CN105181672A - Real-time Raman spectrum wavenumber and strength correction method - Google Patents
Real-time Raman spectrum wavenumber and strength correction method Download PDFInfo
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- CN105181672A CN105181672A CN201510621878.1A CN201510621878A CN105181672A CN 105181672 A CN105181672 A CN 105181672A CN 201510621878 A CN201510621878 A CN 201510621878A CN 105181672 A CN105181672 A CN 105181672A
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- 238000001237 Raman spectrum Methods 0.000 title claims abstract description 57
- 238000012937 correction Methods 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 32
- 239000013307 optical fiber Substances 0.000 claims abstract description 53
- 238000001069 Raman spectroscopy Methods 0.000 claims abstract description 40
- 239000000463 material Substances 0.000 claims abstract description 5
- 238000004451 qualitative analysis Methods 0.000 claims abstract description 5
- 238000004445 quantitative analysis Methods 0.000 claims abstract description 5
- 239000012925 reference material Substances 0.000 claims abstract description 5
- 230000003595 spectral effect Effects 0.000 claims description 42
- 239000000523 sample Substances 0.000 claims description 30
- 238000001228 spectrum Methods 0.000 claims description 17
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- 238000004611 spectroscopical analysis Methods 0.000 description 2
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention relates to a real-time Raman spectrum wavenumber and strength correction method, and belongs to the technical field of Raman spectrum measurement. The method comprises the steps that an external reference optical fiber is placed at the same position as a measuring optical fiber, so that the external reference optical fiber is located in the same environment as the measuring optical fiber; a Raman spectrum signal of a reference material is detected, and after a Raman spectrum signal of a to-be-detected material is measured by the measuring optical fiber, signals returned by the optical fibers are transmitted to an FT Raman spectrumeter; wavenumber and strength signal correction of the Raman spectrum signal obtained by the measuring optical fiber is performed by taking the wave crest position and the wave crest strength obtained by the Raman spectrum signal transmitted by the external reference optical fiber as a reference; preprocessing is performed on the corrected Raman spectrum signal of the to-be-detected material, and qualitative and quantitative analysis are achieved. According to the method, wavenumber and strength drifting caused by external factors (such as external environment changing and an unstable light source) can be eliminated to obtain a more stable Raman spectrum signal.
Description
Technical field
The present invention relates to a kind of Raman spectrum wave number and intensity correction method, by External reference thing and fiber multiplex being realized the method for Raman spectrum wave number and intensity stabilization, belonging to raman spectroscopy measurement technical field.
Background technology
When illumination is mapped on Cucumber, in scattered light except the spectral line identical with incident light frequency, also have the spectral line that sub-fraction intensity is extremely weak, frequency changes (namely frequency increases or reduces), this phenomenon is called Ramam effect, also referred to as Raman spectrum.Raman spectrum is the inelastic scattering of reaction molecular vibration and rotation information, so Raman spectrum also belongs to molecular spectrum.Due to Raman spectrum, there is frequency and intensity, polarization etc. indicate scatterer, make Raman spectrum become the Main Means of research structure of matter analytical test.But (be about 10 of incident intensity because Raman light intensity is more weak
-6), and require colourless, without dust, unstressed configuration, and the thirties in last century infrared spectrum technology progress and commercialization make the application of Raman spectrum plummeted.Until the sixties in last century laser technology development Raman technology is revived, due to high brightness, the advantage such as directivity and polarizability of laser beam, become the perfect light source of Raman spectrum.
High-quality Raman spectrum is most important for follow-up qualitative and quantitative analysis.When utilizing Raman spectrum to analyze sample, although without the need to carrying out pre-service to sample, but Raman spectrum is vulnerable to extraneous interference, as: be accused of spike caused etc. in fluorescence and phosphorescence Beijing of the shot noise of laser machine Raman diffused light, the shot noise of ccd detector, dark current noise, sample or container, the blackbody radiation of surrounding environment, environment.The spectrum peak or intensity that directly cause Raman spectrum convert by these, make inaccuracy and the instability of follow-up analysis result.
Summary of the invention
Technical matters to be solved by this invention is to provide a kind of Raman spectrum wave number and intensity real-time correction method, the method is based on External reference thing and fiber multiplex, realize Raman spectrum wave number and intensity real-time stabilization, solve Raman spectrum and be subject to extraneous interference, thus cause the inaccuracy of follow-up analysis result and instable problem.
The present invention is achieved in that a kind of Raman spectrum wave number and intensity real-time correction method, and the step comprised is as follows:
1) External reference optical fiber is set and measuring optical fiber is placed on same position, under making External reference optical fiber and measuring optical fiber be in identical environment, detect the raman spectral signal of reference material, after measuring optical fiber measures the raman spectral signal of material to be detected, the signal that two-beam fibre returns is transported to FT Raman spectrometer;
2) crest location obtained by the raman spectral signal of External reference Optical Fiber Transmission and peak intensity, as reference, carry out wave number and strength signal corrects to the raman spectral signal that measuring optical fiber obtains;
3) pre-service is carried out to the test substance raman spectral signal after correction, realize Qualitative and quantitative analysis.
2, according to Raman spectrum wave number according to claim 1 and intensity real-time correction method, it is characterized in that, described measuring optical fiber and External reference optical fiber placed side by side.
Further, step 2) in the computation process that corrects of wave number be: raman spectral signal and standard spectrum by reference to fibre-optical probe compare, acquisition wave number calibration curve equation: v=v
0+ Dvr, wherein v is that reference optical fiber probe obtains Raman spectrum wave number, v
0for the Raman spectrum of standard spectrum, Dv is wave number rate of change, and r is external disturbance factor, carries out wave number correction by correction equation to the Raman spectrum that measuring optical fiber is popped one's head in.
Further, for intensity correction process be: by reference to the spectral intensity of the specific wave number that fibre-optical probe obtains, then compare with standard spectrum intensity, obtain intensity correction curve I (v)=I
0(v) (1+DI), wherein I (v) spectral intensity of popping one's head in for reference optical fiber, I
0v () is standard spectrum intensity, DI is light intensity rate of change, and the Raman spectrum then measuring optical fiber obtained and intensity correction curve carry out division arithmetic, carry out intensity correction.
Further, step 1) in, adopt fiber multiplex, utilize photoswitch alternately obtaining two-way raman spectral signal with a branch of optical fiber.
Further, step 1) in, utilize two fiber-optic probe system to obtain two-way raman spectral signal simultaneously.
The present invention compared with prior art, beneficial effect is: compared with existing Raman spectrum wave number stabilization technique, the method realizing Raman spectrum wave number and intensity real-time stabilization based on External reference thing and optical fiber multiplexing method of the present invention, the transmission of two-way raman spectral signal can be realized: a road is measuring-signal by wavelength-division multiplex technique or two measuring probe structure, one tunnel is reference signal, realizes by reference to signal the real-time stabilization measuring Raman signal wave number and intensity.
The present invention is based on the method for the real-time Raman spectrum wave number of External reference thing method and intensity correction, extraneous factor (as external environment conversion, flashing the is fixed) wave number that causes and intensity drift can be eliminated, obtain more stable raman spectral signal.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
A kind of Raman spectrum wave number and intensity real-time correction method, comprising:
(1) system building:
External reference optical fiber is set and measuring optical fiber is placed on same position, under making External reference optical fiber and measuring optical fiber be in identical environment, detect the raman spectral signal of reference material, after measuring optical fiber measures the raman spectral signal of material to be detected, the signal that two-beam fibre returns is transported to FT Raman spectrometer; The external environment (as temperature, light intensity etc.) being realized two-way spectral signal by fiber multiplex is identical, thus obtains the Raman spectrum under equivalent environment.Because the External reference thing selected has very strong stability, the Raman spectrum crest location therefore obtained under various circumstances and peak intensity fluctuation have certain rule, correct the peak intensity of test substance Raman spectrum and crest location according to this characteristic.Or two fiber-optic probe system also can be utilized to obtain two-way raman spectral signal simultaneously.
The structure of External reference thing fibre-optical probe is: fibre-optical probe directly contacts the External reference matter sample pond encapsulated with clear glass (transparent referring to absorbs the light thing of use light source), then carries out water proof anti-soil encapsulation with quartz glass.Test substance fibre-optical probe structure is: encapsulated by fibre-optical probe clear glass, thus reduces extraneous test substance to the pollution of fibre-optical probe and adhesion.
(2) spectral measurement
(1) by measuring optical fiber and External reference optical fiber alternately or the Raman spectrum obtaining determinand and External reference material continuously carry out measuring to gather two groups of raman spectral signals; Measuring optical fiber and External reference optical fiber placed side by side, thus ensure Raman spectrum gather environment facies with.
(2) adopt fiber multiplex, utilize photoswitch alternately obtaining two-way raman spectral signal with a branch of optical fiber; Or utilize two fiber-optic probe system to obtain two-way raman spectral signal simultaneously;
(3) the two groups of raman spectral signals obtained are transferred to FT Raman spectrometer, obtain Raman spectrum data by data acquisition software;
(4) crest location obtained by the raman spectral signal of External reference Optical Fiber Transmission and peak intensity, as reference, carry out wave number and strength signal corrects to the raman spectral signal that measuring optical fiber obtains;
The computation process that wave number corrects is: raman spectral signal and standard spectrum by reference to fibre-optical probe compare, acquisition wave number calibration curve equation: v=v
0+ Dvr, wherein v is that reference optical fiber probe obtains Raman spectrum wave number, v
0for the Raman spectrum of standard spectrum, Dv is wave number rate of change, and r is external disturbance factor, carries out wave number correction by correction equation to the Raman spectrum that measuring optical fiber is popped one's head in.
For intensity correction process be: by reference to the spectral intensity of the specific wave number that fibre-optical probe obtains, then compare with standard spectrum intensity, obtain intensity correction curve I (v)=I
0(v) (1+DI), wherein I (v) spectral intensity of popping one's head in for reference optical fiber, I
0v () is standard spectrum intensity, DI is light intensity rate of change, and the Raman spectrum then measuring optical fiber obtained and intensity correction curve carry out division arithmetic, carry out intensity correction.
(5) pre-service is carried out to the test substance raman spectral signal after correction, realize Qualitative and quantitative analysis.
Spectral signal pre-service: wavelet transformation or curve can be utilized to realize the removal of fluorescence background; Smoothly, filtering, Fourier transformation method realize CCD detection noise; Standard normal conversion, multiplicative scatter correction, Orthogonal Signal Correction Analyze, or utilize the intensity at particular spectral peak or area to be normalized as a reference, realize the removal of sample spectra otherness;
Qualitative spectrometric or quantitative test.Qualitatively refer to the analysis that the method by measure spectrum and standard spectrum comparison realizes test substance composition, quantitative test refers to the spectroscopic data being had light by Raman spectrometer acquisition and sample to be tested component, then by the spectroscopic data of known sample collection and the relation of sample to be tested component, the calibration model (i.e. modeling) of property value is set up; Predict finally by the sample of the model set up to unknown component character.Owing to there is linear relationship between sample Raman spectrum spectral strength and the concentration of component of sample, so can quantitative test be realized by modeling.Method can adopt: multiple linear regression, ridge regression, principal component regression, offset minimum binary, artificial neural network, support vector machine, genetic algorithm etc.
The foregoing is only preferred embodiment of the present invention, not in order to limit the present invention, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Claims (6)
1. Raman spectrum wave number and an intensity real-time correction method, is characterized in that, the step comprised is as follows:
1) External reference optical fiber is set and measuring optical fiber is placed on same position, under making External reference optical fiber and measuring optical fiber be in identical environment, detect the raman spectral signal of reference material, after measuring optical fiber measures the raman spectral signal of material to be detected, the signal that two-beam fibre returns is logical is transported to FT Raman spectrometer;
2) crest location obtained by the raman spectral signal of External reference Optical Fiber Transmission and peak intensity, as reference, carry out wave number and strength signal corrects to the raman spectral signal that measuring optical fiber obtains;
3) pre-service is carried out to the test substance raman spectral signal after correction, realize Qualitative and quantitative analysis.
2., according to Raman spectrum wave number according to claim 1 and intensity real-time correction method, it is characterized in that, described measuring optical fiber and External reference optical fiber placed side by side.
3. according to Raman spectrum wave number according to claim 1 and intensity real-time correction method, it is characterized in that, step 2) in the computation process that corrects of wave number be: raman spectral signal and standard spectrum by reference to fibre-optical probe compare, acquisition wave number calibration curve equation: v=v
0+ Δ vr, wherein v is that reference optical fiber probe obtains Raman spectrum wave number, v
0for the Raman spectrum of standard spectrum, Δ v is wave number rate of change, and r is external disturbance factor, carries out wave number correction by correction equation to the Raman spectrum that measuring optical fiber is popped one's head in.
4. according to Raman spectrum wave number according to claim 1 and intensity real-time correction method, it is characterized in that, for intensity correction process be: by reference to the spectral intensity of the specific wave number that fibre-optical probe obtains, then compare with standard spectrum intensity, obtain intensity correction curve I (v)=I
0(v) (1+ Δ I), wherein I (v) spectral intensity of popping one's head in for reference optical fiber, I
0v () is standard spectrum intensity, Δ I is light intensity rate of change, and the Raman spectrum then measuring optical fiber obtained and intensity correction curve carry out division arithmetic, carry out intensity correction.
5., according to Raman spectrum wave number according to claim 1 and intensity real-time correction method, it is characterized in that, step 1) in, adopt fiber multiplex, utilize photoswitch alternately obtaining two-way raman spectral signal with a branch of optical fiber.
6., according to Raman spectrum wave number according to claim 1 and intensity real-time correction method, it is characterized in that, step 1) in, utilize two fiber-optic probe system to obtain two-way raman spectral signal simultaneously.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105737979A (en) * | 2016-03-30 | 2016-07-06 | 广西科技大学 | Method for adopting optical switch to eliminate dark noise drift of array spectrograph |
| CN106404743A (en) * | 2016-11-01 | 2017-02-15 | 北京华泰诺安技术有限公司 | Raman spectrum and near infrared spectrum combined detection method and detection device |
| CN107340547A (en) * | 2017-07-24 | 2017-11-10 | 山东省职业卫生与职业病防治研究院 | A kind of UAV system spectrum detection system and its control method for danger detection operation |
| CN108106732A (en) * | 2017-12-01 | 2018-06-01 | 中国计量科学研究院 | The scaling method and device of Raman spectrometer wavenumber resolution |
| CN108169200A (en) * | 2016-12-07 | 2018-06-15 | 同方威视技术股份有限公司 | For calibrating the method for Raman spectrum detecting device |
| CN111337446A (en) * | 2020-05-08 | 2020-06-26 | 宁波大学 | Biosensor based on chalcogenide glass optical fiber and preparation method thereof |
| CN111670354A (en) * | 2018-02-05 | 2020-09-15 | 伊莱肯兹公司 | Method for analyzing gases by dual illumination |
| CN112763436A (en) * | 2020-12-24 | 2021-05-07 | 中国原子能科学研究院 | Spectrum measuring system |
| CN113190915A (en) * | 2021-04-19 | 2021-07-30 | 东风柳州汽车有限公司 | Vehicle strength evaluation method and system |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105737979A (en) * | 2016-03-30 | 2016-07-06 | 广西科技大学 | Method for adopting optical switch to eliminate dark noise drift of array spectrograph |
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| CN107340547A (en) * | 2017-07-24 | 2017-11-10 | 山东省职业卫生与职业病防治研究院 | A kind of UAV system spectrum detection system and its control method for danger detection operation |
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| CN111670354B (en) * | 2018-02-05 | 2024-01-23 | 伊莱肯兹公司 | Method for analysing a gas by double illumination |
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| CN111337446A (en) * | 2020-05-08 | 2020-06-26 | 宁波大学 | Biosensor based on chalcogenide glass optical fiber and preparation method thereof |
| CN112763436A (en) * | 2020-12-24 | 2021-05-07 | 中国原子能科学研究院 | Spectrum measuring system |
| CN113190915A (en) * | 2021-04-19 | 2021-07-30 | 东风柳州汽车有限公司 | Vehicle strength evaluation method and system |
| CN113190915B (en) * | 2021-04-19 | 2022-07-22 | 东风柳州汽车有限公司 | Vehicle strength evaluation method and system |
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