CN106596499B - A kind of Raman spectrum real-time calibration method - Google Patents
A kind of Raman spectrum real-time calibration method Download PDFInfo
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Abstract
The invention discloses a kind of Raman spectrum real-time calibration methods, it include: the sample collection location that sample is placed in Raman spectrum acquisition device, laser is opened, the signal acquisition of a length of first duration obtains original spectrum signal S1 when being acquired by Raman spectrum acquisition device, closes laser；The acquisition for carrying out the first duration to bias light obtains background light signal S2；Obtain the difference spectrum signal S of original signal S1 Yu background light signal S2；Laser spectral peak is determined according to signal S, offset Δ ν of the optical maser wavelength relative to laser reference wavelength in this collection process is determined according to the center of laser spectral peak, the Raman spectrum spectral peak that sample is extracted from signal S, the amendment of offset Δ ν is carried out to the Raman spectrum spectral peak of this sample.Raman spectrum calibration method of the invention can be realized without using calibration sample without the operation other than normally detecting, and it is convenient to realize, can effectively improve the Stability and veracity of Raman spectroscopy instrument measurement.
Description
Technical field
The present invention relates to Raman signal processing technology field more particularly to a kind of Raman spectrum real-time calibration methods.
Background technique
The brief introduction of Raman spectrum: Raman spectrum (Raman spectra), is a kind of scattering spectrum.Raman spectrum analysis method
It is the Raman scattering effect found based on India scientist C.V. Raman (Raman), to the scattering different from incident light frequency
Spectrum is analyzed to obtain molecular vibration, rotation aspect information, and is applied to a kind of analysis method of molecular structure research.It draws
Graceful spectral technique with its sensitivity, rapidity and it is easy to operate the advantages that, obtained quick hair in Noninvasive testing field
Exhibition and extensive use.
When illumination is mapped to medium, in addition to Absorption of Medium, reflection and through other than.Always some is scattered, and is scattered
Scattering light including elastic scattering and inelastic scattering elastic scattering is ingredient inelastic scattering identical with excitation wavelength
Scattering light have ingredient longer than excitation wavelength and short, be referred to as Ramam effect.Three can be divided into according to frequency by scattering light
Class.The first kind is caused by certain scattering center (molecule or dust particle), and wave number changes less than 10-5cm- 1Or it is basic
Constant, this kind of scattering is known as Mie scattering；Second class is occurred interaction by the elastic wave in incident light wave field and medium and is produced
Raw scattering, wave number change about 0.1cm- 1, referred to as Brillouin (Brillouin) scattering；The above two classes scattering is generally difficult to
Resolution is collectively referred to as Rayleigh scattering.Third class, wave number variation are greater than 1cm- 1Scattering, be equivalent to molecule rotation, vibration level and electricity
Sub- transition between the energy levels range, referred to as Raman scattering.
The scattering light frequency ν of Raman scattering is changed significantly compared with incident light frequency, i.e. and ν=ν 0 ± | Δ ν |, scattering
Offset of the light frequency ν relative to incident light frequency ν 0, i.e. the frequency displacement Δ ν of Raman spectrum are an important feature amounts of Raman spectrum,
Referred to as Raman shifts.And Raman shifts Δ ν does not change with incident light frequency, is only determined by the property of scatterer.It changes
Sentence is talked about, and can obtain similar Raman shifts under the monochromatic incidence of different frequency.Raman spectrometer is visited by Raman spectrum
Head and spectroanalysis instrument composition, the spectral component for the optical signal that spectroanalysis instrument is arrived for analysis detection, data are exported with absolute
Wavelength nm (or frequency domain wave number cm-1) be unit spectroscopic data.To be converted to Raman shifts, need known laser wavelength ν's 0
On the basis of do subtractive.
It is true usually to carry out calibration measurement for the wavelength of laser when laser dispatches from the factory or when Raman spectrometer dispatches from the factory
It is fixed.But the wavelength of laser can be because small drift occurs for environment temperature, fluctuation of electronic circuit etc..It applies in Raman spectrum
Laser on instrument is usually higher to the stability requirement of optical maser wavelength, it is desirable that ± 2cm-1Or it is higher, stability parameter is direct
Influence the Raman shifts measurement accuracy of instrument.
Its optical maser wavelength is possible to send out after long-time service, environmental change, long-distance transport etc. after Raman spectrometer factory
Raw drift, it will usually optical maser wavelength is modified by modes such as self calibrations.Common method for self-calibrating is: measuring certain mark
The Raman spectrum of quasi- substance (such as polystyrene), and compared with the standard spectrogram of the standard substance, and then learn laser wave
Long offset.The shortcomings that existing self-alignment method, is do not have real-time, can only give a constant amendment
Value, and carry out self-alignment condition under what state and be difficult to grasp.
Summary of the invention
In order to solve the problems, such as that the calibrating mode of Raman spectrum in the prior art does not have real-time and operating process is complicated,
The present invention provides a kind of Raman spectrum real-time calibration methods.
The present invention provides a kind of spectral signal real-time calibration methods, comprising:
Step 1, sample is placed in the sample collection location of Raman spectrum acquisition device, laser is opened, passes through Raman
The signal acquisition of spectra collection device a length of first duration when being acquired obtains original spectrum signal S1, closes the laser
Device；
Step 2, the acquisition of first duration is carried out to bias light by the Raman spectrum acquisition device, obtains background
Optical signal S2；
Step 3, the difference spectrum signal S of the original signal S1 Yu the background light signal S2 is calculated；
Step 4, laser spectral peak is determined according to the difference spectrum signal S, the center according to the laser spectral peak is true
Offset Δ ν of the optical maser wavelength relative to laser reference wavelength in this fixed collection process, from the difference spectrum signal S
The Raman spectrum spectral peak for extracting the sample carries out the offset Δ ν's to the Raman spectrum spectral peak of this sample
Amendment.
Above-mentioned spectral signal real-time calibration method also has the following characteristics that
Between the step 1 and step 2 further include: judge whether the signal strength of the original signal S1 is located at default model
Enclose, if it is greater than or equal to preset range the upper limit, reduce laser laser power and/or reduce acquisition duration after carry out weight
New acquisition, the duration resurveyed is as first duration；If it is less than the lower limit of preset range, the laser of laser is improved
It power and/or is resurveyed after improving acquisition duration, when a length of first duration resurveyed.
Above-mentioned spectral signal real-time calibration method also has the following characteristics that
Notch filtering light piece meets the following conditions in the Raman spectrum acquisition device: making the spectra collection device acquisition
It include laser spectral peak in original spectrum signal S1.
Above-mentioned spectral signal real-time calibration method also has the following characteristics that
The optical density parameter of the notch filtering light piece is the value between 6 to 8.
Raman spectrum calibration method of the invention, can be real without the operation other than normally detecting without using calibration sample
Existing, it is convenient to realize, can effectively improve the Stability and veracity of Raman spectroscopy instrument measurement.
Detailed description of the invention
Fig. 1 is the flow chart of Raman spectrum real-time calibration method in embodiment；
Fig. 2 is the effect picture of initial data when wavelength calibration is not used；
Fig. 3 is the effect picture that alignment mode of the present invention is used in specific embodiment.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention
In attached drawing, technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is
A part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art
Every other embodiment obtained without making creative work, shall fall within the protection scope of the present invention.It needs
Illustrate, in the absence of conflict, the features in the embodiments and the embodiments of the present application can mutual any combination.
Fig. 1 is the flow chart of Raman spectrum real-time calibration method in embodiment.With reference to Fig. 1, spectral signal real time calibration side
Method, comprising:
Step 1, sample is placed in the sample collection location of Raman spectrum acquisition device, laser is opened, passes through Raman
The signal acquisition of spectra collection device a length of first duration when being acquired obtains original spectrum signal S1, closes laser；
Step 2, the acquisition of the first duration is carried out to bias light by Raman spectrum acquisition device, obtains background light signal
S2；
Step 3, the difference spectrum signal S of original signal S1 Yu background light signal S2 is calculated；
Step 4, laser spectral peak is determined according to difference spectrum signal S, is this time adopted according to the determination of the center of laser spectral peak
Offset Δ ν of the optical maser wavelength relative to laser reference wavelength during collection, extracts sample from difference spectrum signal S
Raman spectrum spectral peak, the amendment of offset Δ ν is carried out to the Raman spectrum spectral peak of this sample.That is Raman spectrum spectral peak
Spectrum peak position is νiWhen, the position of revised spectrum spectral peak is νi=νi+Δν。
Wherein, between step 1 and step 2 further include: judge whether the signal strength of original signal S1 is located at preset range,
If it is greater than or equal to preset range the upper limit, reduce laser laser power and/or reduce acquisition duration after carry out again
Acquisition, when a length of first duration resurveyed；If it is less than the lower limit of preset range, improve laser laser power and/
Or it is resurveyed after improving acquisition duration, when a length of first duration resurveyed.
Original spectral signal S1 includes sample spectrum, laser spectrum and bias light spectrum in this method.In order to make original
Beginning spectral signal S1 includes effective laser spectrum, and notch filtering light piece meets the following conditions in Raman spectrum acquisition device: making light
Composing includes laser spectral peak in the original spectrum signal S1 of acquisition device acquisition.Preferably, the optical density parameter of notch filtering light piece is 6
Value between to 8.
Specific embodiment:
Fig. 2 is the effect picture of initial data when wavelength calibration is not used；Such as to the initial data of measurement three times of certain a sample
Shown in Fig. 2, due to the fluctuation of laser, there are biggish offset before the spectral peak measured three times, the main peak measured three times is respectively
995.8cm-1、1001cm-1、1007cm-1, measurement data is inconsistent, and repeatability, the stability of data are poor, will affect when serious
The accuracy matched.
Fig. 2 is the effect picture for the data that method of the invention carries out after wavelength calibration, as shown in figure 3, the wave measured three times
Long correction amount ν is respectively 5.577cm-1、0.855cm-1、-5.545cm-1, the main peak measured three times after amendment is all 1002cm-1, measurement data is consistent, so as to improve repeatability, the stability of system, reduces measurement error.
Raman spectrum calibration method of the invention, can be real without the operation other than normally detecting without using calibration sample
Existing, it is convenient to realize, can effectively improve the Stability and veracity of Raman spectroscopy instrument measurement.
In addition, it should be noted that, the specific embodiments described in this specification, the shape of parts and components are named
Title etc. can be different, and above content is only to structure of the invention example explanation described in this specification.
Descriptions above can combine implementation individually or in various ways, and these variants all exist
Within protection scope of the present invention.
Herein, the terms "include", "comprise" or any other variant thereof is intended to cover non-exclusive inclusion, from
And make the article for including a series of elements or equipment not only includes those elements, but also its including being not explicitly listed
His element, or further include for this article or the intrinsic element of equipment.In the absence of more restrictions, by language
The element that sentence " including ... " limits, it is not excluded that there is also other identical in the article or equipment for including the element
Element.
The above examples are only used to illustrate the technical scheme of the present invention and are not limiting, reference only to preferred embodiment to this hair
It is bright to be described in detail.Those skilled in the art should understand that can modify to technical solution of the present invention
Or equivalent replacement should all cover in claim model of the invention without departing from the spirit and scope of the technical solution of the present invention
In enclosing.
Claims (4)
1. a kind of spectral signal real-time calibration method characterized by comprising
Step 1, sample is placed in the sample collection location of Raman spectrum acquisition device, laser is opened, passes through Raman spectrum
The signal acquisition of a length of first duration when acquisition device is acquired obtains original spectrum signal S1, closes the laser；
Step 2, the acquisition of first duration is carried out to bias light by the Raman spectrum acquisition device, obtains bias light letter
Number S2；
Step 3, the difference spectrum signal S of the original signal S1 Yu the background light signal S2 is calculated；
Step 4, laser spectral peak is determined according to the difference spectrum signal S, this is determined according to the center of the laser spectral peak
Offset Δ ν of the optical maser wavelength relative to laser reference wavelength in secondary collection process is extracted from the difference spectrum signal S
The Raman spectrum spectral peak of the sample carries out the amendment of the offset Δ ν to the Raman spectrum spectral peak of this sample.
2. spectral signal real-time calibration method as described in claim 1, which is characterized in that
Between the step 1 and step 2 further include: judge whether the signal strength of the original signal S1 is located at preset range,
If it is greater than or equal to preset range the upper limit, reduce laser laser power and/or reduce acquisition duration after carry out again
Acquisition, the duration resurveyed is as first duration；If it is less than the lower limit of preset range, the laser function of laser is improved
It rate and/or is resurveyed after improving acquisition duration, when a length of first duration resurveyed.
3. spectral signal real-time calibration method as claimed in claim 1 or 2, which is characterized in that
Notch filtering light piece meets the following conditions in the Raman spectrum acquisition device: making the original of the spectra collection device acquisition
It include laser spectral peak in spectral signal S1.
4. spectral signal real-time calibration method as claimed in claim 3, which is characterized in that
The optical density parameter of the notch filtering light piece is the value between 6 to 8.
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| WO2019080013A1 (en) * | 2017-10-25 | 2019-05-02 | 深圳达闼科技控股有限公司 | Raman detection method and apparatus, storage medium, and electronic device |
| WO2019084817A1 (en) * | 2017-10-31 | 2019-05-09 | 深圳达闼科技控股有限公司 | Method and device for determining focus deviation, storage medium and electronic apparatus |
| CN108169208B (en) * | 2018-01-17 | 2020-08-25 | 南开大学 | Raman spectrum detector calibration method |
| JP6791213B2 (en) * | 2018-07-13 | 2020-11-25 | 横河電機株式会社 | Spectral analyzer and spectroscopic analysis method |
| CN110865067B (en) * | 2019-12-02 | 2022-01-25 | 中国检验检疫科学研究院 | Method for rapidly calibrating Raman spectrometer by using acetaminophen |
| CN113984735B (en) * | 2021-10-27 | 2024-04-16 | 北京华泰诺安探测技术有限公司 | Quantitative detection method and system based on Raman spectrum and Raman spectrometer |
| CN113984734B (en) * | 2021-10-27 | 2024-04-05 | 北京华泰诺安探测技术有限公司 | Background subtraction detection method and system for Raman spectrum and Raman spectrometer |
| CN115266681B (en) * | 2022-09-27 | 2022-12-16 | 南京诺源医疗器械有限公司 | High-precision scanning and rapid marking method for medical Raman spectral imaging |
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