CN106442404A - Real-time on-line multi-component monitoring optical system for stable gas isotopes - Google Patents
Real-time on-line multi-component monitoring optical system for stable gas isotopes Download PDFInfo
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- 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
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Abstract
The invention discloses a real-time on-line multi-component monitoring optical system for stable gas isotopes. The system comprises a laser module, an absorption cell module, a temperature control box and a data processing module. In combination with wavelength scanning, multipass cell adjustment and accurate control of in-cell pressure, temperatures and wavelengths, four trace gas concentrations and isotopes can be monitored in real time on line by the aid of a single multipass cell, and sample preparation is not required in the measurement process. The problems of the heavy weight and the large size of measurement instruments and the inconvenience in carrying the measurement instruments when a balancing detection method is used for measuring a single gas isotope and the problems about measurement results and accuracy because of pressure and temperature control difference during measurement by the aid of two cells are solved, and the limitation that a single multipass cell can only measure one gas isotope is overcome. The whole optical system is compact in size and simple to operate, doesn't require calibration and can monitor the abundance and the concentration of the stable isotopes of four atmospheric pollution gases in real time on line. The system is high in integration degree and can monitor the pollution gas source in the dangerous environment in real time on line.
Description
Technical field
The present invention relates to atmospheric stability isotope abundance field of optical detection, more particularly to a kind of multicomponent gases are stably same
The plain real time on-line monitoring optical system in position.
Background technology
Stable isotope detection technology is in the microenvironment mechanism and really of generation, transmission and the release for disclosing Pollution Gas
Determine in terms of Relative Contribution rate with obvious superiority.Atmospheric molecule Isotope Compositions can reflect atmospheric molecule composition source
The original state in area and the weather system change of Variation Features, large scale.The application of stable isotope is to climate change, environment dirt
The improvement of dye thing has impetus and practical advice meaning, can more preferably understand regional climate characteristics and law study.High-precision
The atmospheric stability isotope measure method of degree has non-to accurate parsing source remittance Variation Features and variation tendency, the measurement error that reduces
Often important meaning, plays more and more important effect in atmospheric environment field of scientific study.
The standard technique for determining isotope abundance is isotopic ratio mass spectrum（IRMS）Technology.The commercial measurement high precision,
But service requirement is also higher, it is difficult to carry out existing field real-time measurement.Particularly to the isotopic measurement of steam, it usually needs tens
Minute gathers steam in several hours from air, then steam is processed and is analyzed, and IRMS technology can not be distinguished
Isomerss molecule isotope, these features limit on-line analysis ability of the IRMS technology to sample.
The spectral technique for developing in recent years overcomes the restriction of traditional IRMS technology.Laser absorption spectroscopy is used for air
Molecule Stable isotope detection, is developing progressively an advanced subject of spectrum of use and isotope analyses research field.Mainly
There is tunable diode laser technology（TDLAS）, quanta cascade laser absorption spectroscopy（QCLAS）, cavity ring-down spectroscopy skill
Art（CRDS）And Fourier transform infrared（FTIR）Spectral technique etc..Laser technology generally analyzes isotopic rotation-vibration jump
The one or more short-wave bands to be formed are moved, its certainty of measurement is higher.However, the usual complex structure of QCLAS, CRDS and FTIR, becomes
This costliness, can only measure a kind of gas isotope abundance, unsuitable for the high sensitivity isotope detection for developing into real-time monitoring
Instrument.TDLAS technology is obtained using diode laser length scanning characteristic in the range of the characteristic absorption spectrum of tested gas
Absorption spectrum, so as to carry out a kind of technology of qualitative or quantitative analyses to dusty gass isotope.The technology has sensitive
Degree is high, selectivity is good, without the need for sampling and sample treatment, can in real time, dynamic, quick, multicomponent be while the advantages of measuring, can develop
Become multicomponent, portable isotope detection device.
Foreign countries have carried out TDLAS stable isotope detection method research from the nineties in last century, but are all pure gases
Stable isotope measurement, has been used successfully to the detection of saturn's atmosphere methane isotope abundance now.Domestic TDLAS stable isotope
Detection belongs to the starting stage, mainly measures around pure gases isotope.Multi-wavelength multicomponent is carried out using TDLAS steady
Determine isotopic abundance measurement system to realize simply, optical fiber coupled modes make system be easily adapted to measuring environment and miniaturization.Swashing
In light device wavelength scanning range, in the case of selecting two Absorption Lines not by other gas componants and its change interference, only to
Ask measurement gas pressure intensity not so high and do not reacted with other gases, it becomes possible to realize non-invasive real-time online stable
Isotope is monitored.In addition, multi-wavelength multicomponent stable isotope abundance measurement device is easily integrated, programming manipulation, without the need for fixed
Mark, can keep prolonged stability, be easy to carry, can carry out field trial, and Pollution Gas source, remittance are changed and I
The research of state's environmental pattern has great importance.
Content of the invention
The invention aims to a kind of multicomponent gases stable isotope abundance measurement system is provided, system structure letter
Single, with preferable pressure and temperature stability, the measurement of four kinds of gas stable isotope abundance can be carried out simultaneously, solve and work as
Front instrument can only can carry out long-term real-time online observation, with respect to single gas to the shortcoming of pure gases isotopic abundance measurement
Body isotope measure device, present invention reduces the cycle of analysis isotope abundance, can system comprehensively to study air main
The source of dusty gass and the dynamic change that converges, grasp its concentration spatial-temporal characteristics.
The present invention adopts tunable diode absorption spectroscopy techniques, according to Lambert-Beer's law selectively to big temperature
Room gas stable isotope abundance is measured.
The technical solution of the present invention：A kind of off-axis stable isotope Measuring abundance of U-bar system of multi-wavelength, including laser instrument
Module, absorption cell module, temperature control box and Signal acquiring and processing module.
The laser module is by four optical fiber output lasers, laser controller, functional generator and band meter composition；
Also include splitting ratio connected with laser instrument for 99:1 fiber optic splitter, optical fiber couples flange, fiber optic collimator camera lens is housed
Three-dimensional trim holder；Laser fiber outfan is connected with fiber optic splitter by optic fibre switching flange；Fiber optic splitter splitting ratio
Big one is connected on the three-dimensional trim holder equipped with fiber optic collimator camera lens, and little one is connected splitting ratio with band meter.
The absorption cell module mainly has corrugated tube, transparent Teflon pipe, concave spherical mirror, calcium fluoride eyeglass, switching
Flange, sealing flange, multidimensional adjustment frame, air valve door, detector, firm banking and attemperating unit composition；
One end of one end of the corrugated tube and transparent Teflon pipe is linked together by adapter flange, corrugated tube and thoroughly
The other end of bright polyfluortetraethylene pipe is connected with the adapter flange for being fixed with incident concave spherical mirror and outgoing concave spherical mirror respectively, close
Envelope flange is fixed together with calcium fluoride eyeglass and is arranged on outside the adapter flange equipped with concave spherical mirror, thus constitutes many logical suctions
Receives pond；The side that many logical ponds are provided with corrugated tube is the incidence end of light；The multidimensional adjustment frame and incidence end sealing flange
It is fixedly connected on base；One end that many logical ponds are provided with transparent Teflon pipe is the exit end of light；The detection
Device installed in the exit ends for leading to pond more；The air intake valve and outlet valve are separately mounted to pond incidence end and the exit ends of leading to more
On sealing flange；The air inlet valve and gas outlet valve are connected with outside gas circuit respectively.
The concave spherical mirror for leading to pond is coated with golden film more, a width of 800 nm～20 μm of the band of its reflected light, average reflectance
For 96%.Its clear aperature is 20cm, and light roundtrip in pond substantially increases the absorption optical path length of measurement gas, from
And improve the precision of monitoring isotope abundance.
The temperature of leading in pond is measured by the exposed platinum resistance sensor of three imported with original packaging 1/3B levels more, and three
The inlet port of absorption cell outer wall, middle and outlet port are close in individual temperature sensor, and sensor is in the air temperature change
Response time within 2s, temperature is controlled by OMRON temperature controller, and control accuracy is closely wrapped up to ± 10mK, heating tape
Wrap many logical ponds and temperature sensor, heating tape external heat conductivity（0.018 W/mK of ＜）The nanoporous aerogel felt parcel of very little
Seal.
In many logical ponds, pressure carries out rear class control using MKS pressure controller, and its control accuracy is up to ± 5Pa.
The temperature control box is by heat conductivity（0.018 W/mK of ＜）The nanoporous aerogel felt parcel of very little is sealed, integument
The highlighted aluminium-foil paper of outermost layer self-adhesion is obturaged, to reduce gas with extraneous heat exchange and static interference as far as possible.
The Signal acquiring and processing module by equipped with preamplifier detector, capture card and be equipped with data processing journey
The computer composition of sequence.Signal that wherein detector is detected is amplified to be conveyed to the data in computer by capture card collection
Processing routine, data processor is write based on Labview software, can carry out frequency stabilization to laser instrument and isotope is rich
Degree collection.Isotope abundance acquisition interface is selected by parameter and spectrum shows that two parts are constituted.In parameter Selection Floater, each
The selection of parameter is all in the form of combobox, convenient to use.In spectrum display floater, data processing is programme can
Automatic peak-seeking, linear regression window width can be adjusted manually, it is achieved that measure in real timeδThe display of value and record, it is not necessary to after
Phase is processed to data.
Description of the drawings
Fig. 1 is the whole optical system diagram of the present invention
Leading to pond schematic diagram Fig. 2 more.
Specific embodiment
The present invention is a kind of off-axis stable isotope Measuring abundance of U-bar system of multi-wavelength, for while measuring four kinds of gas in air
Body stable isotope abundance, this not only reduces measuring instrument when measuring multiple gases stable isotope using balance detection method
Quality and volume and problem inconvenient to carry, and avoid that pressure when measuring using two ponds is different with temperature control to be caused
The not high problem of measurement result and precision.
Specific embodiment is as shown in figure 1, corrugated tube 13 and transparent Teflon pipe 36 are connected by adapter flange 12
Sealing, the adapter flange 10,11 for being provided with concave spherical mirror is connected sealing with corrugated tube 13 and transparent Teflon pipe 36 respectively.
Flange 34,35 equipped with calcium fluoride eyeglass is connected with the adapter flange 10,11 equipped with concave spherical mirror, fixing seal.Inlet port valve
Door 14 is separately mounted on the flange 35,34 equipped with calcium fluoride eyeglass with gas outlet valve 15.Multidimensional adjustment frame 9 is arranged on flange
On 34, the whole length for leading to pond and angle are adjusted more.In view of different wave length angle of incidence of the light in absorption cell not
Same, the flange 35 equipped with calcium fluoride eyeglass is first fixed on fixed mount 37, incidence end concave spherical surface is adjusted using multidimensional adjustment frame 9
Distance between the angle of mirror and two mirrors, after regulating a light path（Such as（1）→（2））, the fixing flange equipped with calcium fluoride eyeglass
35, it is adjusted using 1,3,5,7 pairs of remaining light paths of three-dimensional trim holder, light path mixes up rear adjustment frame 9 and is fixed on fixed mount 37
On.Many logical absorption cells are thus constituted.
Under test gas enter absorption cell from valve 14, flow out from valve 15.
The temperatures for leading to gas in absorption cell congratulate Li Shi by Germany more（Hreaeus）Imported with original packaging 1/3B level Pt100 platinum thermoelectricity
Resistance 39,40,41 is measured, and platinum resistance thermometer sensor, 39,40,41 is close to the outlet port for leading to absorption cell, centre position and air inlet successively
Mouth end.Lead to absorption cell and platinum resistance thermometer sensor, 39,40,41 by 38 tight of heating tape, heating tape external heat conductivity more（＜
0.018 W/mK）The nanoporous aerogel felt parcel of very little is sealed.Heating tape 38 and platinum resistance thermometer sensor, 39,40,41 and OMRON temperature controller
Connection, needs the parameter for setting OMRON temperature controller to be monitored the temperature for absorbing pool gas and control according to measurement.In pond
Pressure is controlled by MKS pressure controller 42, and pressure controller 42 is connected with valve 15, thus constitutes temperature and pressure control
System
Lead to absorption cell more and constitute absorption module with temperature and pressure control system.
In addition to temperature controller and pressure controller 42, the remainder of absorption module is placed in temperature control box 33, temperature control box
33 are shut by nanoporous aerogel felt parcel, and the highlighted aluminium-foil paper of the outermost layer self-adhesion of integument is obturaged, and lead to ponds to reduce as far as possible more
With extraneous heat exchange and static interference.
Laser controller 24,25,26,27 is by injection current wavelength respectively to laser instrument 16,17,18,19 and defeated
Go out power to be controlled.
Functional generator 28,29,30,31 are connected with laser controller 24,25,26,27, by setting sawtooth signal
Length scanning is carried out to laser instrument 16,17,18,19, makes two spectral lines of under test gas scanning will once be tuned in laser instrument
In the range of.
Laser instrument 16,17,18,19 is the narrow line width regulatable diode laser of different wave length.Laser instrument 16,17,18,
19 output laser after fiber optic splitter beam splitting high-power part by equipped with collimating lens three-dimensional trim holder 1,3,5,7
Be respectively coupled to lead in ponds, light in pond after multiple reflections through corresponding light hole be respectively radiated to detector 2,4,6,
On 8；Laser instrument 16,17,18,19 export laser after fiber optic splitter the little part of power be respectively coupled to band meter 20,
21st, on 22,23.The wavelength of 20,21,22,23 pairs of 16,17,18,19 output lights of laser instrument of band meter carries out real-time monitoring and feeds back
To computer 32, the frequency stabilization program in computer 32 is entered to lock frequency stabilization to the wavelength of laser instrument, makes laser wavelength stable in gas to be measured
Body molecular absorption line center.
It is input at the computer 32 equipped with capture card after the signal of absorption cell is by the reception of detector 2,4,6,8
Reason, computer 32 is built with capture card, data processor and frequency stabilization program.Wherein capture card, data processor distinguish logarithm
According to be acquired process.
Computer 32 makees subsequent treatment by self-editing Labview data processor to the data for collecting, it is achieved that swash
What the frequency stabilization of light device wavelength and absorption signal were gathered is synchronously carried out.Wherein band meter is carried by one tunnel of laser instrument frequency stabilization
Labview data read procedure is linked in the Labview data acquisition program that voluntarily writes, by band meter 20,21,22,
The signal of 23 feedbacks carries out Wavelength stabilized process to laser instrument 16,17,18,19, makes the Wavelength stabilized absorption in isotopic molecule
At peak.One tunnel of detector detection absorption signal, interface is selected by parameter and spectrum shows that two parts are constituted, parameter Selection Floater
In, the selection of each parameter is all in the form of combobox, convenient to use.In spectrum display floater, program is using choosing
The pattern of card, the parameter setting of different under test gas, noise is deducted, reference spectrum collection and linear regression etc. are respectively at not
Spectrum after denoising is not only shown by same interface, also the spectrum before and after denoising is carried out same frame and is shown, is conducive to denoising
Effect is assessed in real time, it is achieved that real-time, the continuous and synthetic operation of these modules, and the result of program real time execution is
Required isotope abundanceδValue, it is not necessary to which the later stage is processed to data.
Claims (4)
1. a kind of multicomponent gases stable isotope real time on-line monitoring optical system, including laser module, absorption cell module,
Temperature control box and Signal acquiring and processing module：It is characterized in that：The laser module is by four optical fiber output lasers, laser
Controller, functional generator and band meter composition；Also include fiber optic splitter, optical fiber couples flange, fiber optic collimator camera lens is housed
Three-dimensional trim holder；The laser instrument of four different wave lengths is tunable narrow-linewidth semiconductor laser, for exporting laser
Lead to ponds and band meter to off-axis, the wavelength of four laser instrument will be avoided the Absorption Line of selected under test gas each other, will also prevent more
The interference of other gases；The three-dimensional trim holder laser branch big to splitting ratio carries out optical path adjusting；The laser controller is used for
Noise spectra of semiconductor lasers enters trip temperature and current control；The functional generator enters line frequency using sawtooth signal to laser instrument
And voltage scanning, enable sweep interval to cover two adjacent absorbent spectral lines of under test gas stable isotope；The band meter
For the output wavelength of synchronous real-time monitoring laser instrument, and feed back to signal processing system in time laser wavelength is carried out in time
Correction；The splitting ratio of the fiber optic splitter is 99:1, the laser beam for laser instrument is exported is divided into two parts, and power is big
Branch be coupled in absorption cell through the three-dimensional trim holder that is fixed with collimation camera lens gas measured, the little branch of power
Being coupled to band meter carries out the wavelength of real-time monitoring laser instrument；The absorption cell module mainly has corrugated tube, transparent polytetrafluoroethyl-ne
Alkene pipe, concave spherical mirror, calcium fluoride eyeglass, adapter flange, sealing flange, multidimensional adjustment frame, air valve door, detector, fixation
Base and temperature and pressure control device composition；The corrugated tube, transparent Teflon pipe, concave spherical mirror, calcium fluoride eyeglass, switching method
Blue, sealing flange assembles off-axis many logical ponds；The off-axis ponds that lead to are used for accommodating under test gas more, while make to incide leading to more
Laser in pond roundtrip in the Duo Tongchi, to increase light path, improves the sensitivity to gas detecting；Many Tong Chi two ends
Connect air valve door respectively, for connecting outside gas circuit；The multidimensional adjustment frame is provided with the side of corrugated tube with Duo Tongchi
It is connected, for adjusting many logical length in pond and the angle of concave spherical mirror；The detector includes preamplifier, is mounted in Duo Tongchi
One end of transparent Teflon pipe is installed；The firm banking is used for being installed with the Duo Tongchi of detector；The temperature
Pressure control device is divided into temprature control unit and pressure controlling section, and temprature control unit includes that three imported with original packaging 1/3B levels are naked
Dew platinum resistance sensor, heat tape and nanoporous aerogel felt and OMRON temperature controller, absorption is close in temperature sensor
The inlet port of pond outer wall, middle and outlet port, heating tape tight lives many logical ponds and temperature sensor, heating tape external
Heat conductivity（0.018 W/mK of ＜）The nanoporous aerogel felt parcel of very little is sealed, temperature sensor and heating tape and OMRON temperature
Control device connection is monitored to the temperature for absorbing pool gas and controls, and sensor exists to the response time of in the air temperature change
Within 2s, control accuracy is up to ± 10mK；The pressure controlling section carries out rear class control using MKS pressure controller, its control
Precision processed is up to ± 5Pa；The temperature control box is used for placing except OMRON temperature controller and MKS pressure controller in absorption cell module
Remainder, then shut by nanoporous aerogel felt parcel, the highlighted aluminium-foil paper of the outermost layer self-adhesion of integument is obturaged, with to the greatest extent
Amount reduces the ponds that lead to extraneous heat exchange and static interference more；The OMRON temperature controller is by wire with temperature sensor even
Connect, MKS pressure controller is connected with pool gas by pipeline, be so able to ensure that many logical pool gas temperature and pressure can
Realize temperature control box outer real-time monitoring, control；The signals collecting by capture card and is equipped with data processing journey with data processing module
The computer composition of sequence, mainly includes following two aspects content：（1）The laser beam for accessing band meter is swashed for synchro measure laser
The wavelength of light device, judges whether the output wavelength of laser instrument absorbs line position in gas isotope, according to judged result by number
The wavelength of letter lock frequency technology-locking laser instrument output so as to stable in the center of isotope absorption line；（2）Capture card is gathered
To the absorption spectrum signal of gas stable isotope be transported to computer, by the parameter setting in data processing software, make an uproar
Sound is deducted, reference spectrum is gathered and the orderly process of linear regression, last directly reading object gas stable isotope Abundances.
2. a kind of off-axis stable isotope abundance on-line monitoring system of multi-wavelength is required according to right 1, it is characterised in that off-axis many
Logical pond by corrugated tube, transparent Teflon pipe, two pieces have the concave spherical mirror of four light holes, three adapter flanges, two
Sealing flange, six pieces of calcium fluoride eyeglasses and a multidimensional adjustment frame composition；Wherein, one end of the corrugated tube and transparent polytetrafluoro
One end of ethylene tube is connected and fixed by adapter flange；The concave spherical mirror with four light holes is fixed on switching
On flange, it is connected with the other end of corrugated tube and transparent Teflon pipe respectively；The calcium fluoride eyeglass is fixed on Sealing Method
Lan Shangyu fixes the adapter flange connection sealing of the concave spherical mirror with four light holes, and the side in corrugated tube is incidence
End, the other end of transparent Teflon pipe is exit end；The incidence end is fixed in multidimensional adjustment frame, for adjusting recessed ball
The angle of face mirror and the off-axis length for leading to pond, enable outgoing light to be accurately irradiated on detector more, while elimination leads to pond
The impact to measured signal of interior issuable interference fringe.
3. a kind of off-axis stable isotope abundance on-line monitoring system of multi-wavelength is required according to right 1, it is characterised in that laser instrument
Band meter the Labview data read procedure for carrying and the Labview data acquisition program that voluntarily writes are carried out by frequency stabilization part
Link, the photosignal for being fed back by band meter makes laser wavelength steady while carry out Wavelength stabilized process to four laser instrument
Under test gas molecular absorption line center is scheduled on, can be worked long hours and wavelength does not drift about, and precision reaches 0.001cm-1.
4. a kind of off-axis stable isotope abundance on-line monitoring system of multi-wavelength is required according to right 1, it is characterised in that using volume
Journey software is used for realizing to laser instrument frequency stabilization and the data processing of multiple gases stable isotope while carry out, convenient to use；
Each parameter of wherein under test gas is selected all in the form of combobox, data processing programme can automatic peak-seeking,
Linear regression window width can be adjusted manually, and multiple same position Abundances can show and record in real time, it is not necessary at later data
Reason.
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