CN201983859U - Online Raman spectrometer correcting device - Google Patents

Online Raman spectrometer correcting device Download PDF

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Publication number
CN201983859U
CN201983859U CN201120068485XU CN201120068485U CN201983859U CN 201983859 U CN201983859 U CN 201983859U CN 201120068485X U CN201120068485X U CN 201120068485XU CN 201120068485 U CN201120068485 U CN 201120068485U CN 201983859 U CN201983859 U CN 201983859U
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China
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raman spectrometer
raman
laser
online
optical fiber
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CN201120068485XU
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程明霄
林锦国
张赛军
张进明
赵天琦
蒋书波
於拯威
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Nanjing Tech University
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Nanjing Tech University
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Abstract

The online Raman spectrometer correction device detects the laser power of a laser of an online Raman detection system as reference power, corrects the laser power and the spectrogram position of the online Raman spectrometer in real time by using the position of a Raman spectrum peak obtained by a neon monochromatic source as a reference position, and realizes the correction when the laser power is reduced or deviated and the correction when the spectrogram horizontally deviates under the long-time working condition of the online Raman spectrometer, thereby achieving the long-term effective work of the online Raman spectrometer in a severe environment and ensuring the long-term effective field sample detection of the online Raman spectrometer.

Description

A kind of online Raman spectrometer means for correcting
Technical field
The utility model belongs to field of photoelectric technology, be used for the laser power correction and the spectrogram level correction of online Raman spectrometer, realize that online Raman spectrum works long hours under the situation, laser power descends or the correction when correction when departing from and spectrogram offset, thereby reach the permanently effective work under the online Raman spectrometer rugged surroundings, be a kind of online Raman spectrometer means for correcting.
Background technology
The Raman spectrum analysis technology is a kind of contactless spectral analysis technique based on Raman scattering effect, and it can carry out qualitative, quantitative test to the composition and the structure of material.Raman spectroscopy measurement speed is fast, uses Raman spectrum analysis and can accomplish that original position measures in real time, helps the real time on-line monitoring of process control.After laser appears in nineteen sixty, because advantages such as characteristics such as laser has that monochromaticity is good, concentration of energy, output power are big, especially spectral radiance density height, lasing light emitter volume are little, in light weight, easy automation mechanized operation, so very fast laser is used for the excitation source of Raman spectrometer, thereby makes Raman spectrum obtain new starting point.The Raman spectroscopy of the laser Raman spectroscopy light source that produces.Characteristics such as using laser and have that monochromaticity is good, high directivity, brightness height, coherence are good combines with surface-enhanced Raman effects, has just produced Surface enhanced raman spectroscopy.The conventional Raman spectrum of its remolding sensitivity can improve 10^4~10^7 doubly, and the signal to noise ratio (S/N ratio) of analysis is improved greatly.
Parameter such as traditional process industry working pressure, flow, temperature etc. are indirectly controlled device.We have been incorporated into online raman monitoring device certain petrochemical industry PX device now, can carry out fully directly carrying out direct FEEDBACK CONTROL at the specific targets of product.To produce far-reaching influence to the future of process industry.
In the actual at the scene Raman spectrum quantitative test, the processing of Raman spectrum diagram data is the key in the whole Raman spectrum analysis flow process, has only the reliability height of signal, just can talk about its qualitative, quantitative precision.Yet in the use of reality, laser instrument uses in the rugged environment relatively long-time, phenomenons such as laser power decline departs from can appear, and the power of raman spectral signal and laser power exist certain proportionate relationship, when laser power descends, Raman signal also descends thereupon, thereby influences the accurate letter of Raman spectrogram, brings uncertain influence to measuring to detect.The vibrations of grating can take place in the while unavoidably in use at long-term scene and the stop position that brings that expands with heat and contract with cold is offset, and cause the situations such as horizontal-shift of Raman spectrum imaging.Therefore the Raman spectrometer of on-the-spot long-term online use need a kind of effective instrument calibration system with guarantee its long-term testing accurately, reliable.
Summary of the invention
Problem to be solved in the utility model is: when online Raman spectrometer applies in the arene adsorptive separation apparatus, use under the long-time rugged surroundings, laser power can occur descends or wild effect, and expanding with heat and contract with cold, producing the Raman spectrum spectrogram horizontal drift phenomenon that obtains under the situation such as grating vibrations, when Raman spectrum detects, need proofread and correct at the spectrogram strength variance that these situations cause, to guarantee the validity accuracy of Raman detection.
The technical solution of the utility model is: a kind of online Raman spectrometer means for correcting, laser instrument provides the excitation source of Raman detection for Raman spectrometer, means for correcting comprises beam split optical fiber, laser attenuation module, 45 ° of equidistant gratings and photoelectric detector, the output laser of laser instrument tells one the tunnel through beam split optical fiber, successively through laser attenuation module, 45 ° of equidistant grating input photoelectric detectors.
The laser attenuation module is 2 90% a attenuator.
Further, means for correcting also is provided with the neon lamp monochromatic source, the output light source of neon lamp monochromatic source is incorporated on the sample detection optical fiber of Raman spectrometer through optical fiber, import Raman spectrometer with Raman detection light, the output light source distribution of the grating pair neon lamp monochromatic source of Raman spectrometer is fixed into the image position.
The utility model timing, laser instrument emitted laser under the original state that online Raman spectrometer moves at the beginning, carry out beam split by beam split optical fiber, the laser input laser attenuation module that beam split obtains is carried out attenuation processing, obtain the light of former laser intensity 1%, light after the decay is carried out homogenising by 45 ° of equidistant gratings to be handled, import photoelectric detector again and obtain light intensity, thereby the size of the laser power of laser instrument output under the acquisition original state, with the laser power that obtains as reference power, in the process of online Raman spectrometer operation, the laser power of raman spectral signal intensity correspondence in real time and reference power compare, judge whether raman spectral signal intensity departs from, and obtain the laser power correction amount of laser instrument by the relation of laser power and raman spectral signal intensity.
Further, also carry out the level correction of Raman spectrogram: be fixed into the image position on the Raman spectrometer grating, for the output light source distribution of neon lamp monochromatic source, carry out sample detection simultaneously at Raman spectrometer, be incorporated on the sample detection optical fiber of Raman spectrometer with the light source of an optical fiber the emission of neon lamp monochromatic source, import with Raman detection light and to carry out imaging in the Raman spectrometer, obtain the position of raman spectra of the output light source of neon lamp monochromatic source, it is made as the reference position, in real time the Raman spectrogram position of Raman detection light is proofreaied and correct by described reference position.
The laser power of online Raman spectrum and the real-time correction of spectrogram position have been realized in the technical solutions of the utility model, by to the correction of laser power and the level correction of spectrogram, overcome that laser power that online Raman spectrometer under the long-time rugged surroundings occurs easily descends and grating shakes the spectrogram that brings and is offset inaccurate influence, guaranteed online Raman spectrometer permanently effective carry out sample detection at the scene.
Description of drawings
Fig. 1 is the structural representation of the utility model device laser power correction part.
Fig. 2 is the structural representation of the utility model device spectrogram level correction part.
Embodiment
The utility model means for correcting comprises laser instrument light intensity correction portion 2 and spectrogram rectification part, and two parts independently operate, and combines the correction work of improving that can realize online Raman spectrometer.
As Fig. 1, laser instrument light intensity correction portion is: laser instrument 1 provides the excitation source of Raman detection for online Raman spectrometer 4, laser power correction partly comprises beam split optical fiber 21,22,45 ° of equidistant gratings 23 of laser attenuation module and photoelectric detector 24, the output laser of laser instrument 1 tells one the tunnel through beam split optical fiber 21, successively through 22,45 ° of equidistant grating 23 input photoelectric detectors 24 of laser attenuation module.Here laser attenuation module 22 is 2 90% a attenuator.Excitation source is by optical fiber input test sample 5, and 4 pairs of test sample of online Raman spectrometer 5 are carried out Raman detection.Online Raman spectrometer 4 correspondences are connected with computing machine 6 and carry out the online data processing.
As Fig. 2, on the basis of laser instrument light intensity correction portion, further increase spectrogram level correction part, comprise neon lamp monochromatic source 3, the output light source of neon lamp monochromatic source 3 is incorporated on the sample detection optical fiber of Raman spectrometer through optical fiber, import Raman spectrometer 4 with Raman detection light, the output light source distribution of the grating pair neon lamp monochromatic source 3 of Raman spectrometer 4 is fixed into the image position.
The utility model device is applied to the spectrogram corrective system of Raman spectrometer on the petrochemical industry arene adsorptive separation apparatus, because on-the-spot more complicated, abominable in the arene adsorptive separation apparatus, online Raman spectrum detects the scope position preferable states in 150m by fiber optic conduction, so means for correcting of the present utility model is placed in online Raman detector agent set and analyzes in the cabin, the structure upper volume of the utility model device is less, more convenient simultaneously.
Below in conjunction with preferred embodiment, embodiment, feature and effect thereof that foundation the utility model is provided, after the detailed description, for purpose simply clearly, hereinafter appropriate omission known technology description in case the influence of those unnecessary details to the description of the technical program.
Correction for laser power, when online Raman spectrometer has just been brought into operation, laser instrument 1 emitted laser under the original state just, carry out beam split by beam split optical fiber 21, the laser input laser attenuation module 22 that beam split obtains is carried out attenuation processing, obtain the light of former laser intensity 1%, because there is the problem of uneven homogenize in the laser that obtains, light after the decay is carried out the homogenising processing by 45 ° of equidistant gratings 23 import photoelectric detector 24 again, can fast and effeciently detect light intensity when guaranteeing to detect in the photoelectric detector 24, obtain the size of the laser power of laser instrument 1 output under the original state by photoelectric detector 24, with the laser power that obtains as reference power, operation along with online Raman spectrometer, the laser power of raman spectral signal intensity correspondence in real time and reference power compare, judge whether raman spectral signal intensity departs from, and obtain the laser power correction amount of laser instrument 1 by the relation of laser power and raman spectral signal intensity.For example, by the relation of laser power and Raman signal intensity, extrapolate at the scene under the actual conditions the pairing laser power of the intensity of Raman spectrogram reality, can find with the reference power contrast whether laser instrument phenomenons such as laser power decline departs from occur, thereby proofread and correct.
For the level correction of Raman spectrogram: a neon lamp monochromatic source 3 is set, and be fixed into the image position on Raman spectrometer 4 gratings, for the output light source distribution of neon lamp monochromatic source 3, carry out sample detection simultaneously at Raman spectrometer 4, be incorporated on the sample detection optical fiber of Raman spectrometer 4 with the light source of an optical fiber 3 emissions of neon lamp monochromatic source, import in the Raman spectrometer 4 with Raman detection light, carry out imaging by Raman spectrometer CCD imaging system, because the only monochromatic light that neon lamp monochromatic source 3 is launched, and through of the fixed position imaging of designs fix light neon source at Raman spectrometer 4 gratings, then can obtain the position of raman spectra of the output light source of neon lamp monochromatic source 3, it is made as the reference position, if Raman spectrometer uses under rugged surroundings for a long time, the grating of Raman spectrometer vibrations or owing to reason such as expand with heat and contract with cold can cause moving horizontally of spectrogram, in real time the Raman spectrogram position of Raman detection light is proofreaied and correct by described reference position, obtain desirable spectrogram.
The utility model scheme is in the on-the-spot use of certain petrochemical industry aromatic device at present, and what laser instrument adopted is 532 semiconductor pumped formula laser instruments; Optical fiber is multimode optical fiber; Attenuator is selected two 90% intraocular lens optic attenuators for use, and its effect is for to decay to 1% of former intensity with laser intensity; Photoelectric detector is a photodiode.Raman spectrometer is the online Raman spectrometer of RMAN630 type.
The utility model is at the straightened up in place of online Raman spectrum analysis instrument, and the normal operation of Raman spectrometer is carried out and do not influenced to whole trimming process in real time, guaranteed online Raman spectrometer permanently effective carry out sample detection at the scene.The means for correcting structure realizes that easily volume simple in structure is little, and is good with conventional online Raman spectrum analysis instrument adaptability.

Claims (3)

1. online Raman spectrometer means for correcting, laser instrument (1) provides the excitation source of Raman detection for Raman spectrometer (4), it is characterized in that means for correcting comprises beam split optical fiber (21), laser attenuation module (22), 45 ° of equidistant gratings (23) and photoelectric detector (24), the output laser of laser instrument (1) tells one the tunnel through beam split optical fiber (21), successively through laser attenuation module (22), 45 ° of equidistant gratings (23) input photoelectric detector (24).
2. a kind of online Raman spectrometer means for correcting according to claim 1 is characterized in that laser attenuation module (22) is 2 90% a attenuator.
3. a kind of online Raman spectrometer means for correcting according to claim 1 and 2, it is characterized in that means for correcting also is provided with neon lamp monochromatic source (3), the output light source of neon lamp monochromatic source (3) is incorporated on the sample detection optical fiber of Raman spectrometer through optical fiber, import Raman spectrometer (4) with Raman detection light, the output light source distribution of the grating pair neon lamp monochromatic source (3) of Raman spectrometer (4) is fixed into the image position.
CN201120068485XU 2011-03-15 2011-03-15 Online Raman spectrometer correcting device Expired - Lifetime CN201983859U (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102121902A (en) * 2011-03-15 2011-07-13 南京工业大学 Online Raman spectrometer correction device and correction method thereof
CN103175822A (en) * 2013-02-06 2013-06-26 中国食品药品检定研究院 Method for eliminating table difference of Raman spectrometer
CN110865067A (en) * 2019-12-02 2020-03-06 中国检验检疫科学研究院 Method for rapidly calibrating Raman spectrometer by using acetaminophen

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102121902A (en) * 2011-03-15 2011-07-13 南京工业大学 Online Raman spectrometer correction device and correction method thereof
CN102121902B (en) * 2011-03-15 2012-10-24 南京工业大学 Online Raman spectrometer correction device and correction method thereof
CN103175822A (en) * 2013-02-06 2013-06-26 中国食品药品检定研究院 Method for eliminating table difference of Raman spectrometer
CN103175822B (en) * 2013-02-06 2015-08-05 中国食品药品检定研究院 Eliminate the method for table difference of Raman spectrometer
CN110865067A (en) * 2019-12-02 2020-03-06 中国检验检疫科学研究院 Method for rapidly calibrating Raman spectrometer by using acetaminophen
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

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