CN105203502A - In-situ online collection analysis meter and method for aerosol carbonaceous components - Google Patents

In-situ online collection analysis meter and method for aerosol carbonaceous components Download PDF

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CN105203502A
CN105203502A CN201510501754.XA CN201510501754A CN105203502A CN 105203502 A CN105203502 A CN 105203502A CN 201510501754 A CN201510501754 A CN 201510501754A CN 105203502 A CN105203502 A CN 105203502A
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gas
parsing
valve
boiler tube
joint
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CN105203502B (en
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曾立民
薛瑞
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Peking University
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Peking University
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Abstract

The invention discloses an in-situ online collection analysis meter for aerosol carbonaceous components and an operation method. The meter comprises a carrier gas path system and a sampling-analyzing gas path system. The carrier gas path system comprises a main He gas path, a He gas purging path, a He/Ox gas path and a He/CH4 gas path. The sampling-analyzing gas path system comprises a sampling and analyzing-oxidizing furnace and an analyzing gas path. The online collection analysis method sequentially comprises the steps of sampling, purging, OC analyzing, EC analyzing, methane quantifying, methane determining, meter cooling and standby. According to the meter, other structures except quartz film are not arranged in a laser light path, so the accuracy of the light path is guaranteed; cutting points are calibrated at the same time through transmission lasers and reflection lasers, and change in blackness of the film is reflected comprehensively; a valve body is designed to greatly lower the quantitative error of internal standard gas of methane, so the stability of the internal standard gas is guaranteed, and the accuracy of measured results of EC and OC is improved; the gas paths are designed to guarantee the singularity of components of carrier gas in the systems and the stability of the system background at the analysis phase.

Description

A kind of gasoloid carbonaceous components original position online acquisition analyser and method thereof
Technical field
The present invention relates to environmental quality monitoring instrument, particularly relate to a kind of gasoloid carbonaceous components original position online acquisition analyser and online acquisition analytical approach thereof.
Background technology
Carbonaceous components in atmospheric aerosol, accounts for the 10-70% of Fine Particles mass concentration usually, is the important composition composition of Fine Particles.It can be divided into three major types: organic carbon (OrganicCarbon, OC), elemental carbon (ElementalCarbon, EC) and carbonic acid carbon (CarbonateCarbon, CC).OC refers to a kind of mixture containing hundreds of organic compound (as aliphatics, aromatic series, acids etc.), be mainly derived from the discharge of primary combustion process, biological discharge, and gaseous organic pollutant participates in the discharge of the gentle grain conversion process of photochemical reaction.EC typically refers to the carbonaceous material such as fossil fuel or the living beings agraphitic carbon that directly a kind of crystallinity of discharge is very low after rough burning.CC is mainly present in the corase particles of soil and colliery flying dust, and its mass concentration much smaller than OC and EC, therefore is generally left in the basket.
Carbonaceous components in atmospheric aerosol can have an impact to aspects such as global climate, atmospheric visibility and healths.EC is as optical absorption composition topmost in atmospheric aerosol, not only can absorb the full wave light from infrared to ultraviolet, the color of particle can also be deepened, make some originally not absorb radiation or absorb less particle to produce light absorption, thus increase positive radiation forces.In addition, carbonaceous aerosol can also change concentration and the life-span of water dust in air as the nucleus of condensation, remote effect radiation balance of earth.In visibility, EC significantly can reduce the visibility of regional atmospheric to the large absorption of light intensity and OC to the scattering process of light.In health, the carbonaceous components major part in gasoloid is present in fine particle (0.1-1 μm), and the respiration thus easily via human body enters lung, destroys the 26S Proteasome Structure and Function of lung, causes chronic respiratory disease etc.Therefore, the carbonaceous components of research atmospheric aerosol is significant, also becomes the focus in current environmental monitoring field.
At present, to the research of the carbonaceous components of atmospheric aerosol, mainly contain two kinds of methods: film sampling off-line analysis method and on-line sampling analytic approach.Compared with off-line analysis method, on-line sampling analytic approach overcomes the shortcoming that its temporal resolution is low, artificial interference is larger, has larger application market.But at present commercial online gasoloid carbonaceous components analyser also comes with some shortcomings on 26S Proteasome Structure and Function: 1, cut point bearing calibration is single, only use a certain of transmission laser correction method or reflects laser correction method, can not the change of concentrated expression film blackness; What the heat 2, on quartz film was mainly fired from quartz ampoule inside one encloses the structure and ambient air transmission that contact with quartz film, heats slow and uneven; 3, a quartzy thin slice is fired in boiler tube inside, in use can be polluted, and affects the accuracy of light path; 4, carrier gas uses waste and unreasonable distribution: in methane, gas whole process is discharged, and causes larger waste; Carrier gas consumption is non-constant in whole analytic process, becomes helium+oxygen, background fluctuations can be caused to affect measurement result from helium.5, the valve body structure controlling methane quantitative loop has larger dead volume, and methane peak can be caused unstable.
Summary of the invention
In order to overcome above-mentioned the deficiencies in the prior art, the invention provides a kind of gasoloid carbonaceous components original position online acquisition analyser, this instrument does not arrange other structures except quartz film in laser optical path, ensure that the accuracy of light path; Also achieve transmission laser and reflects laser corrects cut point simultaneously, the change of concentrated expression film blackness; Valve design makes the quantitative error of gas in methane greatly reduce, and ensure that the stable of interior gas, improves the accuracy of organic carbon (OrganicCarbon, OC) and elemental carbon (ElementalCarbon, EC) measurement result; Gas circuit design ensure that carrier gas composition constant in analysis phase system, ensure that the stable of system background.
Principle of work of the present invention is: utilize quartz film to gather aerosol sample, and first stepped heating quartz film under the non-oxidizing atmosphere of He gas, evaporates the OC in particle (some OC carbonizes into EC), then add He/O in carrier gas xand continue cascade raising temperature, make it overflow EC oxidation.OC and EC overflowed from quartz film enters oxidation boiler tube, through MnO 2catalysed oxidn change into CO 2, finally enter NDIR detecting device quantitative.In whole heating process, generating laser launches beam of laser all the time, arrives transmission laser signal detector and reflected laser signals detecting device after quartz film transmittance and reflectance.Transmission laser and reflects laser weaken along with the charing of OC when starting, afterwards again along with the oxygenolysis of EC strengthens gradually, think when returning to initial light intensity and arrive the cut-point of OC, EC, that is: the carbonaceous components that before this point, thermal decomposition goes out is OC, and the carbonaceous components after this point is EC.
Technical scheme provided by the invention is:
A kind of gasoloid carbonaceous components original position online acquisition analyser of Patent design of the present invention, comprises carrier gas air-channel system and sampling-analysis air-channel system two part;
Described carrier gas air-channel system comprises the main gas gas circuit of He, He sweep gas gas circuit, He/Ox gas gas circuit and He/CH 4gas gas circuit;
The main gas gas circuit of described He is made up of He gas cylinder gas, the first reduction valve, the first mass flow controller and the first three-way solenoid valve connected successively;
Described He sweep gas gas circuit is made up of the described He gas cylinder gas connected successively, described first reduction valve and the second mass flow controller;
Described He/Ox gas gas circuit is made up of the He/Ox gas cylinder gas connected successively, the second reduction valve, the 3rd mass flow controller, the second three-way solenoid valve and the 3rd three-way solenoid valve;
Described He/CH 4gas gas circuit is by the He/CH connected successively 4gas cylinder gas, the 3rd reduction valve, the 4th mass flow controller and six-way valve form;
Described first reduction valve is connected with described second mass flow controller with described first mass flow controller by the first three-way connection; Described first mass flow controller is connected with the normal-closed end of described second three-way solenoid valve with the Chang Kaiduan of described first three-way solenoid valve by the second three-way connection; Three mouthfuls of described first three-way solenoid valve normal-closed end and described six-way valve are connected; The Chang Kaiduan of described second three-way solenoid valve is connected with the common port of described 3rd three-way solenoid valve; The common port of described second three-way solenoid valve is connected by with described six-way valve four mouthfuls of the 3rd three-way connection and described 3rd mass flow controller; Two mouthfuls of described six-way valve are connected with five mouthfuls, as the quantitative loop of gas in methane; Six mouthfuls of described six-way valve are set to He/CH 4the emptying end of gas; Described 4th mass flow controller is connected with a bite of described six-way valve;
Described sampling-analysis air-channel system comprises sampling gas circuit, parsing-oxidation furnace and analyzes gas circuit;
Described parsing-oxidation furnace comprises parsing-oxidation boiler tube; Described parsing-oxidation boiler tube comprises resolves stove supervisor, parsing stove looped pipeline and oxidation boiler tube;
Described sampling gas circuit comprise connect successively cutting head, volatile organic compounds (VOCs) remove pipe, ball valve, parsing-oxidation boiler tube, two-way electromagnetic valve, the 5th mass flow controller and sampling pump; In described sampling gas circuit, described VOCs removes pipe and is connected with the primary air inlet of described ball valve; Front end, described ball valve gas outlet arranges a side-inlet, and described ball valve gas outlet is connected with described ball valve side-inlet; The side-inlet of described ball valve is connected with the common port of described first three-way solenoid valve; The gas outlet of described ball valve connects the parsing stove supervisor of described parsing-oxidation boiler tube by the first joint; Described two-way electromagnetic valve primary air inlet rear end arranges a side-inlet, and the primary air inlet of described two-way electromagnetic valve is connected with the side-inlet of described two-way electromagnetic valve; The primary air inlet of described two-way electromagnetic valve is connected with the parsing stove looped pipeline of described parsing-oxidation boiler tube by the second joint; The side-inlet of described two-way electromagnetic valve is connected with described second mass flow controller; The gas outlet of described two-port valve is connected with described 5th mass flow controller;
Described analysis gas circuit comprises the parsing-oxidation boiler tube of the described parsing-oxidation furnace connected successively, the 4th three-way solenoid valve, NDIR (Non-Dispersive Infrared) spectrum (NDIR) detecting device and flowmeter;
Described first joint and the second joint inside arrange a reflects laser corrective system and a transmission laser corrective system; The outlet of the oxidation boiler tube of described parsing-oxidation boiler tube is connected by the common port of the 3rd joint with described 4th three-way solenoid valve; The normal-closed end of described 4th three-way solenoid valve is connected with the normal-closed end of described 3rd three-way solenoid valve; The inlet end of Chang Kaiduan and the NDIR detecting device of described 4th three-way solenoid valve is connected; Described NDIR detecting device endpiece is connected with described flowmeter inlet end; Described flowmeter outlet end is set to the emptying end of tail gas.
For above-mentioned gasoloid carbonaceous components original position online acquisition analyser, further, in described carrier gas air-channel system and sampling-analysis air-channel system, connect described steel cylinder gas, pipeline that reduction valve, mass flow controller, sampling cutting head, VOCs remove pipe and ball valve adopts stainless-steel tube or copper pipe; All the other gas circuits adopt stainless-steel tube, copper pipe, silicone rubber tube or polyfluortetraethylene pipe.
For above-mentioned gasoloid carbonaceous components original position online acquisition analyser, further, described parsing-oxidation boiler tube also comprises the first arm, the second arm and be enclosed within described parsing stove supervisor in sample feeding pipe, the axis of each described pipe fitting is in the same plane; Described parsing-oxidation furnace also comprises shell, electric furnace heating wire and K type thermopair; K type thermopair comprises the first thermometric K type thermopair and the second thermometric K type thermopair; Described parsing-oxidation boiler tube is placed in described shell; The manganese dioxide-catalyst of the pure level of the inner Filling Analysi of center section of described oxidation boiler tube;
Described sample feeding pipe to be responsible for described parsing stove by the 4th joint and to be fixedly connected with; Described parsing stove supervisor and described parsing stove looped pipeline in alignment, and fire a quartzy porous plate in the middle of junction, quartz film is placed in described sample feeding pipe and described quartzy porous plate centre; Described parsing-oxidation boiler tube is at position outer wrap one electric furnace heating wire corresponding to described quartzy porous plate; Described parsing stove supervisor and described parsing stove looped pipeline junction also arrange described oxidation boiler tube and described first arm, be responsible for the linear vertical at place, and both lay respectively at this straight line both sides with described parsing stove; End closure before described first arm, it is inner inserts described first thermometric K type thermopair, and is fixed by the 5th joint, end in contact before described first thermometric K type thermopair top and described first arm; Described second arm is arranged on described oxidation boiler tube center section near described parsing stove supervisor side, and vertical with described oxidation boiler tube, described second arm front end open-ended; Described second thermometric K type thermopair is placed in described oxidation boiler tube outside, and be oxidized furnace tube outer wall described in end in contact before described second thermometric K type thermopair, described oxidation boiler tube is wrapped in another electric furnace heating wire together with described second thermometric K type thermopair; The gas outlet of described second arm is connected with the Chang Kaiduan of described 3rd three-way solenoid valve by the 6th joint.
The shell of above-mentioned parsing-oxidation furnace is aluminium sheet, be close to described outer casing inner wall and have one layer of heat preservation plate, burner hearth is divided into Resolution Room and oxidizing chamber two parts by a part of described warming plate: described parsing boiler tube supervisor, described parsing stove looped pipeline and described first arm are positioned at described Resolution Room; Described oxidation boiler tube and described second arm are positioned at described oxidizing chamber; Described warming plate adopts mullite material to be processed into; The insulation material of ceramic fiber cotton is filled in described oxidizing chamber inside.
Parsing-oxidation furnace is provided with a blower fan of being sidelong by described parsing stove supervisor side, described quartzy porous plate position in the corresponding described Resolution Room in described fan outlet position; Described shell and the corresponding air outlet position of described warming plate are emptied; Described shell upper is provided with a ventilation duct, and described ventilation duct and described shell junction are positioned at directly over described quartzy porous plate, and described shell and the corresponding position, junction of described warming plate are emptied; Described ventilation duct exit is arranged on the outside of described gasoloid carbonaceous components original position online acquisition analyser.
In parsing-oxidation furnace, the operating voltage of electric furnace heating wire is 220V, and power is 1500W, and its outer cover has quartz fibre sleeve pipe, and described electric furnace heating wire adoption rate integral calculus carries out computer heating control in conjunction with pulse-width modulation method.
Resolve-be oxidized boiler tube each several part and be high temperature resistant quartz material, described parsing boiler tube is responsible for as external diameter is 20 millimeters, described parsing boiler tube looped pipeline external diameter is 10 millimeters, described oxidation boiler tube center section external diameter is 13 millimeters, described first arm and described second arm external diameter are 6.35 millimeters, and described sample feeding pipe external diameter is 16 millimeters.
In parsing-oxidation furnace, described quartzy porous plate is an annulus quartz plate being evenly distributed with six small sircle holes, and the internal diameter of described annulus quartz plate is 6 millimeters, and external diameter is 17 millimeters, and the diameter of small sircle hole is 2 millimeters; Described quartz film contacts with described quartzy porous plate, and described quartzy porous plate plays the effect of support to described quartz film.
In parsing-oxidation furnace, further, the first joint and the second joint inside arrange a reflects laser corrective system and a transmission laser corrective system;
Described reflects laser corrective system comprises a generating laser, piezoid, the first optical filter and a reflected laser signals detecting device; Described transmission laser corrective system comprises described generating laser, described piezoid, the second optical filter and transmission laser signal detector;
It is inner that described reflects laser corrective system is positioned at described first joint: described first joint arranged outside one is for plugging the generating laser groove of fixing described generating laser, and the center line of described generating laser groove overlaps with the center line of described first joint; Described piezoid encloses sealing by O and is fixed in described generating laser groove, and is close to the placement of described generating laser front end; Described generating laser groove front end also arranges first air drain be communicated with described sample feeding pipe; Described first joint side arranges one perpendicular to the second air drain of described first air drain, is interconnected between described first air drain and described second air drain; One is also arranged for plugging the reflected laser signals detecting device groove of fixing described reflected laser signals detecting device inside described first joint; Described first optical filter encloses sealing by O and is fixed in described reflected laser signals detecting device groove, and is close to the placement of described reflected laser signals detecting device front end; It is inner that described transmission laser corrective system is positioned at described second joint: described second joint arranged outside one is for plugging the transmission laser signal detector groove of fixing described transmission laser signal detector, and its center line overlaps with the center line of described second joint; Described second optical filter encloses sealing by O and is fixed in described transmission laser signal detector groove, and is close to the placement of described transmission laser signal detector front end; Described transmission laser signal detector groove front end also arranges the 3rd air drain be communicated with described looped pipeline; Described second joint side also arranges one perpendicular to the 4th air drain of described 3rd air drain, is interconnected between described 3rd air drain and described 4th air drain.
Above-mentioned generating laser adopts that center emission wavelength is 660nm, the point-like red laser transmitter of power to be 50mW and transmission frequency be 1Hz; It is the optical filter of 8nm that described optical filter adopts centre wavelength to be 660nm and bandwidth; Described transmission laser signal detector and reflected laser signals detecting device are the photodiode that can produce highly sensitive linear response to 660nm laser.
In above-mentioned gasoloid carbonaceous components original position online acquisition analyser, first, second joint is the aluminium matter joint of interior configuration O circle; Three, the 5th, the 6th joint is the stainless joint of interior configuration O circle; 4th joint is the adapter of plastic of interior configuration O circle.
Gasoloid carbonaceous components original position online acquisition analyser provided by the invention operationally, by control circuit, single-chip microcomputer and industrial computer triplicity, realizes the Automated condtrol to acquisition and analysis instrument; Described control circuit provides operating voltage and DO, AO control signal for all hardware in acquisition and analysis instrument, is responsible for gathering and amplifying corresponding detection signal simultaneously, carries out A/D conversion, then by described industrial computer is read and identifies for described single-chip microcomputer; Described NDIR detecting device then directly communicates with described industrial computer.The computer software write by utilizing computerese carries out Automated condtrol to acquisition and analysis instrument neatly, and carries out automatic analysis to data; This computer software comprises control program and data processor two parts; Be nested with state display window to change mouth in described control program, setting parameter window, each valve body control separately window, calibration curve window; Described state display window to change mouth can show the parameter of the real-time running state of acquisition and analysis instrument and temperature, flow, laser, NDIR, and described setting parameter window can carry out each carrier gas flux, sampling time and flow, heating schedule, temperature control pid parameter, CO 2the setting of time delay, described each valve body controls separately the opening and closing that window can control each valve body, so that status checking and malfunction elimination; Described calibration curve window can generate typical curve automatically according to the multi-point calibration result of input; Described data processor can obtain OC and the EC concentration of sample according to typical curve.
The present invention also provides the online acquisition analytical approach utilizing above-mentioned gasoloid carbonaceous components original position online acquisition analyser, comprises sample phase, purge stages, OC analysis phase, EC analysis phase, methane quantitative stage, methane calibration phase, instrument cooling and standby phase successively; Specifically comprise following process:
1) sample phase: gather air sample by sampling gas circuit;
Sampling time and sampling flow can according to atmospheric pollution situation by user's sets itself;
After sample phase starts, the ball valve 212 of instrument (gasoloid carbonaceous components original position online acquisition analyser), pump 215, two-way electromagnetic valve 213, blower fan 24 are opened, air enters cutting head 210 successively under the effect of pump 215, VOCs removes pipe 211, ball valve 212, and enters in parsing stove supervisor 2210 by joint 220; When air sample is by quartz film 2218, particle is trapped within quartz film 2218; Meanwhile, the main gas of He is entered by the side-inlet of mass flow controller 112, three-way solenoid valve 113, ball valve 212 and resolves stove supervisor 2210; He/O xcarrier gas by mass flow controller 132, three-way solenoid valve 133, three-way solenoid valve 134, three-way solenoid valve 230, enter oxidation boiler tube 2212; The main gas of He, He/O xcarrier gas and sampled air are mixed together and are discharged after resolving stove looped pipeline 2211, two-way electromagnetic valve 213, mass flow controller 214, sampling pump 215.In this process, the main gas of He and He/O xcarrier gas ensures that resolving-be oxidized boiler tube 221 is in dry environment, prevents steam from entering in oxidation boiler tube 2212 and causes catalyst poisoning; Each three-way solenoid valve and six-way valve all keep non-"on" position: C (public) end of three-way solenoid valve valve body is communicated with NO (often opening) end, and 12 mouthfuls, 34 mouthfuls, 56 mouthfuls of six-way valve communicate; Oxidation furnace keeps 500 DEG C; Sampling time and sampling flow can according to atmospheric pollution situation by user's sets itself.
2) the main gas of purge: He, He sweep gas and He/O xcarrier gas is mixed together, and purge continues for some time;
After purge stages starts, instrument ball valve 212, pump 215, two-way electromagnetic valve 213, blower fan 24 are closed, and He primary air road is constant; He sweep gas is entered by the side-inlet of mass flow controller 122, two-way electromagnetic valve 213 and resolves stove looped pipeline 2211; He/O xcarrier gas enters arm 2215 by mass flow controller 132, three-way solenoid valve 133, three-way solenoid valve 134; The main gas of He, He sweep gas and He/O xcarrier gas is mixed together by oxidation boiler tube 2212, three-way solenoid valve 230, NDIR detecting device 231, flowmeter 232 being discharged.Purge continues 200s, and to ensure gas remaining in boiler tube fully to be blown out, and quartz film 2218 is in non-oxidizing atmosphere.In this process, resolve stove and keep 10 DEG C, oxidation furnace is rapidly heated and remains on 870 DEG C, and at the 30s reciprocal of purge stages, software starts record each supplemental characteristic and start drawing image.
3) OC analytic process: OC is volatilized by progressively Thermal desorption in He gas oxygen-free environment; Be converted into CO 2and it is quantitative by NDIR detecting device;
OC analytic process: after OC analytic process starts, each valve body and mass flow controller state remain unchanged, namely each carrier gas flux and gas circuit flow to and remain unchanged.OC on quartz film 2218 user in the heating schedule of main separation by progressively Thermal desorption out, enter in oxidation boiler tube 2212 and be converted into CO 2and it is quantitative by NDIR detecting device 231; Oxidation furnace keeps 870 DEG C.
4) EC analytic process: EC is oxidized in an oxidizing environment, is further converted to CO 2and it is quantitative by NDIR detecting device;
After EC analytic process starts, three-way solenoid valve 113,133 and 134 is opened, and namely the C end of valve body is communicated with NC end, and all the other three-way solenoid valves still keep non-"on" position.He sweep gas gas circuit remains unchanged, and the main gas of He enters 4 mouthfuls of six-way valve 143 by mass flow controller 112, three-way solenoid valve 133; He/O xcarrier gas is mixed with the main gas of He by mass flow controller 132, three-way connection 153, then enters resolve stove supervisor 2210 through six-way valve 143, three-way solenoid valve 113; In this process, quartz film 2218 is in well-oxygenated environment, and the EC that on it, original EC and a part of OC carbonize is oxidized in heating schedule, enters in oxidation boiler tube 2212 and is further converted to CO 2and it is quantitative by NDIR detecting device 231; Oxidation furnace 2212 keeps 870 DEG C.
5) methane dosing process: inject He/CH in quantitative loop 4interior gas;
After methane dosing process starts, each valve body state and upper stage are consistent, the main gas of He, He sweep gas and He/O xcarrier gas gas circuit and flow all remain unchanged; Mass flow controller 142 is opened, He/CH 4interior gas enters the pipeline (quantitative loop) of six-way valve 2 mouthfuls and 5 mouthfuls centres by mass flow controller 142, six-way valve 1 mouthful, and this process maintains 50s, treats He/CH 4after interior gas is full of quantitative loop, unnecessary He/CH 4interior gas is by 6 mouthfuls of discharges of six-way valve.In this process, blower fan 24 is opened, and lowers the temperature to parsing boiler tube 2210; Oxidation boiler tube 2212 keeps 870 DEG C.
6) the main gas of methane calibration process: He and He/O xcarrier gas combination gas is by He/CH original in quantitative loop 4interior gas blows out and is oxidized, and is converted into CO 2quantitative by NDIR detecting device;
After methane calibration process starts, each three-way solenoid valve valve body state and upper stage are consistent, and six-way valve 143 is opened, and namely 16 mouthfuls, 23 mouthfuls, 45 mouthfuls of valve body are connected; Mass flow controller 142 cuts out, He/CH 4flow is 0.He sweep gas gas circuit remains unchanged; The main gas of He enters six-way valve 143 by mass flow controller 112, three-way solenoid valve 133; He/O xcarrier gas is mixed with the main gas of He by mass flow controller 132, three-way connection 153, the main gas of He and He/O xcarrier gas combination gas enters six-way valve 143, by He/CH original in quantitative loop 4interior gas is blown into three-way solenoid valve 113, finally enters and resolves stove supervisor 2210, and is converted into CO in oxidation boiler tube 2212 2and it is quantitative by NDIR detecting device 231.This process maintains 15s, and period blower fan 24 maintenance is opened, and continues cooling to parsing stove 2210; Oxidation furnace 2212 keeps 870 DEG C.
7) cooling procedure: instrument is lowered the temperature, and automatically stops the analysis phase, preserves data and curve, enters standby;
After cooling procedure starts, state and the EC process of each three-way solenoid valve body and mass flow controller are consistent, and six-way valve cuts out; Blower fan 24 maintains to be opened, and continues cooling to parsing boiler tube 2210; Oxidation boiler tube 2212 keeps 870 DEG C.When resolving boiler tube 2210 temperature and being down to below 75 DEG C, instrument stops the analysis phase automatically, preserves data and curve, enters standby, waits pending-analysis of next time sampling.
8) standby: wait pending-analysis of next time sampling.
After cooling procedure terminates, instrument enters standby, and state and the purge of each valve body and mass flow controller are consistent, and namely each carrier gas flux flows to consistent with purge with gas circuit.Blower fan maintains to be opened, and resolve furnace temperature and be set as 10 DEG C, oxidation furnace temperature is down to 500 DEG C.
Compared with prior art, the invention has the beneficial effects as follows:
The invention provides a kind of gasoloid carbonaceous components original position online acquisition analyser, other structures except quartz film are not set in laser optical path, ensure that the accuracy of light path; Also achieve transmission laser and reflects laser corrects cut point simultaneously, the change of concentrated expression film blackness; Valve design makes the quantitative error of gas in methane greatly reduce, and ensure that the stable of interior gas, improves the accuracy of EC, OC measurement result; Gas circuit design ensure that in whole analysis phase system, carrier gas composition remains unchanged, and ensure that the stable of system background.The present invention takes above technical scheme, particularly, has the following advantages:
1, other structures except quartz film are not set in laser optical path, the laser that LASER Light Source sends directly arrives reflection and transmission laser detecting device after quartz film reflection and transmission, effectively ensure that the accuracy of the laser that detecting device receives, make the judgement of cut-point more accurate;
2, comprehensive employing reflects laser photodetector system and transmission laser photodetector system, the blackness change of quartz film surface and thickness direction can be reflected simultaneously, be convenient to comprehensive descision cut-point, and the time interval of transmission laser and reflects laser OC/EC cut-point can also reflect the quick degree that system heats up further;
3, use six-way valve to gas in methane quantitatively and injection control, greatly reduce the situation of gas volume instability in causing because three-way solenoid valve valve body dead volume is excessive, improve the accuracy of EC, OC measurement result;
4, designed, designed air-channel system, rational arrangement has been carried out to the use of each gas, not only save the use amount of carrier gas efficiently, in whole workflow, also achieved the consistance of carrier gas, improve the stability of analysis phase stove intracavity gas background and gas pressure intensity; And all have carrier gas to pass through around generating laser, transmittance and reflectance laser detector, take away a part of heat of generating laser, the generation of transmittance and reflectance laser detector, be conducive to the stable of laser detection system;
5, the temperature of stove silk controls adoption rate integral calculus algorithm in conjunction with pulse width modulating technology, makes continuous heating become PULSE HEATING, increases the serviceable life of stove silk, and the long-term stability being conducive to instrument is run.
The present invention is practical, and operating cost is low, convenient management, is applicable to the use of laboratory study and environmental protection automatic monitor station in all parts of the country, can obtain data that are more true and atmospheric aerosol carbonaceous components accurately.
Use technical scheme provided by the invention, Monitoring Data more accurately can be obtained, provide support for more clearly understanding aerocolloidal pollution situation, control atmosphere pollution and improving air quality.
Accompanying drawing explanation
Fig. 1 is the structural drawing of the gasoloid carbonaceous components original position online acquisition analyser that the embodiment of the present invention provides;
Fig. 2 is the structural drawing of parsing-oxidation furnace that the embodiment of the present invention provides;
In Fig. 1 ~ Fig. 2,1-carrier gas air-channel system; 2-sampling-analyze air-channel system; The main gas gas circuit of 11-He; 12-He sweep gas gas circuit; 13-He/O xgas gas circuit; 14-He/CH 4gas gas circuit; 110-He gas cylinder gas 110; 111-the first reduction valve; 112-the first mass flow controller; 113-the first three-way solenoid valve; 122-the second mass flow controller; 130-He/O xgas cylinder gas; 131-the second reduction valve; 132-the three mass flow controller; 133-the second three-way solenoid valve; 134-the three three-way solenoid valve; 140-He/CH 4gas cylinder gas; 141-the three reduction valve; 142-the four mass flow controller; 143-six-way valve; 151-the first three-way connection; 152-the second three-way connection; 153-the three three-way connection; 21-sampling gas circuit; 22-parsing-oxidation furnace; 23-analyze gas circuit; 210-cutting head; 211-VOCs removes pipe; 212-ball valve; 213-two-way electromagnetic valve; 214-the five mass flow controller; 215-sampling pump; 220-the first joint; 221-resolve-oxidation boiler tube; 222-the second joint; 223-the three joint; 224-electric furnace heating wire; 225-K type thermopair; 226-shell; 227-the four joint; 228-the five joint; 229-the six joint; 230-the four three-way solenoid valve; 231-NDIR detecting device; 232-flowmeter; 2210-resolve stove supervisor; 2211-resolve stove looped pipeline; The oxidation boiler tube of 2212-parsing-oxidation boiler tube; 2214-the first arm; 2215-the second arm; 2216-sample feeding pipe; 2217-quartzy porous plate; 2218-quartz film;
Fig. 3 is the structural drawing of the laser-adjusting system that the embodiment of the present invention provides;
Fig. 4 is the structural drawing of the reflects laser corrective system that the embodiment of the present invention provides;
Fig. 5 is the structural drawing of the transmission laser corrective system (not containing generating laser) that the embodiment of the present invention provides;
In Fig. 3 ~ Fig. 5,30-reflects laser corrective system; 31-transmission laser corrective system; 301-generating laser; 302-piezoid; 303-the first optical filter; 304-reflected laser signals detecting device; 310-the second optical filter; 311-transmission laser signal detector; 305-generating laser groove; 306-the first air drain; 307-the second air drain; 308-reflected laser signals detecting device groove; 312-transmission laser signal detector groove; 313-the three air drain; 314-the four air drain.
Fig. 6 is gasoloid carbonaceous components original position online acquisition analyser each stage workflow block diagram that the embodiment of the present invention provides.
Embodiment
Below in conjunction with accompanying drawing, further describe the present invention by embodiment, but the scope do not limited the present invention in any way.
The invention provides a kind of gasoloid carbonaceous components original position online acquisition analyser, other structures except quartz film are not set in laser optical path, ensure that the accuracy of light path; Also achieve transmission laser and reflects laser corrects cut point simultaneously, the change of concentrated expression film blackness; Valve design makes the quantitative error of gas in methane greatly reduce, and ensure that the stable of interior gas, improves the accuracy of EC, OC measurement result; Gas circuit design ensure that carrier gas composition constant in analysis phase system, ensure that the stable of system background.
As shown in Figure 1, the gasoloid carbonaceous components original position online acquisition analyser that the embodiment of the present invention provides mainly comprises: carrier gas air-channel system 1 and sampling-analysis air-channel system 2 two parts.Carrier gas air-channel system 1 comprises the main gas gas circuit 11 of He, He sweep gas gas circuit 12, He/O xgas gas circuit 13 and He/CH 4gas gas circuit 14, wherein: the main gas gas circuit 11 of He is made up of the He gas cylinder gas 110 connected successively, reduction valve 111, mass flow controller 112, three-way solenoid valve 113, He main gas gas circuit 11 is mainly used in controlling main carrier gas He gas; The He gas cylinder gas 110 that He sweep gas route connects successively, reduction valve 111, mass flow controller 122 form, and are mainly used in purging and supplementing bypass gas; He/O xgas gas circuit 13 is by the He/O connected successively xgas cylinder gas 130, reduction valve 131, mass flow controller 132, three-way solenoid valve 133, three-way solenoid valve 134 form; He/CH 4gas gas circuit 14 is by the He/CH connected successively 4gas cylinder gas 140, reduction valve 141, mass flow controller 142, six-way valve 143 form.Reduction valve 111 is connected with mass flow controller 122 with mass flow controller 112 by three-way connection 151; Mass flow controller 112 is connected with the normal-closed end of three-way solenoid valve 133 with the Chang Kaiduan of three-way solenoid valve 113 by three-way connection 152; The normal-closed end of three-way solenoid valve 113 is connected with 3 of six-way valve mouthfuls; The Chang Kaiduan of three-way solenoid valve 133 is connected with the common port of three-way solenoid valve 134; The common port of three-way solenoid valve 133 is connected by with six-way valve 143 4 mouthfuls of three-way connection 153 and described mass flow controller 132; 1 mouthful of mass flow controller 142 and six-way valve 143 is connected; 2 mouthfuls of six-way valve 143 are connected with 5 mouthfuls, as the quantitative loop of gas in methane; 6 mouthfuls of six-way valve 143 are set to He/CH 4the emptying end of gas.
In above-described embodiment, the He gas used in carrier gas air-channel system 1 is high-purity He gas of 99.99%, He/O xgas is O 2volumetric concentration is the combination gas of 10%, He/CH 4for CH 4volumetric concentration is the combination gas of 5%.
In above-described embodiment, connect in carrier gas air-channel system 1 steel cylinder gas, reduction valve, mass flow controller pipeline can adopt stainless-steel tube or copper pipe; All the other gas circuits can adopt stainless-steel tube, copper pipe, silicone rubber tube or polyfluortetraethylene pipe.
As depicted in figs. 1 and 2, sampling of the present invention-analysis air-channel system 2 comprises sampling gas circuit 21, parsing-oxidation furnace 22, analyzes gas circuit 23, wherein: sampling gas circuit 21 comprises the cutting head 210, VOCs removal pipe 211, ball valve 212, parsing-oxidation boiler tube 221, two-way electromagnetic valve 213, mass flow controller 214, the sampling pump 215 that connect successively; VOCs removes pipe 211 and is connected with the primary air inlet of ball valve 212; Front end, ball valve 212 gas outlet arranges a side-inlet, and ball valve 212 gas outlet is connected with side-inlet, and this side-inlet is connected with the common port of three-way solenoid valve 113; The gas outlet of ball valve 212 is responsible for 2210 by joint 220 with the parsing stove resolve-being oxidized boiler tube 221 and is connected; The primary air inlet rear end of two-way electromagnetic valve 213 arranges a side-inlet, and primary air inlet is connected with side-inlet, and primary air inlet is connected by joint 222 resolves stove looped pipeline 2211; The side-inlet of two-way electromagnetic valve 213 is connected with mass flow controller 122; The gas outlet of two-way electromagnetic valve 213 is connected with the air intake opening of mass flow controller 214, and the gas outlet of mass flow controller 214 is connected with sampling pump 215.Analyze gas circuit 23 and comprise the parsing-oxidation boiler tube 221, three-way solenoid valve 230, NDIR detecting device 231, the flowmeter 232 that connect successively, the outlet of resolving-being oxidized the oxidation boiler tube 2212 of boiler tube 221 is connected by the common port of joint 223 with three-way solenoid valve 230; The normal-closed end of three-way solenoid valve 230 is connected with the normal-closed end of three-way solenoid valve 134; The inlet end of Chang Kaiduan and the NDIR detecting device 231 of three-way solenoid valve 230 is connected; The endpiece of NDIR detecting device 231 is connected with the inlet end of flowmeter 232; The endpiece of flowmeter 232 is set to the emptying end of tail gas.Parsing-oxidation furnace 22 comprises parsing-oxidation boiler tube 221, electric furnace heating wire 224, K type thermopair 225, shell 226.Resolve-oxidation boiler tube 221 is placed in described shell 226; Resolve-oxidation boiler tube 221 comprise resolve stove supervisor 2210, resolve stove looped pipeline 2211, oxidation boiler tube 2,212 first arm 2214, second arm 2215 and is enclosed within the sample feeding pipe 2216 of resolving in stove supervisor 2210, each pipe fitting axis is in the same plane.Sample feeding pipe 2216 is responsible for 2210 by joint 227 with parsing stove and is fixedly linked; Resolve stove supervisor 2210 in alignment with parsing stove looped pipeline 2211, and a quartzy porous plate 2217 is fired in the middle of junction, resolve-be oxidized the position outer wrap electric furnace heating wire 224 of boiler tube 221 in quartzy porous plate 2217 correspondence, in the middle of sample feeding pipe 2216 and quartzy porous plate 2217, place quartz film 2218; Parsing stove supervisor 2210 and looped pipeline 2211 junction arrange oxidation boiler tube 2212 and the first arm 2214, be responsible for the linear vertical at 2210 places, and lay respectively at this straight line both sides with parsing stove; End closure before first arm 2214, it is inner inserts a thermometric K type thermopair 225, and is fixed by joint 228, end in contact before K type thermopair 225 top and the first arm 2214; Second arm 2215 is arranged on oxidation boiler tube 2212 center section and is responsible for 2210 sides near resolving stove, and vertical with oxidation boiler tube 2212, the second arm 2215 front end open-ended; Another thermometric K type thermopair 225, K type thermopair 225 front end catalytic oxidation boiler tube 2212 center section outer wall is placed in oxidation boiler tube 2212 outside; Oxidation boiler tube 2212 is wrapped in electric furnace heating wire 224 described in another together with thermometric K type thermopair 225; The gas outlet of the second arm 2215 is connected with the Chang Kaiduan of three-way solenoid valve 134 by joint 229.
In above-described embodiment, connect sampling cutting head 210, VOCs removes pipe 211, the pipeline of ball valve 212 can adopt stainless-steel tube or copper pipe; All the other gas circuits can adopt stainless-steel tube, copper pipe, silicone rubber tube or polyfluortetraethylene pipe.
In above-described embodiment, joint 220,222 is the aluminium matter joint of interior configuration O circle; Joint 223,225,229 is the stainless joint of interior configuration O circle; Joint 227 is the adapter of plastic of interior configuration O circle.
In above-described embodiment, the manganese dioxide-catalyst of the pure level of the inner Filling Analysi of oxidation boiler tube 2212 center section.
In above-described embodiment, shell 226 is the aluminium sheet of thickness 10 millimeters, be close to shell 226 inwall and have one layer of heat preservation plate, burner hearth is divided into Resolution Room and oxidizing chamber two parts by some warming plate: resolve boiler tube supervisor 2210, parsing stove looped pipeline 221 and the first arm 2214 and be positioned at Resolution Room; Oxidation boiler tube 2212, second arm 2215 is positioned at oxidizing chamber; Warming plate adopts mullite material to be processed into; The insulation material of ceramic fiber cotton is filled in oxidizing chamber inner space.
In above-described embodiment, K type temperature thermocouple 225 connects temperature controller, and temperature controller controls the heating of electric furnace heating wire 224 again by solid-state relay; The operating voltage of electric furnace heating wire 224 is 220V, and power is 1500W, and its outer cover has quartz fibre sleeve pipe, and the computer heating control adoption rate integral calculus algorithm of electric furnace heating wire 224 is in conjunction with pulse width modulating technology.
In above-described embodiment, resolve boiler tube 221 each several part and be high temperature resistant quartz material, being responsible for 2210 external diameters is 20 millimeters, looped pipeline 2211 external diameter is 10 millimeters, oxidation boiler tube 2212 center section external diameter is 13 millimeters, first arm 2214 and the second arm 2215 external diameter are 6.35 millimeters, and sample feeding pipe 2216 external diameter is 16 millimeters.
In above-described embodiment, in order to realize larger sampling flow, the sample that guarantee collects can be evenly distributed on quartz film 2218, and ensures that quartz film 2218 can be heated by Quick uniform, and parsing stove supervisor 2210 and parsing stove looped pipeline 2211 junction are fired and fixed a cellular quartz plate 2217; Place quartz film 2218 in the middle of sample feeding pipe 2216 and quartzy porous plate 2217, cellular quartz plate 2217 and quartz film 2218 fit tightly; Quartz porous plate 2217 is the annulus quartz plates being evenly distributed with 6 small sircle holes, and the internal diameter of annulus quartz plate is 6 millimeters, and external diameter is 17 millimeters, and the diameter of small sircle hole is 2 millimeters.
In above-described embodiment, parsing-oxidation furnace 22 is responsible for 2210 sides by described parsing stove and is provided with a blower fan of being sidelong 24, and its air outlet position correspondence resolves indoor quartzy porous plate 2217 position; Shell 226 and the corresponding air outlet position of warming plate are emptied.Shell 226 top is provided with a ventilation duct 25, and ventilation duct 25 and shell 226 junction are positioned at directly over quartzy porous plate 2217, and the position of shell 2217 and the corresponding junction of warming plate is emptied; Ventilation duct 25 outlet is arranged on instrument outside.
As shown in Fig. 3, Fig. 4 and Fig. 5, first joint 220 and the second joint 222 inside arrange reflects laser corrective system 30 and a transmission laser corrective system 31, and reflects laser corrective system 30 comprises a generating laser 301, piezoid 302, first optical filter 303 and a reflected laser signals detecting device 304; Transmission laser corrective system 31 comprises generating laser 301, second optical filter 310 and transmission laser signal detector 311.It is inner that reflects laser corrective system 30 is positioned at the first joint 220: the first joint 220 arranged outside one is for plugging the generating laser groove 305 of fixed laser transmitter 301, and coaxial with the first joint 220; Piezoid 302 encloses sealing by O and is fixed in generating laser groove 305, and is close to the placement of generating laser 301 front end; The front end of the first joint 220 inner laser transmitter groove 305 also arranges first air drain 306 be communicated with sample feeding pipe 2216; First joint 220 side also arranges one and is interconnected perpendicular between the second air drain 307, first air drain 306 of the first air drain 306 and the second air drain 307; One is also arranged for plugging the reflected laser signals detecting device groove 308 of fixation reflex laser signal detecting device 304 inside first joint 220; First optical filter 303 encloses sealing by O and is fixed in reflected laser signals detecting device groove 308, and is close to the placement of reflected laser signals detecting device 308 front end.It is inner that transmission laser corrective system 31 is positioned at the second joint 222: the second joint 222 arranged outside one is for plugging the transmission laser signal detector groove 312 of fixed transmittance laser signal detecting device 311, and it is coaxial with the second joint 222; Second optical filter 310 encloses sealing by O and is fixed in transmission laser signal detector groove 312, and is close to the placement of transmission laser signal detector 311 front end; In second joint 222, transmission laser photoelectric detector groove 312 front end also arranges the 3rd air drain 313 be communicated with looped pipeline 2211; Second joint 222 side also arrange one perpendicular to the 4th air drain the 314, three air drain 313 of the 3rd air drain 313 and the 4th air drain 314 between be interconnected.
In above-described embodiment, generating laser 301 adopts center emission wavelength 660nm, the point-like red laser transmitter of power 50mW, transmission frequency 1Hz, and its emission of light is concentrated, and dispersion angle is little; Centered by first optical filter 303, second optical filter 310, the optical filter of wavelength 660nm, bandwidth 8nm, effectively can filter the parasitic light of its all band, avoid interference; Reflected laser signals detecting device 309 and transmission laser signal detector 311 are photodiode, can produce highly sensitive linear response to 660nm laser.
The present invention, by control circuit 4, single-chip microcomputer 5 and industrial computer 6 triplicity, realizes the Automated condtrol to whole instrument.Control circuit 4 provides operating voltage and DO, AO control signal for all hardware in whole instrument, is responsible for gathering and amplifying corresponding detection signal simultaneously, carries out A/D conversion, then by industrial computer 6 is read and identifies for single-chip microcomputer 5.NDIR detecting device 231 directly communicates with industrial computer 6.
In above-described embodiment, single-chip microcomputer 5 can be transformed by AD conversion and IO, realizes laser value, (the main gas of He, He purge carrier gas, He/Ox carrier gas and He/CH to resolve furnace temperature angle value, oxidation furnace temperature value, flowmeter flow, sampling and each gas circuit 4interior gas) collection of flow signal, and be presented on the program interface of industrial computer; The real-time control to mass flow controller, three-way solenoid valve, two-way electromagnetic valve, ball valve, electric furnace heating wire, blower fan, sampling pump, generating laser can also be realized simultaneously.The present invention utilizes computerese to write software, comprises control program and data processor two parts, can carry out Automated condtrol flexibly, and carry out automatic analysis to data to acquisition and analysis instrument; Be nested with state display window to change mouth in control program, setting parameter window, each valve body control separately window, calibration curve window: state display window to change mouth can show the parameter of the real-time running state of acquisition and analysis instrument and temperature, flow, laser, NDIR, and setting window can carry out each carrier gas flux, sampling time and flow, heating schedule, temperature control pid parameter, CO 2the setting of time delay, each valve body controls separately the opening and closing that window can control each valve body, so that status checking and malfunction elimination; Calibration curve window can generate typical curve automatically according to the multi-point calibration result of input; Data processor can obtain OC and the EC concentration of sample according to typical curve.
As shown in Figure 6, specific works process of the present invention is as follows:
1) sample phase: after sample phase starts, the ball valve 212 of instrument, pump 215, two-way electromagnetic valve 213, blower fan 24 are opened, air enters cutting head 210 successively under the effect of pump 215, VOCs removes pipe 211, ball valve 212, and enters in parsing stove supervisor 2210 by joint 220; When air sample is by quartz film 2218, particle is trapped within quartz film 2218; Meanwhile, the main gas of He is entered by the side-inlet of mass flow controller 112, three-way solenoid valve 113, ball valve 212 and resolves stove supervisor 2210; He/O xcarrier gas by mass flow controller 132, three-way solenoid valve 133, three-way solenoid valve 134, three-way solenoid valve 230, enter oxidation boiler tube 2212; The main gas of He, He/O xcarrier gas and sampled air are mixed together and are discharged after resolving stove looped pipeline 2211, two-way electromagnetic valve 213, mass flow controller 214, sampling pump 215.In this process, the main gas of He and He/O xcarrier gas ensures that resolving-be oxidized boiler tube 221 is in dry environment, prevents steam from entering in oxidation boiler tube 2212 and causes catalyst poisoning; Each three-way solenoid valve and six-way valve all keep non-"on" position: C (public) end of three-way solenoid valve valve body is communicated with NO (often opening) end, and 12 mouthfuls, 34 mouthfuls, 56 mouthfuls of six-way valve communicate; Oxidation furnace keeps 500 DEG C; Sampling time and sampling flow can according to atmospheric pollution situation by user's sets itself.
2) purge: after purge stages starts, instrument ball valve 212, pump 215, two-way electromagnetic valve 213, blower fan 24 are closed, and He primary air road is constant; He sweep gas is entered by the side-inlet of mass flow controller 122, two-way electromagnetic valve 213 and resolves stove looped pipeline 2211; He/O xcarrier gas enters arm 2215 by mass flow controller 132, three-way solenoid valve 133, three-way solenoid valve 134; The main gas of He, He sweep gas and He/O xcarrier gas is mixed together by oxidation boiler tube 2212, three-way solenoid valve 230, NDIR detecting device 231, flowmeter 232 being discharged.Purge continues 200s, and to ensure gas remaining in boiler tube fully to be blown out, and quartz film 2218 is in non-oxidizing atmosphere.In this process, resolve stove and keep 10 DEG C, oxidation furnace is rapidly heated and remains on 870 DEG C, and at the 30s reciprocal of purge stages, software starts record each supplemental characteristic and start drawing image.
3) OC analytic process: after OC analytic process starts, each valve body and mass flow controller state remain unchanged, namely each carrier gas flux and gas circuit flow to and remain unchanged.OC on quartz film 2218 user in the heating schedule of main separation by progressively Thermal desorption out, enter in oxidation boiler tube 2212 and be converted into CO 2and it is quantitative by NDIR detecting device 231; Oxidation furnace keeps 870 DEG C.
4) EC analytic process: after EC analytic process starts, three-way solenoid valve 113,133 and 134 is opened, and namely the C end of valve body is communicated with NC end, and all the other three-way solenoid valves still keep non-"on" position.He sweep gas gas circuit remains unchanged, and the main gas of He enters 4 mouthfuls of six-way valve 143 by mass flow controller 112, three-way solenoid valve 133; He/O xcarrier gas is mixed with the main gas of He by mass flow controller 132, three-way connection 153, then enters resolve stove supervisor 2210 through six-way valve 143, three-way solenoid valve 113; In this process, quartz film 2218 is in well-oxygenated environment, and the EC that on it, original EC and a part of OC carbonize is oxidized in heating schedule, enters in oxidation boiler tube 2212 and is further converted to CO 2and it is quantitative by NDIR detecting device 231; Oxidation furnace 2212 keeps 870 DEG C.
5) methane dosing process: after methane dosing process starts, each valve body state and upper stage are consistent, the main gas of He, He sweep gas and He/O xcarrier gas gas circuit and flow all remain unchanged; Mass flow controller 142 is opened, He/CH 4interior gas enters the pipeline (quantitative loop) of six-way valve 2 mouthfuls and 5 mouthfuls centres by mass flow controller 142, six-way valve 1 mouthful, and this process maintains 50s, treats He/CH 4after interior gas is full of quantitative loop, unnecessary He/CH 4interior gas is by 6 mouthfuls of discharges of six-way valve.In this process, blower fan 24 is opened, and lowers the temperature to parsing boiler tube 2210; Oxidation boiler tube 2212 keeps 870 DEG C.
6) methane calibration process: after methane calibration process starts, each three-way solenoid valve valve body state and upper stage are consistent, and six-way valve 143 is opened, and namely 16 mouthfuls, 23 mouthfuls, 45 mouthfuls of valve body are connected; Mass flow controller 142 cuts out, He/CH 4flow is 0.He sweep gas gas circuit remains unchanged; The main gas of He enters six-way valve 143 by mass flow controller 112, three-way solenoid valve 133; He/O xcarrier gas is mixed with the main gas of He by mass flow controller 132, three-way connection 153, the main gas of He and He/O xcarrier gas combination gas enters six-way valve 143, by He/CH original in quantitative loop 4interior gas is blown into three-way solenoid valve 113, finally enters and resolves stove supervisor 2210, and is converted into CO in oxidation boiler tube 2212 2and it is quantitative by NDIR detecting device 231.This process maintains 15s, and period blower fan 24 maintenance is opened, and continues cooling to parsing stove 2210; Oxidation furnace 2212 keeps 870 DEG C.
7) cooling procedure: after cooling procedure starts, state and the EC process of each three-way solenoid valve body and mass flow controller are consistent, and six-way valve cuts out; Blower fan 24 maintains to be opened, and continues cooling to parsing boiler tube 2210; Oxidation boiler tube 2212 keeps 870 DEG C.When resolving boiler tube 2210 temperature and being down to below 75 DEG C, instrument stops the analysis phase automatically, preserves data and curve, enters standby, waits pending-analysis of next time sampling.
8) standby: after cooling procedure terminates, instrument enters standby, each valve body and mass flow controller state and purge consistent, namely each carrier gas flux flows to consistent with purge with gas circuit.Blower fan maintains to be opened, and resolve furnace temperature and be set as 10 DEG C, oxidation furnace temperature is down to 500 DEG C.
It should be noted that the object publicizing and implementing example is to help to understand the present invention further, but it will be appreciated by those skilled in the art that: in the spirit and scope not departing from the present invention and claims, various substitutions and modifications are all possible.Therefore, the present invention should not be limited to the content disclosed in embodiment, and the scope that the scope of protection of present invention defines with claims is as the criterion.

Claims (11)

1. a gasoloid carbonaceous components original position online acquisition analyser, comprises carrier gas air-channel system and sampling-analysis air-channel system;
Described carrier gas air-channel system comprises the main gas gas circuit of He, He sweep gas gas circuit, He/O xgas gas circuit and He/CH 4gas gas circuit;
The main gas gas circuit of described He is made up of He gas cylinder gas, the first reduction valve, the first mass flow controller and the first three-way solenoid valve connected successively;
Described He sweep gas gas circuit is made up of the described He gas cylinder gas connected successively, described first reduction valve and the second mass flow controller;
Described He/O xgas gas circuit is by the He/O connected successively xgas cylinder gas, the second reduction valve, the 3rd mass flow controller, the second three-way solenoid valve and the 3rd three-way solenoid valve composition;
Described He/CH 4gas gas circuit is by the He/CH connected successively 4gas cylinder gas, the 3rd reduction valve, the 4th mass flow controller and six-way valve form;
Described first reduction valve is connected with described second mass flow controller with described first mass flow controller by the first three-way connection; Described first mass flow controller is connected with the normal-closed end of described second three-way solenoid valve with the Chang Kaiduan of described first three-way solenoid valve by the second three-way connection; Three mouthfuls of described first three-way solenoid valve normal-closed end and described six-way valve are connected; The Chang Kaiduan of described second three-way solenoid valve is connected with the common port of described 3rd three-way solenoid valve; The common port of described second three-way solenoid valve is connected by with described six-way valve four mouthfuls of the 3rd three-way connection and described 3rd mass flow controller; Two mouthfuls of described six-way valve are connected with five mouthfuls, as the quantitative loop of gas in methane; Six mouthfuls of described six-way valve are set to He/CH 4the emptying end of gas; Described 4th mass flow controller is connected with a bite of described six-way valve;
Described sampling-analysis air-channel system comprises sampling gas circuit, parsing-oxidation furnace and analyzes gas circuit;
Described parsing-oxidation furnace comprises parsing-oxidation boiler tube; Described parsing-oxidation boiler tube comprises resolves stove supervisor, parsing stove looped pipeline and oxidation boiler tube;
Described sampling gas circuit comprise connect successively cutting head, volatile organic compounds remove pipe, ball valve, parsing-oxidation boiler tube, two-way electromagnetic valve, the 5th mass flow controller and sampling pump; In described sampling gas circuit, described VOCs removes pipe and is connected with the primary air inlet of described ball valve; Front end, described ball valve gas outlet arranges a side-inlet, and described ball valve gas outlet is connected with described ball valve side-inlet; The side-inlet of described ball valve is connected with the common port of described first three-way solenoid valve; The gas outlet of described ball valve connects the parsing stove supervisor of described parsing-oxidation boiler tube by the first joint; Described two-way electromagnetic valve primary air inlet rear end arranges a side-inlet, and the primary air inlet of described two-way electromagnetic valve is connected with the side-inlet of described two-way electromagnetic valve; The primary air inlet of described two-way electromagnetic valve is connected with the parsing stove looped pipeline of described parsing-oxidation boiler tube by the second joint; The side-inlet of described two-way electromagnetic valve is connected with described second mass flow controller; The gas outlet of described two-port valve is connected with described 5th mass flow controller;
Described analysis gas circuit comprises the parsing-oxidation boiler tube of the described parsing-oxidation furnace connected successively, the 4th three-way solenoid valve, NDIR (Non-Dispersive Infrared) spectroscopic detector and flowmeter;
Described first joint and the second joint inside arrange a reflects laser corrective system and a transmission laser corrective system; The outlet of described oxidation boiler tube is connected by the common port of the 3rd joint with described 4th three-way solenoid valve; The normal-closed end of described 4th three-way solenoid valve is connected with the normal-closed end of described 3rd three-way solenoid valve; The Chang Kaiduan of described 4th three-way solenoid valve is connected with the inlet end of NDIR (Non-Dispersive Infrared) spectroscopic detector; Described NDIR (Non-Dispersive Infrared) spectroscopic detector endpiece is connected with described flowmeter inlet end; Described flowmeter outlet end is set to the emptying end of tail gas.
2. gasoloid carbonaceous components original position online acquisition analyser as claimed in claim 1, it is characterized in that, in described carrier gas air-channel system and sampling-analysis air-channel system, connect described steel cylinder gas, pipeline that reduction valve, mass flow controller, sampling cutting head, volatile organic compounds remove pipe and ball valve adopts stainless-steel tube or copper pipe; All the other gas circuits adopt stainless-steel tube, copper pipe, silicone rubber tube or polyfluortetraethylene pipe.
3. gasoloid carbonaceous components original position online acquisition analyser as claimed in claim 1, it is characterized in that, described parsing-oxidation boiler tube also comprises the first arm, the second arm and be enclosed within described parsing stove supervisor in sample feeding pipe, the axis of each described pipe fitting is in the same plane; Described parsing-oxidation furnace also comprises shell, electric furnace heating wire and K type thermopair; K type thermopair comprises the first thermometric K type thermopair and the second thermometric K type thermopair; Described parsing-oxidation boiler tube is placed in described shell; The manganese dioxide-catalyst of the pure level of the inner Filling Analysi of center section of described oxidation boiler tube;
Described sample feeding pipe to be responsible for described parsing stove by the 4th joint and to be fixedly connected with; Described parsing stove supervisor and described parsing stove looped pipeline in alignment, and fire a quartzy porous plate in the middle of junction, quartz film is placed in described sample feeding pipe and described quartzy porous plate centre; Described parsing-oxidation boiler tube is at position outer wrap one electric furnace heating wire corresponding to described quartzy porous plate; Described parsing stove supervisor and described parsing stove looped pipeline junction also arrange described oxidation boiler tube and described first arm, be responsible for the linear vertical at place, and both lay respectively at this straight line both sides with described parsing stove; End closure before described first arm, it is inner inserts described first thermometric K type thermopair, and is fixed by the 5th joint, end in contact before described first thermometric K type thermopair top and described first arm; Described second arm is arranged on described oxidation boiler tube center section near described parsing stove supervisor side, and vertical with described oxidation boiler tube, described second arm front end open-ended; Described second thermometric K type thermopair is placed in described oxidation boiler tube outside, and be oxidized furnace tube outer wall described in end in contact before described second thermometric K type thermopair, described oxidation boiler tube is wrapped in another electric furnace heating wire together with described second thermometric K type thermopair; The gas outlet of described second arm is connected with the Chang Kaiduan of described 3rd three-way solenoid valve by the 6th joint.
4. gasoloid carbonaceous components original position online acquisition analyser as claimed in claim 3, it is characterized in that, the shell of described parsing-oxidation furnace is aluminium sheet, be close to described outer casing inner wall and have one layer of heat preservation plate, burner hearth is divided into Resolution Room and oxidizing chamber two parts by a part of described warming plate: described parsing stove supervisor, described parsing stove looped pipeline and described first arm are positioned at described Resolution Room; Described oxidation boiler tube and described second arm are positioned at described oxidizing chamber; Described warming plate adopts mullite material to be processed into; The insulation material of ceramic fiber cotton is filled in described oxidizing chamber inside.
5. gasoloid carbonaceous components original position online acquisition analyser as claimed in claim 4, it is characterized in that, described parsing-oxidation furnace is provided with a blower fan of being sidelong by described parsing stove supervisor side, and the air outlet position of described blower fan corresponds to the quartzy porous plate position in described Resolution Room; Described shell and the corresponding air outlet position of described warming plate are emptied; Described shell upper is provided with a ventilation duct, and described ventilation duct and described shell junction are positioned at directly over described quartzy porous plate, and the position, junction of described shell and ventilation duct corresponding to described warming plate and shell is emptied; Described ventilation duct exit is arranged on the outside of described gasoloid carbonaceous components original position online acquisition analyser.
6. gasoloid carbonaceous components original position online acquisition analyser as claimed in claim 3, it is characterized in that, the operating voltage of described electric furnace heating wire is 220V, power is 1500W, its outer cover has quartz fibre sleeve pipe, and described electric furnace heating wire adoption rate integral calculus carries out computer heating control in conjunction with pulse-width modulation method.
7. gasoloid carbonaceous components original position online acquisition analyser as claimed in claim 3, it is characterized in that, described parsing-oxidation boiler tube each several part is high temperature resistant quartz material, described parsing stove is responsible for as external diameter is 20 millimeters, described parsing stove looped pipeline external diameter is 10 millimeters, described oxidation boiler tube center section external diameter is 13 millimeters, and described first arm and described second arm external diameter are 6.35 millimeters, and described sample feeding pipe external diameter is 16 millimeters.
8. gasoloid carbonaceous components original position online acquisition analyser as claimed in claim 3, it is characterized in that, described quartzy porous plate is an annulus quartz plate being evenly distributed with six small sircle holes, and the internal diameter of described annulus quartz plate is 6 millimeters, external diameter is 17 millimeters, and the diameter of small sircle hole is 2 millimeters; Described quartz film contacts with described quartzy porous plate, and described quartzy porous plate plays the effect of support to described quartz film.
9. gasoloid carbonaceous components original position online acquisition analyser as claimed in claim 1, it is characterized in that, described reflects laser corrective system comprises a generating laser, piezoid, the first optical filter and a reflected laser signals detecting device; Described transmission laser corrective system comprises described generating laser, described piezoid, the second optical filter and transmission laser signal detector; It is inner that described reflects laser corrective system is positioned at described first joint: described first joint arranged outside one is for plugging the generating laser groove of fixing described generating laser, and the center line of described generating laser groove overlaps with the center line of described first joint; Described piezoid encloses sealing by O and is fixed in described generating laser groove, and is close to the placement of described generating laser front end; Described generating laser groove front end also arranges first air drain be communicated with described sample feeding pipe; Described first joint side arranges one perpendicular to the second air drain of described first air drain, is interconnected between described first air drain and described second air drain; One is also arranged for plugging the reflected laser signals detecting device groove of fixing described reflected laser signals detecting device inside described first joint; Described first optical filter encloses sealing by O and is fixed in described reflected laser signals detecting device groove, and is close to the placement of described reflected laser signals detecting device front end; It is inner that described transmission laser corrective system is positioned at described second joint: described second joint arranged outside one is for plugging the transmission laser signal detector groove of fixing described transmission laser signal detector, and its center line overlaps with the center line of described second joint; Described second optical filter encloses sealing by O and is fixed in described transmission laser signal detector groove, and is close to the placement of described transmission laser signal detector front end; Described transmission laser signal detector groove front end also arranges the 3rd air drain be communicated with described looped pipeline; Described second joint side also arranges one perpendicular to the 4th air drain of described 3rd air drain, is interconnected between described 3rd air drain and described 4th air drain.
10. gasoloid carbonaceous components original position online acquisition analyser as claimed in claim 9, is characterized in that, described generating laser adopts that center emission wavelength is 660nm, the point-like red laser transmitter of power to be 50mW and transmission frequency be 1Hz; It is the optical filter of 8nm that described optical filter adopts centre wavelength to be 660nm and bandwidth; Described transmission laser signal detector and reflected laser signals detecting device are the photodiode that can produce highly sensitive linear response to 660nm laser.
The 11. online acquisition analytical approachs utilizing the arbitrary described gasoloid carbonaceous components original position online acquisition analyser of claim 1 ~ 10, comprise sample phase, purge stages, OC analysis phase, EC analysis phase, methane quantitative stage, methane calibration phase, instrument cooling and standby phase successively; Specifically comprise following process:
1) sampling process: gather air sample by sampling gas circuit;
2) the main gas of purge: He, He sweep gas and He/O xcarrier gas is mixed together and purges;
3) OC analytic process: OC is volatilized by progressively Thermal desorption in He gas oxygen-free environment, is converted into CO 2and it is quantitative by NDIR (Non-Dispersive Infrared) spectroscopic detector;
4) EC analytic process: EC is oxidized in an oxidizing environment, is further converted to CO 2and it is quantitative by NDIR (Non-Dispersive Infrared) spectroscopic detector;
5) methane dosing process: inject He/CH in the pipeline of six-way valve 2 mouthfuls and 5 mouthfuls centres 4interior gas; Treat He/CH 4after interior gas is full of, unnecessary He/CH 4interior gas is by 6 mouthfuls of discharges of six-way valve;
6) the main gas of methane calibration process: He and He/O xcarrier gas combination gas is by He/CH original in the pipeline of six-way valve 2 mouthfuls and 5 mouthfuls centres 4interior gas blows out and is oxidized, and is converted into CO 2quantitative by NDIR (Non-Dispersive Infrared) spectroscopic detector;
7) cooling procedure: instrument is lowered the temperature, and automatically stops the analysis phase, preserves data and curve, enters standby;
8) standby: wait pending sampling analysis next time.
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