CN106525761A - Nitrite detection method based on terahertz spectroscopy scanning - Google Patents
Nitrite detection method based on terahertz spectroscopy scanning Download PDFInfo
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- IOVCWXUNBOPUCH-UHFFFAOYSA-M Nitrite anion Chemical compound [O-]N=O IOVCWXUNBOPUCH-UHFFFAOYSA-M 0.000 title claims abstract description 32
- 238000001514 detection method Methods 0.000 title claims abstract description 24
- 238000004611 spectroscopical analysis Methods 0.000 title claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000000034 method Methods 0.000 claims abstract description 19
- 238000010521 absorption reaction Methods 0.000 claims abstract description 11
- 230000003595 spectral effect Effects 0.000 claims abstract 3
- 238000001228 spectrum Methods 0.000 claims description 35
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 239000002253 acid Substances 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 6
- 238000012937 correction Methods 0.000 claims description 3
- 239000006185 dispersion Substances 0.000 claims description 3
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 abstract description 24
- 235000010288 sodium nitrite Nutrition 0.000 abstract description 12
- 238000012545 processing Methods 0.000 abstract description 3
- 238000013178 mathematical model Methods 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 14
- 229910019142 PO4 Inorganic materials 0.000 description 5
- 235000013305 food Nutrition 0.000 description 5
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 5
- 239000010452 phosphate Substances 0.000 description 5
- 238000000862 absorption spectrum Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 4
- 239000000243 solution Substances 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 238000009360 aquaculture Methods 0.000 description 3
- 244000144974 aquaculture Species 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 238000000149 argon plasma sintering Methods 0.000 description 2
- 238000004587 chromatography analysis Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000004401 flow injection analysis Methods 0.000 description 2
- 238000002795 fluorescence method Methods 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 238000007689 inspection Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000010703 silicon Substances 0.000 description 2
- 235000010344 sodium nitrate Nutrition 0.000 description 2
- 239000004317 sodium nitrate Substances 0.000 description 2
- 238000001328 terahertz time-domain spectroscopy Methods 0.000 description 2
- 208000036626 Mental retardation Diseases 0.000 description 1
- IOVCWXUNBOPUCH-UHFFFAOYSA-N Nitrous acid Chemical compound ON=O IOVCWXUNBOPUCH-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 238000009395 breeding Methods 0.000 description 1
- 230000001488 breeding effect Effects 0.000 description 1
- 230000000711 cancerogenic effect Effects 0.000 description 1
- 231100000315 carcinogenic Toxicity 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 231100000206 health hazard Toxicity 0.000 description 1
- 150000002484 inorganic compounds Chemical class 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000008621 organismal health Effects 0.000 description 1
- 230000002688 persistence Effects 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 231100000683 possible toxicity Toxicity 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002123 temporal effect Effects 0.000 description 1
- 238000012549 training Methods 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
Classifications
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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
- G01N21/25—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
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3577—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing liquids, e.g. polluted water
-
- 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
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3581—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using far infrared light; using Terahertz radiation
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- Physics & Mathematics (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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- Toxicology (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention discloses a nitrite detection method based on terahertz spectroscopy scanning. The nitrite detection method includes the steps that (1) samples of a nitrite water solution with the preset concentration range are prepared; (2) the terahertz frequency domain spectral information of all the samples in the wave band range of 0.2 THz to 2.0 THz is obtained; (3) after the terahertz frequency domain spectral information is subjected to de-noising processing, characteristic absorption peaks are extracted; (4) a model between the characteristic absorption peaks and the nitrite water solution concentration is established; (5) the characteristic absorption peaks of to-be-detected water samples are obtained and input the model, and the detection result corresponding to the nitrite concentration is obtained. According to the nitrite detection method, terahertz spectroscopy scanning is adopted, the speed is high, operating is easy, and the problems that the traditional water-body nitrite detection method is tedious in process, slow in speed and the like are solved. As a relationship forecasting mathematical model is established between terahertz spectroscopy and the sodium nitrite content, the high forecasting accuracy can be obtained.
Description
Technical field
The present invention relates to water quality, environment, Food Safety Analysis evaluate field, more particularly to it is a kind of using terahertz time-domain light
The method that spectrum and frequency domain spectra method determine Nitrite content.
Background technology
Nitrite is the general name of a class inorganic compound, refers mainly to sodium nitrite, and sodium nitrite is soluble in water white
Color is to pale yellow powder or graininess.Nitrite is widely present in human environment, is most common nitrogen in nature
Compound.Generally believe that now nitrite is a kind of strong blood poisonous substance, and there is potential toxicity and carcinogenic threat, it is right
Organism health hazard is very big.Especially in aquaculture field, coastal area aquaculture fast development in recent years, with cultivation
The increasing of density and cultivating pool it is aging, the higher problem of breeding process nitrite is highlighted, aquaculture
The sub- pin phosphate content of water quality directly affects cultivation success or failure and food safety.Thus, the content for determining Nitrite is food
Very important project in product safety detection.
At present, the sub- pin phosphate content detection of water body mainly have spectrophotography, fluorescence method, chemoluminescence method, electrochemical process,
Chromatography and Flow Injection Analysis etc..Wherein, may there is the interference of same absworption peak material in spectrophotography, and just cannot obtain
True data, degree of accuracy are relatively low；The diverging direction of the fluorescence of fluorescence method is not concentrated, the light intensity of fluorescence is not high, and phosphor persistence
Time it is shorter, so linear situation is sometimes undesirable；Chemoluminescence method needs to consume luminous agent, while quantum efficiency is relative
It is relatively low；The voltage and current potentially unstable of electrochemical process, causes the nano material for preparing uneven, affects performance；Chromatography
Qualitative ability it is poor, when the sterling for not having determinand or corresponding chromatographic qualitative data are used as control, it is impossible to from chromatographic peak
Provide qualitative results；The analysis of Flow Injection Analysis and complex operation.Using said method, not only pretreatment process is loaded down with trivial details, and manually
Mode measures not only speed and slowly, can also there is larger personal error.Therefore, the physicochemical characteristicss of the sub- pin hydrochlorate of water body are studied
With the coupled relation of sub- pin phosphate content, the content information of sub- pin hydrochlorate, exploitation are gathered using the fresh approach such as spectrum technology
It is a kind of accurate, stable, easy, quick, adapt to produce, process, check the nitrite that each link is used qualitative and quantitative square
Method, with good theoretical significance and actual application value.
The content of the invention
The invention provides a kind of nitrite detection method scanned based on tera-hertz spectra, is capable of achieving water nitrite acid
Salt is quick, objectively qualitative and quantitative detection, and other content of nitrite in foods is detected and food processing link
The monitoring of nitrous acid content also has important using value.
A kind of nitrite detection method scanned based on tera-hertz spectra, including：
(1) configure the sample of the sub- pin acid salt aqueous solution of predetermined concentration scope；
(2) obtain terahertz light spectrum information of each sample in 0.2～2.0THz wavelength bands；
(3) characteristic absorption peak will be extracted after the Terahertz frequency domain spectra information denoising；
(4) model set up between characteristic absorption peak and sub- pin acid salt aqueous solution concentration；
(5) obtain the characteristic absorption peak of water sample to be detected and be input into the model, obtain corresponding sub- pin hydrochlorate concentration inspection
Survey result.
As substantial amounts of molecular vibration and rotational energy level are all in terahertz wave band, terahertz time-domain spectroscopy detection technique exists
There is during measurement advantage, which can be used as fingerprint characteristic and analyze its characteristic spectrum, research thing to absorbing strong to terahertz emission
The inside composition of matter.Further, since the Terahertz for producing is to excite instantaneous carrying-current to be formed by the femto-second laser of ultra-narrow band,
The features such as there is high s/n ratio, mental retardation, broadband property, coherence, transient state, perspectivity also.Therefore, can using tera-hertz spectra
Realize the quick of water nitrite, high accuracy, the detection of low cost.
Implement the time-domain signal detecting system (THZ-TDS) that the inventive method can build tera-hertz spectra in advance, step (1)
The middle sub- pin acid salt aqueous solution sample for preparing variable concentrations, using sodium nitrite and pure water accurate formulation.
Preferably, the mass percent concentration scope of multiple samples is 10.1%～34.0% in step (1).
As it is further preferably, the Concentraton gradient of multiple samples is at intervals of 0.1%.
For each sample, take a drop every time, drip in the thin silicon wafer for reflecting platform in Terahertz, obtain sample 0.2～
Terahertz light spectrum information in 2.0THz wavelength bands.
For the ease of follow-up data processing, preferably, the tera-hertz spectra information includes time-domain spectroscopy information, with
And time-domain spectroscopy information is fourier transformed the frequency domain spectra information after (FFT).
Preferably, the denoising of step (3) is first to carry out additional dispersion correction again using 9 points of average smooth methods
(MSC)。
Inhalation effects of the eliminating water to tera-hertz spectra can be effectively gone in the denoising of the present invention, and remove from high frequency with
Machine noise, baseline drift, the uneven, light scattering of sample etc. affect.
Preferably, in step (3), extracting the absworption peak at 1.67THz, 1.86THz, 1.45THz wave band as feature
Absworption peak.
Suitable characteristic absorption peak is selected accurately to detect sub- pin phosphate content.
Preferably, the model that step (4) is set up is LS-SVM models.
Relative to other kinds of model, for the detection of sub- pin phosphate content, least square method supporting vector machine (LS-
SVM) model can improve the precision of prediction of model, especially the precision of prediction to low concentration sample and reduction Monitoring lower-cut.
Compared with prior art, the present invention is fast using tera-hertz spectra scanning speed, simple to operate, it is to avoid traditional water body
The problems such as nitrite detection method process is loaded down with trivial details, speed is slow.By setting up pre- between tera-hertz spectra and content of sodium nitrite
Relation mathematic model is surveyed, higher precision of prediction can be obtained.
Description of the drawings
Fig. 1 is the time-domain spectroscopy figure of pure water and inferior sodium nitrate aqueous solution.
Fig. 2 is the frequency domain spectra figure of pure water and inferior sodium nitrate aqueous solution.
Specific embodiment
A kind of nitrite detection method scanned based on tera-hertz spectra of the present embodiment, is comprised the following steps：
(1) prepared by sample：It is 2ml with sodium nitrite and pure water accurate formulation capacity, concentration is 10.1%～34.0%
Sodium nitrite sample solution 240, Concentraton gradient is at intervals of 0.1%.
(2) spectrum is obtained：The solution that a drop configures is taken every time to drip in the thin silicon wafer for reflecting platform in Terahertz, obtains sample
This terahertz time-domain spectroscopy information in 0.2～2.0THz wavelength bands, referring to Fig. 1, and after being fourier transformed (FFT)
Frequency domain spectra information, referring to Fig. 2, wherein pulsewidth l-2ps, temporal resolution 0.067PS, effective time window 16.7PS.
(3) spectroscopic data is processed：The Pretreated spectra of additional dispersion correction (MSC) is carried out again using 9 points of average smooth methods
Algorithm, effectively goes inhalation effects of the eliminating water to tera-hertz spectra, and removes from high-frequency random noises, baseline drift, sample not
Uniformly, light scattering etc. affects.
Characteristic wave bands are extracted：Relative analyses pure water and the frequency domain spectra figure of low concentration sodium nitrite solution, calculate and absorb
Spectrum, according to absorption spectrum find sodium nitrite have characteristic peak at 1.67THz, 1.86THz, 1.45THz wave band, extract this 3
Basis of characterization of the individual characteristic peak as nitrite.Absorption spectrum computing formula is：
Refractive index：
Absorptance：
Wherein, ω, A,C, d, respectively frequency, signal amplitude ratio, signal phase difference, the thickness of the light velocity and sample.
(4) by the sodium nitrite solution of 240 variable concentrations according to 2:1 ratio is divided, and 160 samples of calibration set are tested
Card 80 samples of collection.
Using 160 samples of calibration set, according to the content of sodium nitrite of the characteristic absorption spectrum for extracting and corresponding sample
Set up LS-SVM models.
(5) the LS-SVM models for having set up the characteristic absorption spectrum input of 80 samples of checking collection, obtain corresponding
Predict the outcome.
Wherein LS-SVM models adopt Radial basis kernel function (RBF), using grid data service obtain optimal regular parameter λ and
Kernel parameter σ2Respectively (16,0.0039).
Wherein, training set T={ (x1,y1),(x2,y2),…,(xN,yN)}。αkFor Lagrange multiplier, it is one by N-dimensional
Elementary composition vector：αk=[a1,a1,…aN], belong to N-dimensional real number set RN：αk∈RN。ykFor single element dependent variable, belong to real
Manifold closes R：yk∈R。
It is 0.82 by the detected value of the calculated sodium nitrite solution sample of above-mentioned model and the correlation coefficient of actual value,
Root-mean-square error is 0.95, illustrates that detected value is good with the actual value goodness of fit, shows the Terahertz water nitrite inspection of the present invention
Survey method has preferable practicality.
Claims (7)
1. it is a kind of based on tera-hertz spectra scan nitrite detection method, it is characterised in that include：
(1) configure the sample of the sub- pin acid salt aqueous solution of predetermined concentration scope；
(2) obtain terahertz light spectrum information of each sample in 0.2～2.0THz wavelength bands；
(3) characteristic absorption peak will be extracted after the Terahertz frequency domain spectra information denoising；
(4) model set up between characteristic absorption peak and sub- pin acid salt aqueous solution concentration；
(5) obtain the characteristic absorption peak of water sample to be detected and be input into the model, obtain corresponding sub- pin hydrochlorate Concentration Testing knot
Really.
2. the nitrite detection method for being scanned based on tera-hertz spectra as claimed in claim 1, it is characterised in that step
(1) in, the mass percent concentration scope of multiple samples is 10.1%～34.0%.
3. the nitrite detection method for being scanned based on tera-hertz spectra as claimed in claim 2, it is characterised in that multiple samples
This Concentraton gradient is at intervals of 0.1%.
4. the as claimed in claim 1 nitrite detection method scanned based on tera-hertz spectra, it is characterised in that it is described too
Hertz spectral information includes time-domain spectroscopy information, and the frequency domain spectra information after time-domain spectroscopy information is fourier transformed.
5. the nitrite detection method for being scanned based on tera-hertz spectra as claimed in claim 1, it is characterised in that step
(3) denoising is first to carry out additional dispersion correction again using 9 points of average smooth methods.
6. the nitrite detection method for being scanned based on tera-hertz spectra as claimed in claim 1, it is characterised in that step
(3), in, the absworption peak at 1.67THz, 1.86THz, 1.45THz wave band is extracted as characteristic absorption peak.
7. the nitrite detection method for being scanned based on tera-hertz spectra as claimed in claim 1, it is characterised in that step
(4) model set up is LS-SVM models.
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Cited By (6)
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| CN107024445A (en) * | 2017-04-17 | 2017-08-08 | 中国科学院南京土壤研究所 | The modeling method and detection method of the quick detection of Nitrate in Vegetable |
| CN107703090A (en) * | 2017-10-11 | 2018-02-16 | 浙江大学 | A kind of method of the tera-hertz spectra detection rape leaf moisture content of feature based extraction |
| CN108181259A (en) * | 2017-12-28 | 2018-06-19 | 深圳市太赫兹科技创新研究院有限公司 | The detection method and system of Radix Angelicae Sinensis sample |
| CN108760672A (en) * | 2018-05-22 | 2018-11-06 | 深圳市太赫兹科技创新研究院 | The detection method of melamine |
| CN109001834A (en) * | 2018-06-22 | 2018-12-14 | 天和防务技术（北京）有限公司 | One kind being based on active Terahertz safety inspection method |
| CN109490245A (en) * | 2019-01-04 | 2019-03-19 | 上海理工大学 | Acetone liquid concentration detection method based on terahertz time-domain spectroscopic technology |
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| CN107703090A (en) * | 2017-10-11 | 2018-02-16 | 浙江大学 | A kind of method of the tera-hertz spectra detection rape leaf moisture content of feature based extraction |
| CN108181259A (en) * | 2017-12-28 | 2018-06-19 | 深圳市太赫兹科技创新研究院有限公司 | The detection method and system of Radix Angelicae Sinensis sample |
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| CN109490245A (en) * | 2019-01-04 | 2019-03-19 | 上海理工大学 | Acetone liquid concentration detection method based on terahertz time-domain spectroscopic technology |
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