CN106442404B - A kind of multicomponent gas stable isotope real time on-line monitoring optical system - Google Patents
A kind of multicomponent gas stable isotope real time on-line monitoring optical system Download PDFInfo
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- 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 kind of multicomponent gas stable isotope real time on-line monitoring optical systems, including laser module, absorption cell module, temperature control box and data processing module.Present invention combination length scanning, multi-pass pond adjust, in pond pressure, temperature and wavelength accurate control, real time on-line monitoring can be carried out to four kinds of trace gas concentrations and isotope simultaneously using single multi-pass, measurement process does not need sample preparation.The quantity for reducing instrument when measuring using pure gas isotope when balance detection using double ponds, overcomes the limitation that a kind of gas isotope can only be measured using single multi-pass pond.Entire optical system volume compact, it is easy to operate, without calibration, it can be realized and real time on-line monitoring simultaneously is carried out to the stable isotope abundance and concentration of four kinds of Pollution Gas.The system integration degree is high, and the real time on-line monitoring of polluted gas source remittance can be carried out under hazardous environment.
Description
Technical field
The present invention relates to atmospheric stability isotope abundance field of optical detection more particularly to a kind of multicomponent gas to stablize together
The plain real time on-line monitoring optical system in position.
Background technique
Stable isotope detection technology is in the microenvironment mechanism for disclosing generation, transmission and the release of Pollution Gas and really
Determine that there is apparent superiority in terms of relative contribution rate.Atmospheric molecule Isotope Compositions can reflect that atmospheric molecule forms source
The original state and Variation Features in area, the variation of the weather system of large scale.The application of stable isotope is dirty to climate change, environment
The improvement for contaminating object has impetus and practical advice meaning, can more preferably understand regional climate characteristics and law study.It is high-precision
The atmospheric stability isotope measure method of degree has accurate parsing source remittance Variation Features and variation tendency, reduction measurement error non-
Often important meaning, plays increasingly important role in atmospheric environment field of scientific study.
The standard technique for determining isotope abundance is isotopic ratio mass spectrum (IRMS) technology.The technology measurement accuracy is high,
But service requirement is also higher, is difficult to carry out live real-time measurement.Especially to the measurement of steam isotope, it usually needs tens
Steam is acquired from atmosphere in minute to several hours, and then steam is handled and analyzed, IRMS technology can not be distinguished
Isomer molecule isotope, these features limit IRMS technology to the on-line analysis ability of sample.
The spectral technique developed in recent years overcomes the limitation of traditional IRMS technology.Laser absorption spectroscopy is used for atmosphere
Molecule Stable isotope detection is developing progressively an advanced subject of spectrum of use and isotope analysis research field.Mainly
There are 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 usually analyzes rotation-vibration jump of isotope
The one or more short-wave bands to be formed are moved, measurement accuracy is higher.However, usually structure is complicated by QCLAS, CRDS and FTIR, at
This valuableness can only measure a kind of gas isotope abundance, the unsuitable highly sensitive isotope detection for developing into real-time monitoring
Instrument.TDLAS technology is obtained and is tested within the scope of the characteristic absorption spectrum of gas using diode laser length scanning characteristic
Absorption spectrum, to carry out a kind of qualitative or quantitative analysis technology to polluted gas isotope.The technology has sensitive
Spend high, selectivity is good, without sampling and sample treatment, can in real time, dynamic, quickly, multicomponent while the advantages that measure, can develop
At 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 gas
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 gas isotope.It is steady that multi-wavelength multicomponent is carried out using TDLAS
Determine isotopic abundance measurement system and realizes that simply, fiber coupling mode makes system be easily adapted to measurement environment and miniaturization.Swashing
In light device wavelength scanning range, in the case where selecting the Absorption Line that two are not interfered by other gas componants and its variation, only want
It asks measurement gas pressure intensity not so high and is not reacted with other gases, it will be able to realize that the real-time online of non-intruding is stablized
Isotope monitoring.In addition, multi-wavelength multicomponent stable isotope abundance measurement device is easily integrated, programming manipulation, without fixed
Mark, is able to maintain prolonged stability, easy to carry, is able to carry out field trial, and to Pollution Gas source, remittance changes and I
The research of state's environmental pattern has great importance.
Summary of the invention
The purpose of the invention is to provide a kind of multicomponent gas stable isotope abundance measurement system, system structure letter
It is single, there is preferable pressure and temperature stability, the measurement of four kinds of gas stable isotope abundance can be carried out simultaneously, solve and work as
The shortcomings that preceding instrument can only be to pure gas isotopic abundance measurement can be carried out long-term real-time online observation, relative to single gas
Body isotope measure device, present invention reduces the period of analysis isotope abundance, can system comprehensively to study atmosphere main
The source of polluted gas and the dynamic change of remittance grasp its concentration spatial-temporal characteristics.
The present invention uses tunable diode absorption spectroscopy techniques, according to Lambert-Beer's law selectively to big temperature
Room gas stable isotope abundance measures.
Technical solution of the invention: a kind of off-axis stable isotope Measuring abundance of U-bar system of multi-wavelength, including laser
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, function generator and wavemeter composition；
It further include the fiber optic splitter that the splitting ratio that is connected with laser is 99:1, fiber coupling flange, equipped with fiber optic collimator camera lens
Three-dimensional trim holder；Laser fiber output end is connected by optic fibre switching flange with fiber optic splitter；Fiber optic splitter splitting ratio
Big one is connected on the three-dimensional trim holder equipped with fiber optic collimator camera lens, and small one of splitting ratio connect with wavemeter.
The absorption cell module mainly has bellows, transparent Teflon pipe, concave spherical mirror, calcirm-fluoride eyeglass, switching
Flange, sealing flange, multidimensional adjustment frame, air valve door, detector, firm banking and temperature control device composition；
One end of the bellows and one end of transparent Teflon pipe are linked together by adapter flange, bellows
With the other end of transparent Teflon pipe respectively be fixed with incident concave spherical mirror and be emitted the adapter flange phase of concave spherical mirror
Even, sealing flange and calcirm-fluoride eyeglass, which are fixed together, is mounted on outside the adapter flange equipped with concave spherical mirror, thus constitutes
Multi-pass absorption cell；The side that the multi-pass pond is equipped with bellows is the incidence end of light；The multidimensional adjustment frame and incidence end are close
Envelope flange is fixedly connected on pedestal；One end that the multi-pass pond is equipped with transparent Teflon pipe is the exit end of light；Institute
State the exit end that detector is mounted on multi-pass pond；The air intake valve and outlet valve are separately mounted to multi-pass pond incidence end and go out
It penetrates on the sealing flange at end；The air inlet valve and gas outlet valve respectively with outside air circuit connection.
The concave spherical mirror in the multi-pass pond is coated with golden film, and the bandwidth of reflected light is 800 nm~20 μm, average reflectance
It is 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.
Temperature is measured by 1/3B grades of exposed platinum resistance sensors of three imported with original packaging in the multi-pass pond, and three
A temperature sensor is tightly attached to inlet port, centre and the outlet port of absorption cell outer wall, and sensor is to temperature change in air
Response time within 2s, temperature is controlled by OMRON temperature controller, control the reachable ± 10mK of precision, heating tape is closely wrapped
Wrap multi-pass pond and temperature sensor, the nanoporous aerogel felt package of heating tape external application thermal coefficient (0.018 W/mK of <) very little
It seals.
Pressure carries out rear class control using MKS pressure controller in the multi-pass pond, controls the reachable ± 5Pa of precision.
The temperature control box is sealed by the nanoporous aerogel felt package of thermal coefficient (0.018 W/mK of <) very little, wrapping layer
Outermost layer highlights aluminium-foil paper with self-adhesion and obturages, to reduce gas and extraneous heat exchange and electrostatic interference to the greatest extent.
The Signal acquiring and processing module is by the detector equipped with preamplifier, capture card and equipped with data processing journey
The computer of sequence forms.The signal that wherein detector detects is amplified to acquire the data being conveyed in computer by capture card
Processing routine, data processor are write based on Labview software, can carry out frequency stabilization to laser and isotope is rich
Degree acquisition.Isotope abundance acquisition interface shows that two parts are constituted by parameter selection and spectrum.In parameter selection panel, each
The selection of parameter is all made of the form of combobox, convenient to use.In spectrum display panel, data processing is programme can
Automatic peak-seeking, linear regression window width can manually adjust, and realize real-time measurementδThe display of value and record, after not needing
Phase handles data.
Detailed description of the invention
Fig. 1 is entire optical system diagram of the invention
Fig. 2 multi-pass pond schematic diagram.
Specific embodiment
The present invention is a kind of off-axis stable isotope Measuring abundance of U-bar system of multi-wavelength, for measuring four kinds of gas in atmosphere simultaneously
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 pressure and temperature when measuring using two ponds and control caused by difference
Measurement result and the not high problem of precision.
Specific embodiment is as shown in Figure 1, bellows 13 and transparent Teflon pipe 36 are connected by adapter flange 12
Sealing, the adapter flange 10,11 for being equipped with concave spherical mirror connect sealing with bellows 13 and transparent Teflon pipe 36 respectively.
Flange 34,35 equipped with calcirm-fluoride eyeglass connect 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 calcirm-fluoride eyeglass with gas outlet valve 15.Multidimensional adjustment frame 9 is mounted on flange
The length and angle in entire multi-pass pond are adjusted on 34.In view of different wave length incidence angle of the light in absorption cell not
Together, the flange 35 equipped with calcirm-fluoride eyeglass is first fixed on fixed frame 37, adjusts incidence end concave spherical surface using multidimensional adjustment frame 9
Distance between the angle of mirror and two mirrors regulates after an optical path (such as (1) → (2)), the fixed flange that calcirm-fluoride eyeglass is housed
35, it is adjusted using 1,3,5,7 pair of remaining optical path of three-dimensional trim holder, optical path mixes up rear adjustment frame 9 and is fixed on fixed frame 37
On.Thus constitute multi-pass absorption cell.
Under test gas enters absorption cell from valve 14, flows out from valve 15.
The temperature of gas congratulates 1/3B grades of Pt100 platinum thermoelectricity of Li Shi (Hreaeus) imported with original packaging by Germany in multi-pass absorption cell
39,40,41 measurement of resistance, platinum resistance thermometer sensor, 39,40,41 are successively tightly attached to outlet port, middle position and the air inlet of multi-pass absorption cell
Mouth end.Multi-pass absorption cell and platinum resistance thermometer sensor, 39,40,41 are by 38 tight of heating tape, heating tape external application thermal coefficient (<
0.018 W/mK) very little nanoporous aerogel felt package seal.Heating tape 38 and platinum resistance thermometer sensor, 39,40,41 and OMRON temperature controller
Connection is monitored and controls to the temperature for absorbing pool gas according to the parameter that measurement needs to set OMRON temperature controller.In pond
Pressure is controlled by MKS pressure controller 42, and pressure controller 42 is connect with valve 15, thus constitutes temperature and pressure control
System
Multi-pass absorption cell and temperature and pressure control system form absorption module.
Other than 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 package, and the outermost layer of wrapping layer highlights aluminium-foil paper with self-adhesion and obturages, to reduce multi-pass pond to the greatest extent
With extraneous heat exchange and electrostatic interference.
Laser controller 24,25,26,27 passes through the Injection Current wavelength to laser 16,17,18,19 and defeated respectively
Power is controlled out.
Function generator 28,29,30,31 is connected with laser controller 24,25,26,27, by setting sawtooth signal
Length scanning is carried out to laser 16,17,18,19, two spectral lines of under test gas is made once to tune scanning in laser
In range.
Laser 16,17,18,19 is the narrow line width regulatable diode laser of different wave length.Laser 16,17,18,
The laser of 19 outputs high-power part after fiber optic splitter beam splitting passes through the three-dimensional trim holder 1,3,5,7 equipped with collimation lens
Be respectively coupled in multi-pass pond, light in pond after multiple reflections through corresponding light hole be respectively radiated to detector 2,4,6,
On 8；Laser 16,17,18,19 export laser after fiber optic splitter the small part of power be respectively coupled to wavemeter 20,
21, on 22,23.The wavelength of 20,21,22,23 pairs of 16,17,18,19 output lights of laser of wavemeter carries out real-time monitoring and feeds back
To computer 32, the frequency stabilization program in computer 32 into locking frequency stabilization, stablizes laser wavelength in gas to be measured the wavelength of laser
Body molecular absorption line center.
It is input at the computer 32 equipped with capture card after the signal of absorption cell is received by detector 2,4,6,8
Reason, computer 32 are provided with capture card, data processor and frequency stabilization program.Wherein capture card, data processor distinguish logarithm
It is handled according to being acquired.
Computer 32 makees subsequent processing to collected data by self-editing Labview data processor, realizes sharp
The synchronous progress that the frequency stabilization of light device wavelength is acquired with absorption signal.Wherein laser frequency stabilization all the way carries wavemeter
Labview data read procedure is linked into the Labview data acquisition program voluntarily write, by wavemeter 20,21,22,
The signal of 23 feedbacks carries out Wavelength stabilized processing to laser 16,17,18,19, makes the Wavelength stabilized absorption in isotopic molecule
At peak.Detector detects absorption signal all the way, and interface shows that two parts are constituted by parameter selection and spectrum, parameter selection panel
In, the selection of each parameter is all made of the form of combobox, convenient to use.In spectrum display panel, program is using choosing
The parameter setting of different under test gas, noise deduction, reference spectrum acquisition and linear regression etc. are respectively at not by the mode of item card
Same interface not only shows the spectrum after denoising, also show with frame by the spectrum of denoising front and back, be conducive to denoising
Effect is assessed in real time, and real-time, continuous and synthetic operation, the result of program real time execution for realizing these modules are
Required isotope abundanceδValue, not needing the later period handles data.
Claims (4)
1. a kind of multicomponent gas 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 by: the laser module is by four optical fiber output lasers, laser
Controller, function generator and wavemeter composition；It further include fiber optic splitter, fiber coupling flange is equipped with fiber optic collimator camera lens
Three-dimensional trim holder；The laser of four different wave lengths is tunable narrow-linewidth semiconductor laser, for exporting laser
To off-axis multi-pass pond and wavemeter, the wavelength of four lasers will avoid the Absorption Line of selected under test gas each other, also prevent
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 carries out temperature and current control；The function generator carries out frequency to laser using sawtooth signal
And voltage scanning, so that sweep interval is covered two adjacent absorbent spectral lines of under test gas stable isotope；The wavemeter
For synchronizing the output wavelength of real-time monitoring laser, and timely feedbacks and laser wavelength is carried out in time to signal processing system
Correction；The splitting ratio of the fiber optic splitter is 99:1, and the laser beam for laser to be exported is divided into two parts, and power is big
Branch be coupled in absorption cell by being fixed with the three-dimensional trim holder of collimation camera lens gas measured, the small branch of power
It is coupled to the wavelength that wavemeter carries out real-time monitoring laser；The absorption cell module mainly has bellows, transparent polytetrafluoroethyl-ne
Alkene pipe, concave spherical mirror, calcirm-fluoride eyeglass, adapter flange, sealing flange, multidimensional adjustment frame, air valve door, detector, fixation
Pedestal and temperature and pressure control device composition；The bellows, transparent Teflon pipe, concave spherical mirror, calcirm-fluoride eyeglass, switching method
Blue, sealing flange assembles off-axis multi-pass pond；The off-axis multi-pass pond makes to be incident on multi-pass for accommodating under test gas
Laser in the pond roundtrip in multi-pass pond improves the sensitivity to gas detection to increase light path；Multi-pass pond both ends
It is separately connected air valve door, for connecting outside gas circuit；The multidimensional adjustment frame and multi-pass pond are equipped with the side of bellows
It is connected, for adjusting the length in multi-pass pond and the angle of concave spherical mirror；The detector includes preamplifier, is mounted in multi-pass pond
One end of transparent Teflon pipe is installed；The firm banking is used to be fixedly installed with the multi-pass pond of detector；The temperature
Pressure control device is divided into temprature control unit and pressure controlling section, and temprature control unit includes three 1/3B grades of imported with original packaging naked
Dew platinum resistance sensor, heat tape and nanoporous aerogel felt and OMRON temperature controller, temperature sensor are tightly attached to absorption
Inlet port, centre and the outlet port of pond outer wall, heating tape tight live multi-pass pond and temperature sensor, heating tape external application
Nanoporous aerogel felt package of the thermal coefficient less than 0.018W/mK seals, and temperature sensor and heating tape and OMRON temperature controller connect
Connect and the temperature for absorbing pool gas be monitored and controlled, sensor to response time of temperature change in air 2s with
It is interior, control the reachable ± 10mK of precision；The pressure controlling section carries out rear class control, control essence using MKS pressure controller
Spend reachable ± 5Pa；The temperature control box is used to place in absorption cell module surplus in addition to OMRON temperature controller and MKS pressure controller
Then remaining part point is shut by nanoporous aerogel felt package, the outermost layer of wrapping layer highlights aluminium-foil paper with self-adhesion and obturages, to subtract as far as possible
Few multi-pass pond and extraneous heat exchange and electrostatic interference；The OMRON temperature controller is connect by conducting wire with temperature sensor, MKS
Pressure controller is connect by pipeline with pool gas, can ensure that multi-pass pool gas temperature and pressure can be realized temperature in this way
Control the outer real-time monitoring of case, control；The signal acquisition and data processing module are by capture card and equipped with the meter of data processor
Calculation machine composition, mainly includes following two aspects content: (1) accessing the laser beam of wavemeter for synchro measure laser
Wavelength judges that the output wavelength of laser whether in gas isotope absorption line position, passes through digital frequency locked according to judging result
The wavelength of technology-locking laser output, stablizes it in the center of isotope absorption line；(2) the collected gas of capture card
The absorption spectrum signal of body stable isotope is transported to computer, deducted by the parameter setting in data processing software, noise,
The orderly processing of reference spectrum acquisition and linear regression, finally directly reads object gas stable isotope Abundances.
2. requiring a kind of multicomponent gas stable isotope real time on-line monitoring optical system, feature according to right 1
It is that there is bellows in off-axis multi-pass pond, there are four the concave spherical mirrors of light hole, three switchings for transparent Teflon pipe, two pieces of tools
Flange, two sealing flanges, six pieces of calcirm-fluoride eyeglasses and a multidimensional adjustment frame composition；Wherein, one end of the bellows and
One end of transparent Teflon pipe is connected and fixed by adapter flange；There are four the concave spherical mirrors of light hole for the tool
It is fixed on adapter flange, is connect respectively with the other end of bellows and transparent Teflon pipe；The calcirm-fluoride eyeglass is solid
It is scheduled on sealing flange and connect sealing with the fixed adapter flange for having the concave spherical mirror there are four light hole, one in bellows
Side is incidence end, and the other end of transparent Teflon pipe is exit end；The incidence end is fixed on multidimensional adjustment frame, is used for
The angle of concave spherical mirror and the length in off-axis multi-pass pond are adjusted, so that outgoing light is accurately irradiated on detector, disappears simultaneously
Except the influence of issuable interference fringe to measured signal in multi-pass pond.
3. requiring a kind of multicomponent gas stable isotope real time on-line monitoring optical system, feature according to right 1
It is that laser frequency stabilization part adopts the Labview data read procedure that wavemeter carries with the Labview data voluntarily write
Collection program is linked, and the photosignal fed back by wavemeter carries out Wavelength stabilized processing to four lasers simultaneously, makes to swash
Light device is Wavelength stabilized under test gas molecular absorption line center, can work long hours and wavelength does not drift about, and precision reaches
0.001cm-1。
4. requiring a kind of multicomponent gas stable isotope real time on-line monitoring optical system, feature according to right 1
It is to be used to realize to laser frequency stabilization and the data processing of multiple gases stable isotope while carrying out using programming software, uses
It is convenient and efficient；Wherein each parameter selection of under test gas is all made of the form of combobox, and data processing is programme can
Automatic peak-seeking, linear regression window width can manually adjust, and a variety of isotope abundance values can display real-time and record, and not need
Later data processing.
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