CN104777144A - Industrial gas multi-component analysis optical path system based on Raman spectrum detection - Google Patents
Industrial gas multi-component analysis optical path system based on Raman spectrum detection Download PDFInfo
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- CN104777144A CN104777144A CN201510116542.XA CN201510116542A CN104777144A CN 104777144 A CN104777144 A CN 104777144A CN 201510116542 A CN201510116542 A CN 201510116542A CN 104777144 A CN104777144 A CN 104777144A
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Abstract
The invention relates to the field of gas spectrum analysis instruments, and relates to an industrial gas multi-component analysis optical path system based on Raman spectrum detection. The system is used to detect industrial gas in a gas cavity (9), and comprises a lens (3), a dichroscope (2), a light filter (4), a convergent lens (5), and a spectrometer (6), which are arranged on a same optical path. A laser (1) is used to generate an excited light beam; the lens (3) is used to focus the excited light beam, the focal point is in the gas cavity (9), the aperture angle of the lens (3) is in a range of 30 to 80 degrees; the diameter of the excited light beam is in a range of 0.5 to 5 mm and is smaller than the diameter of the lens (3), and Raman scattered lights in the front and rear depth fields of the focal point can be coupled into the lens (3). The provided system can enlarge the spacial range of the excited gas, and improve the collection efficiency of Raman scattered signals, and thus the detection sensitivity of the system can be effectively improved.
Description
Art
The present invention relates to gas spectrometer device field, particularly a kind of industrial gasses multicomponent analysis light path system.
Background technology
Along with the fast development of China's economic, industrial gasses are as one of foundation of national economy industry key element, and the critical role in national economy and effect highlight day by day.In the present invention, industrial gasses mainly comprise the whole organic and inorganic gas except inert gas, relate to the process gas product in the fields such as petrochemical complex, oil-gas exploration, Gas Energy Source, iron and steel, cement, food, papermaking, environmental monitoring, energy-saving and emission-reduction or final gaseous product, it accurately fast detects will directly decide operational efficiency and the economic benefit of relevant industries, and provide foundation for the optimal control in later stage.But, due to the complicacy of Multi-Component Gas Analyzing, its detection technique is stagnated for many years, particularly embody a concentrated reflection of the field such as oil-gas exploration, Gas Energy Source, detect while relating to organic and inorganic gas, be difficult to adopt same technology it to be carried out to the detection of space-time uniformity, often need to adopt knockdown gas detection technology, cause the analysis efficiency of related industry low, and have a strong impact on further developing of related industry.
Traditional Multi-Component Gas Analyzing method has: vapor-phase chromatography, infrared spectroscopy, ultraviolet difference photometry, analysis of thermal conductivity method and the electrochemical methods being representative with various electrochemical gas sensor, and these methods are mostly difficult to realize detecting while organic and inorganic gas simultaneously.Wherein vapor-phase chromatography needs to utilize chromatographic column to carry out separation and concentration to gas, time-consuming, effort, costly, and consumptive material needed for instrument is numerous, it is complicated to safeguard, causes its detection efficiency deviation, is difficult to meet the demand that industrial gasses detect in real time.Infrared spectroscopy and ultraviolet difference photometry cannot detect non-polar gas composition, and analysis of thermal conductivity method is non-specific physical detection technology, its sensor application scope is narrower, pot life many factors, and the polycomponent that cannot meet industrial gasses particularly complicated gas detects simultaneously.Although electrochemical gas sensor volume is little, price is low, but it is not high to the resolution of gas, often be subject to environmental gas interference in using and occur wrong report, situation about failing to report, and sensor easily poisoning, serviceable life is low, therefore cannot meet the accuracy requirement that industrial gasses detect.And the Raman spectrum detection technique used in the present invention, then efficiently solve the problem existing for said method.
What early stage Raman spectrum detecting instrument adopted is filter sheet structure, the spectral information that this structure obtains is only some the isolated spectral slice in Raman spectrogram, if publication number is the detection method proposed in the patent of CN104198461A, the method only can analyze 4-16 kind fixed gas composition simultaneously, has certain limitation in commercial Application.
Summary of the invention
The object of the invention is to the above-mentioned deficiency overcoming prior art, a kind of light path system being applicable to the full spectral analysis of polycomponent industrial gasses is provided.Adopt the gas Raman spectral detection system that light path system of the present invention realizes, the high flux polycomponent that can realize industrial gasses detects simultaneously; Higher detection sensitivity is realized by simple mode.Technical scheme of the present invention is as follows:
A kind of industrial gasses multicomponent analysis light path system detected based on Raman spectrum, for detecting the industrial gasses being positioned at air chamber (9), comprising: comprise the lens (3) be arranged in successively in same light path, dichroic mirror (2), light filter (4), convergent lens (5) and spectrometer (6).Wherein,
Laser instrument (1), for generation of excitation beam;
Dichroic mirror (2), for reflects laser topknot, allows Raman scattering light beam to pass through;
Lens (3), for focusing on excitation beam, its focus is positioned at air chamber (9), and the aperture angle scope of lens (3) is at 30 °-80 °; Excitation beam diameter excitation beam diameter, at 0.5mm-5mm, is less than the diameter of lens (3), and the Raman scattering luminous energy before and after focus in field depth is coupled into lens (3);
Light filter (4), for filtering excitation beam;
Convergent lens (5), for converging to spectrometer (6) by Raman diffused light;
Spectrometer (6), for analyzing the Raman diffused light after overconvergence.
Preferably, excitation beam diameter is 1mm, and the aperture angle scope of lens (3) is at 50 °.The present invention also comprises thermostatically-controlled equipment (8), for keeping the temperature stabilization of light path part, to ensure the steady operation of optics.
The present invention proposes a kind of light path system being applicable to industrial gasses multicomponent analysis Raman spectrum and detecting, by to the parameter designing of lens and excitation beam or control, before and after the lens focus focus making to be positioned at air chamber, certain space scope inner laser intensity is all very high, thus increases the spatial dimension of the gas that is excited.And when collecting, the Raman diffused light before and after focus in field depth can be coupled into lens 3, therefore improve the collection efficiency of system to Raman scattering signal, and then effectively improve the detection sensitivity of system.
Accompanying drawing explanation
Fig. 1 is the industrial gasses multicomponent analysis Raman spectrum system adopting light path system of the present invention to realize.
In figure, 1 is laser instrument, and 2 is dichroic mirror, 3 is lens, and 4 is optical filter, and 5 is convergent lens, 6 is spectrometer, and 7 is CCD, and 8 is thermostatically-controlled equipment, 9 is air chamber, and 10 is window, and 11 is air chamber air admission hole, 1213 is reduction valve, 14 is admission line, and 15 is outlet pipe, and 16 is gas circuit heating apparatus.
Fig. 2 is the Raman spectrum of oxygen, nitrogen, methane.
Fig. 3 is the catalogue of the common industrial gasses with Raman spectrum system analysis detection of the present invention.
Embodiment
Below in conjunction with accompanying drawing and application scenarios of the present invention, the present invention is described in detail.
Fig. 1 shows the structural representation of the industrial gasses multicomponent analysis Raman spectrum system adopting light path system of the present invention to realize, and details are as follows.
It is 400nm-1550nm that laser instrument 1 produces wavelength coverage, and power bracket is 50mW-2W, and live width scope is the excitation beam of 0.01nm-0.6nm.
The laser center wavelength that the present embodiment adopts is 450nm, power is the excitation beam of 0.1nm at about 100mW and live width.
The Raman scattering light beam that dichroic mirror 2 allows wavelength longer passes through, and the excitation beam that reflection wavelength is shorter, but only rely on dichroic mirror 2 cannot remove excitation beam completely, therefore need optical filter 4 filtering excitation beam further.
Lens 3 pairs of excitation beams focus on, and its focus is positioned at air chamber 9, and excitation beam diameter, at 0.5mm-5mm, is less than the diameter of lens 3; The aperture angle scope of lens 3 is at 30 °-80 °.The present embodiment adopts diameter to be the light beam of 1mm, and the aperture angle scope of lens 3 is at 50 °.
The present invention controls owing to introducing the depth of field, and excitation beam adopts light pencil incident, during focusing the convergent angle of light beam and the angle of divergence all smaller, therefore before and after focus, certain space scope inner laser intensity is all very high, thus increases the spatial dimension of the gas that is excited.And when collecting, the Raman diffused light before and after focus in field depth can be coupled into lens 3, therefore greatly improve the collection efficiency of system to Raman scattering signal, and then effectively improve the detection sensitivity of system.
Wherein, the excitation beam of optical filter 4 filtering 450nm.
Raman diffused light is converged to the slit place of spectrometer 6 by convergent lens 5.
Spectrometer 6 should be corresponding with the centre wavelength of laser instrument 1 with a point optical range of CCD7, and resolution should be less than 10cm-1, and its F value will match with convergent lens 5, and spectrometer F value used herein is 2.
Thermostatically-controlled equipment 8 by the temperature stabilization of the light path part of Raman spectrum system at about 15 DEG C, to ensure the steady operation of optics.
Air chamber 9 inner length should be not less than 4cm, and the length of the present embodiment is 5cm, to reduce cavity rear end spurious signal to the interference of gas Raman scattered signal.
Window 10 is circular quartz window, thickness 3mm, to ensure that air chamber can not be broken under pressurized state.
Air chamber air admission hole 11 should have certain angle with window 10, is advisable with 30 °, can purge window 10, effectively reduce the dead volume in air chamber 9 simultaneously during to ensure that gas to be measured flows into air chamber 9.
Reduction valve 12,13 for carrying out Isobarically Control to air chamber 9, and to ensure the stability of gas circuit, two reduction valve match simultaneously, and realize cavity supercharging, boost range is between 1 ~ 100 atmospheric pressure.Usually can control at 10 atm higher.In this way, effectively can increase gas molecule quantity in cavity, thus Raman scattering signal intensity is improved 1 ~ 2 order of magnitude.
Industrial gasses enter system by admission line 14, and the gas after analysis discharges system by outlet pipe 15.
Gas circuit heating apparatus 16 is by gas piping, the temperature comprising air chamber 9 and the corresponding parts such as admission line 14, outlet pipe 15 is warmed to more than 50 DEG C, under being all in gaseous state to make whole components of industrial gasses to be measured, thus ensure that accuracy and the stability of analytic system.
Fig. 2 illustrates that system records the Raman spectrum of oxygen, nitrogen, methane.
The industrial gasses multicomponent analysis Raman spectrum system adopting light path system of the present invention to realize, Main Basis Raman scattering effect is to the accurate reflection of gas molecule energy level variations, because the feature of the change of gas molecule energy level and gas molecule structure is closely connected and possesses uniqueness, so Raman spectrum can identify other gas molecule structure except inert gas, accurately distinguish each industrial gasses.Meanwhile, organically combine chemometrics method, the Accurate Determining of industrial gasses component content information can be realized.By the direct measurement of industrial gasses, accurately can estimate value or the harmfulness of gas, as fuel value, greenhouse effect, toxicity etc., being the core composition of the industry on-line analyses such as gas industry, oil-gas exploration, petrochemical complex, iron and steel, cement, food, papermaking, environmental monitoring, energy-saving and emission-reduction, is also the key that related industries realizes optimized control.
Claims (3)
1. the industrial gasses multicomponent analysis light path system detected based on Raman spectrum, for detecting the industrial gasses being positioned at air chamber (9), comprising: comprise the lens (3) be arranged in successively in same light path, dichroic mirror (2), light filter (4), convergent lens (5) and spectrometer (6).Wherein,
Laser instrument (1), for generation of excitation beam;
Dichroic mirror (2), for reflects laser topknot, allows Raman scattering light beam to pass through;
Lens (3), for focusing on excitation beam, its focus is positioned at air chamber (9), the aperture angle scope of lens (3) 30 °-
80 °; Excitation beam diameter excitation beam diameter, at 0.5mm-5mm, is less than the diameter of lens (3), and the Raman scattering luminous energy before and after focus in field depth is coupled into lens (3);
Light filter (4), for filtering excitation beam;
Convergent lens (5), for converging to spectrometer (6) by Raman diffused light;
Spectrometer (6), for analyzing the Raman diffused light after overconvergence.
2. the industrial gasses multicomponent analysis light path system detected based on Raman spectrum according to claim 1, it is characterized in that, excitation beam diameter is 1mm, and the aperture angle scope of lens (3) is at 50 °.
3. Raman spectrum system according to claim 1, is characterized in that, native system also comprises thermostatically-controlled equipment (8), for keeping the temperature stabilization of light path part, to ensure the steady operation of optics.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112666088A (en) * | 2021-01-21 | 2021-04-16 | 上海菁一科技有限公司 | Spectrophotometry test method sample treatment test capsule |
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| FR2292959A1 (en) * | 1974-11-26 | 1976-06-25 | Allied Chem | APPARATUS AND METHOD FOR SPECTROSCOPIC ANALYSIS OF LUMINOUS RADIATION WITH PERIODIC SPECTRAL COMPONENTS |
| JPS5852549A (en) * | 1981-09-24 | 1983-03-28 | Natl Aerospace Lab | Reference cell used for measuring coherent anti-stokes raman scattering spectrum |
| CN101652653A (en) * | 2007-01-29 | 2010-02-17 | 坎布留斯公司 | The chemical analyzer that is used for industrial process control |
| CN102323703A (en) * | 2011-07-27 | 2012-01-18 | 中国科学院长春光学精密机械与物理研究所 | Reflector path optical system based on miniature Raman spectrometer |
| CN102495041A (en) * | 2011-12-08 | 2012-06-13 | 吉林大学 | Optical diagnostic system on basis of laser spontaneous Raman scattered ray imaging |
| CN103822910A (en) * | 2012-11-16 | 2014-05-28 | 福州高意通讯有限公司 | Raman probes for miniature Raman spectrometer |
| CN104198461A (en) * | 2014-09-10 | 2014-12-10 | 宁波海恩光电仪器有限责任公司 | Industrial process gas analyzer based on Raman effect |
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2015
- 2015-05-21 CN CN201510116542.XA patent/CN104777144A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR2292959A1 (en) * | 1974-11-26 | 1976-06-25 | Allied Chem | APPARATUS AND METHOD FOR SPECTROSCOPIC ANALYSIS OF LUMINOUS RADIATION WITH PERIODIC SPECTRAL COMPONENTS |
| JPS5852549A (en) * | 1981-09-24 | 1983-03-28 | Natl Aerospace Lab | Reference cell used for measuring coherent anti-stokes raman scattering spectrum |
| CN101652653A (en) * | 2007-01-29 | 2010-02-17 | 坎布留斯公司 | The chemical analyzer that is used for industrial process control |
| CN102323703A (en) * | 2011-07-27 | 2012-01-18 | 中国科学院长春光学精密机械与物理研究所 | Reflector path optical system based on miniature Raman spectrometer |
| CN102495041A (en) * | 2011-12-08 | 2012-06-13 | 吉林大学 | Optical diagnostic system on basis of laser spontaneous Raman scattered ray imaging |
| CN103822910A (en) * | 2012-11-16 | 2014-05-28 | 福州高意通讯有限公司 | Raman probes for miniature Raman spectrometer |
| CN104198461A (en) * | 2014-09-10 | 2014-12-10 | 宁波海恩光电仪器有限责任公司 | Industrial process gas analyzer based on Raman effect |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112666088A (en) * | 2021-01-21 | 2021-04-16 | 上海菁一科技有限公司 | Spectrophotometry test method sample treatment test capsule |
| CN112666088B (en) * | 2021-01-21 | 2023-03-28 | 上海菁一科技有限公司 | Spectrophotometry test method sample treatment test capsule |
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Application publication date: 20150715 |