A kind of temperature precise control device for the spectral technique isotope analysis of integration chamber
Technical field
The present invention relates to a kind of temperature precise control device, is the device that a kind of temperature being applied to integration chamber spectral technique gas isotope analysis field accurately controls in particular.
Background technology
Stable Isotopic Analysis comes into one's own day by day in the application of environmental science and field of Environment Protection in recent years, especially in the research of air, soil, water quality and ecologic environment, has all played vital role.As applied stable isotope Plantago fengdouensis, research and indicative for environments pollution source and pollution level; Utilize the Detectable effects of stable isotope, the discharge source of greenhouse gases can be distinguished, analyze mankind's activity if combustion of fossil fuel, manufacture of cement, cultivation herding and agricultural production are to the contribution of greenhouse gas emission, not only accurately can estimate that the total emission volumn of each emission source is implemented " energy-saving and emission-reduction " work also have certain directive significance to factory, city; Contribute to understanding the physical and chemical changes mechanism of converging in methane source in air by measuring methane isotope, for the quantitative examination of the discharge of methane such as rice field, wetland mechanism and oxygenation efficiency.In addition Stable Isotopic Analysis is also widely used at multiple subjects such as geology, nuclear industry, archaeology, ecologic environment scientific research, biology and chemical research, water resources development, agricultural production, food security, clinical medicine.
Integration chamber spectral technique is the time integral light intensity by measuring through optical cavity, and with the difference of incident intensity, calculate gas concentration to be measured, this method, closer to traditional direct absorption spectrum, more meets Beer-Lambert law.This technology has high survey frequency, spectral resolution and measurement sensistivity, simple and the result of measuring equipment structure is demarcated without the need to complexity, and can Miniaturized portable be made, auxiliary other physical means same laser isotope analyser can realize analyzing gas-liquid-solid three-state sample, and the isotope analysis instrument of therefore comparing based on mass-spectrometric technique has many advantages.
In the spectral technique isotope measure analytic process of integration chamber, in order to make instrument system itself play maximum performance except selecting independently except LASER Light Source, single a, stationary temperature and minimum ambient vibration is kept also to be absolutely necessary.Temperature adjusting speed is all electricity systems, LASER Light Source, instrument size, and the velocity of sound etc. are in interior major influence factors.These parameters can have 10 along with the change of every Kelvin under normal circumstances
-4~ 10
-5variable quantity.If measurement target is solid or liquid, the change of temperature will cause the greatly inaccurate of drift that system is larger even measurement result.When adopting integration chamber spectroscopy measurement gas isotope to analyze, as: C
14o
2, C
13o
2, C
12o
2, the change of temperature will affect different isotopic Boltzman distribution situation, and even the inaccurate of the isotopic ratio of known fixed component situation is measured in aggravation.And, the measurement of the real concentration of gas isotope and the stability of ultraprecise light path depend on temperature stability to a great extent, otherwise measurement result accurately cannot be obtained, and accurately, quick and stable temperature accurately controls, one of important indicator also making instrument zero shift minimum exactly.Therefore accurate temperature control equipment is for the suitable environment expanding integration chamber spectral technique isotope analysis instrument, and the actual effect that raising detects and accuracy all tool are of great significance.
Summary of the invention
Technology of the present invention is dealt with problems: overcome the deficiencies in the prior art, there is provided a kind of temperature precise control device for the spectral technique isotope analysis of integration chamber, to solve the accuracy of existing integration chamber spectral technique isotope analysis temperature influence in measuring process, stability and zero shift problem.
Technical scheme of the present invention is as follows: a kind of temperature precise control device for the spectral technique isotope analysis of integration chamber, is characterized in that comprising: optical path system 1, once sealing housing 2, four platinum resistance temperature sensors 3, secondary seal housing 5, two thermal controls apparatus, nitrogen 9 atmosphere, temperature controller 10, drive circuit module 11, rigid support 13 and shock absorbing foam 14, described two thermal controls apparatus are installed on the housing two ends of secondary seal housing 5 symmetry respectively, each thermal controls apparatus piles 6 by semiconductor refrigerating, weblike heat interchanger 7 and fan 8 form, 1/3 part of weblike heat interchanger 7 is installed on the inside of semiconductor refrigerating heap 6 and piles 6 closed seamless with semiconductor refrigerating and be connected, the exchange heat between weblike heat interchanger 7 and semiconductor refrigerating heap 6 is made to reach the most sufficient situation, fan 8 is installed on the same side of weblike heat interchanger 7, installation site should be consistent with left or same right, heat interchange air-flow under fan 8 is acted on forms clockwise or counterclockwise laminar flow 4 direction, it is inner that optical path system 1 is installed on once sealing housing 2, and once sealing housing 2 carries out heat isolation and vibration damping by shock absorbing foam 14, and then it is inner to be fixed on secondary seal housing 5 by rigid support 13, described once sealing housing 2 inside and secondary seal housing 5 inside all need to be full of nitrogen 9 atmosphere, two platinum resistance temperature sensors in four platinum resistance temperature sensors 3 are installed respectively and are embedded in diagonal angle two end housing of once sealing housing 2, and two other platinum resistance temperature sensor is arranged on weblike heat interchanger 7 one end away from fan 8 respectively, all platinum resistance temperature sensors 3 are all connected with the temperature controller 10 being installed on secondary seal housing 5 outside, and Real-time Obtaining once sealing housing 2 is inner and the temperature conditions of secondary seal housing 5 inside, temperature controller 10 is according to the feedback information of different platinum resistance temperature sensors 3, control to export by PID the drive circuit module 11 controlling to be installed on secondary seal housing 5 outside to carry out temperature and accurately control work, when the PID of temperature controller 3 controls to send temperature control command, drive circuit module 11 starts normal work, semiconductor refrigerating heap 6 is driven to carry out heating or refrigeration control, and start the circulation of fan 8 accelerated heat, shorten temperature controlled time and the efficiency that improve heat interchange greatly, thus ensure the stability of temperature, and drive circuit module 11 controls until reach assigned temperature according to the temperature controller 10 instruction real-time circulation received in real time in operational process, simultaneously treatment temperature situation of change in real time in the course of the work, carries out cycle control until reach assigned temperature.
Described optical path system 1 comprises Distributed Feedback Laser 301, beams converge collimation lens set 302, collimated light beam 303, optics cavity 304, laser beam plus lens 306, InGaAs detector 307.The laser driving source 308 that Distributed Feedback Laser 301 is subject to being installed on once sealing housing 2 and secondary seal housing 5 outside drives generation modulated laser, laser beam forms (spot diameter≤1mm) collimated light beam 303 through beams converge collimation lens set 302, after the gas to be measured 305 of collimated light beam 303 through optics cavity 304 inside absorbs, converge on the photosurface of InGaAs detector 307 through laser beam plus lens 306, it converges spot size≤1mm
2.Then the signal after photoelectricity turns sends into by cable 12 inverting that the signal subsequent processing units 309 being installed on once sealing housing 2 and secondary seal housing 5 outside carries out follow-up signal transacting and gas isotopic abundance, and this all parts of system is all in nitrogen 9 atmosphere.
Described laser driving source 308 is installed on once sealing housing 2 and secondary seal housing 5 is outside, comprising: the signal generator unit of the temperature controller that laser instrument drives, current controller and generation triangular voltage sweep signal, sinewave modulation signal; Temperature controller, current controller drive Distributed Feedback Laser (301) normally to work, and signal generator unit makes Distributed Feedback Laser 301 produce modulated laser.
Described Distributed Feedback Laser 301 is semiconductor laser with tunable.
Described subsequent processing units 309 is installed on once sealing housing 2 and secondary seal housing 5 is outside, comprising: optical signal amplification circuit, lock-in amplifier, data collecting card and computing machine; The output signal of InGaAs detector 308 sends into optical signal amplification circuit, signal feeding lock-in amplifier after amplifying circuit amplifies carries out demodulation and obtains corresponding harmonic signal, and harmonic signal is undertaken gathering the inverting then carrying out follow-up signal transacting and gas isotopic abundance by the data collecting card being installed on computer-internal.
Described optics cavity 304 is from axle integration chamber, and cavity side connects air inlet/outlet, makes laser beam 303 multiple reflections back and forth incided in chamber simultaneously, greatly increases the absorption optical path length of measurement gas, thus improves the sensitivity detecting gas.
Described PID controls to be adopted as Fuzzy Adaptive PID Control algorithm, action has temperature setting, data acquisition, PID to control to export, by comparing the difference between real time temperature, design temperature, exported by PID and control semiconductor refrigerating heap 6 refrigeration or heat, make optical path system 1 keep stable in a certain temperature.
The all power supplies of described system all adopt DC-24V to power.
The present invention's advantage is compared with prior art:
(1) it is have high sensitivity, high precision that existing integration chamber spectroscopic isotope analytical technology measures general requirement, and device itself should firm, portable, applied range.Such as, when instrument is exposed to the change of some ambient temperature frequently, exist in the environment of vibrations, the temperature precise control device analyzed of integration chamber spectroscopic isotope just must not the interference of heated environment and vibration environment, keep stability and the accuracy of height, and the invention solves the temperature stability issues of existing integration chamber spectral technique isotope analysis in measuring process, improve the accuracy of measurement, stability, and extraneous factor impact can be reduced, improve the advantage of system zero drift.
(2) the optical path system sealing be made up of laser instrument, eyeglass, optics cavity and InGaAs detector is carried out once sealing by the present invention together, then put into secondary seal housing again to seal, temperature is carried out to whole secondary seal housing and accurately controls.The object that temperature accurately controls not is control temperature in a certain temperature accurately, but pursues system light path in the stability of a certain temperature, at least can reach ± 0.01K, preferably can reach ± stable the amplitude of 0.001K.
(3) each several part of the present invention integration packaging respectively, adopts multiple temperature measurement and control system, adopts closed-loop control pid algorithm to reach real-time temperature detection and real-time precise and stable control.
(4) the present invention adopts the parts such as semiconductor refrigerating heap, weblike heat interchanger, fan to shorten the temperature controlled time greatly and improve the efficiency of heat interchange, and the temperature achieved in very short time accurately controls with long temperature precise and stable.
(5) the present invention's fan, rigid support and anti-seismic material of adopting vibrations less, while guarantee temperature control precision and degree of stability, ensure that shock resistance and the structural stability of system.
(6) once sealing housing of the present invention and secondary seal housing are strict air-proof condition, and its inside is filled with nitrogen atmosphere, in isotope measure process, therefore eliminate the impact of other interference gas.
Accompanying drawing explanation
Fig. 1 is the plan view from above of bulk temperature accuracy-control system of the present invention;
Fig. 2 is the side plan view of bulk temperature accuracy-control system of the present invention;
Fig. 3 is the optical path system diagram of once sealing housing of the present invention.
Embodiment
As shown in Figure 1, Figure 2, Figure 3 shows, apparatus of the present invention comprise two parts: one is optical path system 1; Two secondary sealing systems being used to precise control of temperature; The secondary sealing system of precise control of temperature comprises: optical path system 1 carries out first time sealing by once sealing housing 2, platinum resistance temperature sensor 3, gas laminar flow 4, secondary seal housing 5, semiconductor refrigerating heap 6, weblike heat interchanger 7, fan 8, nitrogen 9 atmosphere, temperature controller 10, drive circuit module 11, cable 12, rigid support 13, shock absorbing foam 14.
Optical path system 1 as shown in Figure 3, mainly comprise: the Distributed Feedback Laser 301 being installed on once sealing housing 2 and secondary seal housing 5 outside, beams converge collimation lens set 302, collimated light beam 303, optics cavity 304, the gas to be measured 305 of optics cavity 304 inside, laser beam plus lens 306, InGaAs detector 307.The laser driving source 308 that Distributed Feedback Laser 302 is subject to being installed on once sealing housing 2 and secondary seal housing 5 outside drives generation modulated laser, laser beam after modulation forms (spot diameter≤1mm) collimated light beam 303 through beams converge collimation lens set 302, after the gas to be measured 305 of collimated light beam 303 through optics cavity 304 inside absorbs, converge on the photosurface of InGaAs detector 307 through laser beam plus lens 306, it converges spot size≤1mm
2then the signal after photoelectricity turns sends into by cable 12 inverting that the signal subsequent processing units 309 being installed on once sealing housing 2 and secondary seal housing 5 outside carries out follow-up signal transacting and gas isotopic abundance, and this all parts of system is all in the nitrogen atmosphere 9 of once sealing housing 2 inside.
Detailed process of the invention process is: first, and optical path system 1 carries out first time sealing by being installed on once sealing housing 2 inside, and once sealing housing 2 uses coefficient of heat conductivity metal material that is comparatively large, that be convenient to process to be material.Then, the inside that optical path system 1 and once sealing housing 2 are sealed in secondary seal housing 5 is jointly sealed again, the object of such design is the complete heat isolation in order to ensure external environment, and the material of secondary seal housing 5 can use the rigid plastic with better heat-proof quality to be material.Once sealing housing 2 carries out heat isolation and vibration damping by shock absorbing foam 14, such as: isocyanurate foam, ethylenic copolymer foam etc. carry out heat isolation and vibration damping, and then the inside of secondary seal housing 5 is fixed on by rigid support 13, between rigid support 13 and secondary seal housing 5, the same shock absorbing foam 14 that adopts carries out vibration damping again.All platinum resistance temperature sensors 3 are all connected with the temperature controller 10 being installed on secondary seal housing 5 outside, the temperature conditions of and secondary seal housing 5 inside inner for Real-time Obtaining once sealing housing 2.The temperature information that temperature controller 10 feeds back according to the platinum resistance temperature sensor 3 of different parts, the temperature of being carried out each temperature measuring point and temperature control point by Fuzzy Adaptive PID Control algorithm is compared, and send different steering orders to the drive circuit module 11 being installed on secondary seal housing 5 outside according to comparative result by cable 12, drive circuit module 11 carries out the accurate control work of temperature according to the operation that the PID steering order that receives controls semiconductor refrigerating heap 6 and fan 8.In order to make the homogeneous temperature temperature variation of optical path system 1, in the opposite of secondary seal housing 5, a set of thermal controls apparatus being respectively installed, having mainly contained semiconductor refrigerating heap 6, weblike heat interchanger 7, fan 8 formed.Its installation situation is: weblike heat interchanger 7 about 1/3 part is installed on the inside of semiconductor refrigerating heap 6 and piles 6 closed seamless with semiconductor refrigerating and be connected, exchange heat is made to reach the most sufficient situation, two fans 8 are installed on the same side of two weblike heat interchangers 7, and installation site should be consistent with left or same right.When the PID of temperature controller 10 controls to send temperature control command, drive circuit module 11 starts normal work, drive the semiconductor refrigerating heap 6 based on peltier effect, semiconductor refrigerating heap 6 can carry out heating or refrigerating operation under the control of direction of current.When the temperature generation subtle change of semiconductor refrigerating heap 6, start fan 8 and control rotating speed, the weblike heat interchanger 7 that semiconductor refrigerating piles 6 inside can carry out very rapidly responding to and heat transfer piles the part beyond 6 to semiconductor refrigerating, and rapidly heat to be delivered to nitrogen 9(by fan 8 also can be the clean gas that other thermal conductivity coefficients are very little) in atmosphere, carry out the circulation controlling accelerated heat atmosphere flexibly.The material of weblike heat interchanger 7 is generally metal material, has fabulous thermal conductivity, can carry out heat interchange fast.Under the effect of above thermal controls apparatus, heat-exchange gas is according to forming gas laminar flow 4 clockwise or counterclockwise, clockwise or anticlockwise gas laminar flow 4 is subject to the impact of secondary seal housing 5, be characterized in that central speed is large, edge flow velocity is little, thus on once sealing housing 2 shell of optical path system 1, heat interchange air-flow is defined, facilitate control time and the heat exchanger effectiveness of temperature greatly, adding nitrogen 9 is also the material that a kind of thermal conductivity coefficient is very little, therefore the heat interchange formed between optical path system 1 and flowing nitrogen 9 is very little, thus ensure that the stability of temperature.Meanwhile, temperature controller 10 treatment temperature situation of change in real time, sends instruction in real time to drive circuit module 11 in the course of the work, and drive circuit module 11 carries out cycle control according to the instruction received in real time thus reaches the object of heat isolation and homogeneous temperature.When guarantee said temperature accurately controls and is stable, the spectral technique isotope analysis of integration chamber is in duty accurately, namely optical system is in the course of work of normal table, that is: Distributed Feedback Laser 302 is subject to the laser driving source 308 driving generation modulated laser being installed on once sealing housing 2 and secondary seal housing 5 outside, laser beam after modulation forms (spot diameter≤1mm) collimated light beam 303 through beams converge collimation lens set 302, after the gas to be measured 305 of collimated light beam 303 through optics cavity 304 inside absorbs, converge on the photosurface of InGaAs detector 307 through laser beam plus lens 306, it converges spot size≤1mm
2, the signal then after photoelectricity turns sends into by cable 12 inverting that the signal subsequent processing units 309 being installed on once sealing housing 2 and secondary seal housing 5 outside carries out follow-up signal transacting and gas isotopic abundance.Above-described all parts is all in nitrogen 9 atmosphere of once sealing housing 2 inside and secondary seal housing 5 inside, guarantees the existence of noiseless gas.Finally guarantee that the accuracy of integration chamber spectral technique isotope analysis temperature influence in measuring process, stability and zero shift problem are reduced to minimum.The power supply used in above-mentioned integration chamber spectral technique isotope analysis system provides by DC-24V power supply.
Non-elaborated part of the present invention belongs to techniques well known.