CN106290896A (en) * | 2016-07-27 | 2017-01-04 | 东北师范大学 | A kind of photonic crystal fiber immunosensor and application thereof |
| CN106290896B (en) * | 2016-07-27 | 2018-05-18 | 东北师范大学 | A kind of photonic crystal fiber immunosensor and its application |
| CN110567934A (en) * | 2019-08-16 | 2019-12-13 | 北京工业大学 | Raman test auxiliary adjustment coupling real-time imaging system and testing method based on micro-structure optical fiber |
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