CN110044663A - Laboratory flames intermediate product sampling system and analysis method - Google Patents
Laboratory flames intermediate product sampling system and analysis method Download PDFInfo
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- CN110044663A CN110044663A CN201910314722.7A CN201910314722A CN110044663A CN 110044663 A CN110044663 A CN 110044663A CN 201910314722 A CN201910314722 A CN 201910314722A CN 110044663 A CN110044663 A CN 110044663A
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- 238000004458 analytical method Methods 0.000 title claims abstract description 47
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/2202—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling
- G01N1/2205—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling with filters
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/24—Suction devices
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/16—Injection
- G01N30/20—Injection using a sampling valve
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/64—Electrical detectors
- G01N30/66—Thermal conductivity detectors
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/16—Injection
- G01N30/20—Injection using a sampling valve
- G01N2030/201—Injection using a sampling valve multiport valves, i.e. having more than two ports
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/16—Injection
- G01N30/20—Injection using a sampling valve
- G01N2030/202—Injection using a sampling valve rotary valves
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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Engineering & Computer Science (AREA)
- Biomedical Technology (AREA)
- Molecular Biology (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
- Sampling And Sample Adjustment (AREA)
Abstract
The invention discloses a kind of laboratory flames intermediate product sampling systems, including gas sample module and on-line analysis module, gas sample module includes burner, microprobe, particulate filter, remove water screen pipe, microprobe installation is mounted on five logical Pneumatic rotary valves by the first reducing adapter, five logical Pneumatic rotary valves and particulate filter, remove water screen pipe, on-line detecting system is sequentially connected by stainless steel tube, the pipeline that water removal screen pipe is connect with on-line detecting system is equipped with first switch valve, the front end of on-line detecting system is connect by the second reducing adapter with stainless steel tube.The present invention also provides a kind of analysis methods based on above-mentioned sampling system, laboratory flames gas sampling system of the present invention and analysis method, the deviation that can reduce existing apparatus provides more accurate, favorable reproducibility flame intermediate product on-line period system and analysis method.
Description
Technical field
The present invention relates to quartz probe on-line period technical fields, and in particular to a kind of laboratory flames intermediate product sampling
System and analysis method.
Background technique
Currently, energy consumption is still based on fossil fuel in the world, and about 85% consumption is fired from fossil according to statistics
The burning of material, burning is along with the presence of more serious pollution and noxious emission problem, especially carbon dioxide, polycyclic aromatic hydrocarbon
With the substances such as soot particulate, therefore, reduce the discharge, research and the application cleaning burning energy of carbon dioxide and pollutant with can
Continuous energy is extremely urgent.
The combustion research of domestic and international many scientific research persons all Efforts To Develops in this respect now, utilizes laboratory flames
Actual combustion condition is imitated, so as to be applied to Actual combustion situation, headed by reducing carbon dioxide and soot particulate
Pollutant emission is generated flame using one-dimensional laminar flow opposed-flow diffusion flames burner, jet flame burner etc., is taken using probe
Sample system and gas analysis and detecting instrument have carried out correlative study analysis to the inter-level and generation product of flame, but still have perhaps
More problems not yet solve, and consult according to pertinent literature and patent, and offline sample detection is taken to analyze in research mostly, offline sample
Acquisition and storage depend on multiple groups quantitative loop and multidigit gas sampling valve, thus allow for the concentration acquisition of multiple sample spots,
Although saving the sample time but having ignored the sample acquired in thermal-flame may be occurred always by the storage mode
Change phenomenon, to keep polycyclic aromatic hydrocarbon quantitative result deviation larger, data are under-represented, and its maintenance requirement and frequency
It is high；There are also a few studies to turn to on-line period analysis mode, and such as application No. is the patents of invention of CN201610445663.3
It discloses and is analyzed using flame real time sample, avoid the leakage maintenance operation of multiple groups quantitative loop, but containing a large amount of in its sampling
Moisture, and moisture has damage to a certain extent to the survey common chromatographic column of hydro carbons, it is serious chromatographic column to be made to fail；Shen
Please number for CN200910057246.1 a kind of on-line chromatograph analysis method of disclosure of the invention, utilize the chromatographic column point of water-tolerant
Bleed reduces moisture from entering system, but still has a degree of harm, because being used for hydro carbons especially non-aromatic hydrocarbon mixture
Isolated capillary chromatographic column is generally very sensitive to water, and water can not only change the polarity of chromatographic column, leads to peak hangover broadening, point
From effect be deteriorated, while also result in column bleed aggravate, chromatographic column lose water-resistance, peak bifurcated, baseline be deteriorated, detection limit mention
A series of problems, such as high, quantitative data repeatability is deteriorated, it is most of can only be by being condensed into gas and liquid two phases post analysis offline；Shen
Number a kind of quartz probe on-line period system please be disclosed for a patent of invention of CN201610577469.0, providing one kind being capable of needle
On-line period is carried out to liquid fuel combustion flame, and can be precisely controlled at different flame locations and carry out real-time online point
The laboratory flames quartz probe on-line period system and sampling method of analysis, but cannot achieve the accurate of each middle hydrocarbons and divide
From inferior separating effect.
Summary of the invention
For above-mentioned there are problem, the purpose of the present invention is to provide a kind of laboratory flames intermediate product sampling system and
Analysis method reduces the deviation of existing apparatus, provides more accurate, favorable reproducibility flame gas on-line period system and analysis
Method.
To achieve the above object, the technical solution adopted by the present invention is that: a kind of laboratory flames intermediate product sampling system,
Including gas sample module and on-line analysis module, it is characterised in that: the gas sample module include burner, microprobe,
Particulate filter, water removal screen pipe, the microprobe are mounted on five logical Pneumatic rotary valves by the first reducing adapter, described
Five logical Pneumatic rotary valves are sequentially connected with particulate filter, water removal screen pipe, on-line detecting system by stainless steel tube, described to remove
The pipeline that water screen pipe is connect with on-line detecting system is equipped with the front end of first switch valve, the on-line detecting system by the
Two reducing adapters are connect with stainless steel tube.
Further, the on-line analysis module include the first quantitative loop, the second quantitative loop, the first sampling valve, second sampling
Valve, switching valve, vacuum pump, analysis instrument, carrier gas bottle, wherein first sampling valve and switching valve are six-way valve,
Second sampling valve is ten-way valve, and first sampling valve, the second sampling valve, switching valve are arranged successively, first sampling
Valve is set along clockwise direction there are six interface A-F, and the second sampling valve is equipped with ten interface G-P, switching along clockwise direction
Valve is set along clockwise direction there are six interface Q-V, and sample is passed through by the interface E of the first sampling valve, first sampling valve and the
It is connected between interface D and O between two sampling valves by stainless steel pipeline, the stainless steel tube road between the interface D and O is set
There is pressure sensor, is connected between interface H and Q and is equipped with by stainless steel pipeline between the second sampling valve and switching valve
Second packed column, the first quantitative loop are connected between F and C, and the second quantitative loop is connected between interface P and N, are equipped between I and L
First packed column, carrier gas bottle are separately connected three road-load gas and are separately connected interface A, J and G, and third packed column, B are equipped between R and S
Linking parsing instrument and between be equipped with the first capillary column, T linking parsing instrument, vacuum pump inlet end connecting interface N, and vacuum
It is equipped with second switch valve and pressure vacuum gauge between pump and switching valve interface N, current limiter is equipped between V and U.
Further, the analysis instrument is gas chromatography mass spectrometer, wherein interface B connection mass detector, interface T connection
Thermal conductivity detector (TCD).
Further, the on-line analysis module further includes computer, heat tape and thermostat, the gas chromatography mass spectrometer
With computer by electrical connection, the heat tape and thermostat, which pass through, to be electrically connected, from microprobe to the second quantitative loop end by
Heat tape winding, and control setting is carried out to its temperature by thermostat.
Further, the bottom end circle valve port of described five logical Pneumatic rotary valves is connected with stainless steel tube, and five ventilation is dynamic
The four additional circle valve port of rotary valve is sequentially connected with the first reducing adapter and microprobe by stainless steel tube respectively, described
The center line of the four additional circle valve port of five logical Pneumatic rotary valves is located in same level, and two adjacent round valves
The center line of mouth is mutually perpendicular to, and external pneumatic is utilized to control to adjust position.
Further, the water removal screen pipe is transparent quartz tube, and there is the filter hole for being covered with uniform ventilation hole at both ends respectively
Plate is equipped with sealed entry at top for loading water removal material and plug for seal, wherein filling water removal material, arrival end filling
Material silica gel particle dry agent is removed water, the water removal material of outlet end filling is molecular sieve desiccant, wherein the silica gel particle choosing
It is the A type spherical silica-gel of 5mm diameter, the molecular sieve desiccant is the 3A molecular sieve that diameter is 5mm, the orifice filter
Aperture≤5mm.
It further, further include fixed mechanism, the fixed mechanism includes cross connecting piece and fixed bracket, and microprobe passes through
Cross connecting piece is fixed on fixed bracket.
It further, further include emission-control equipment, the emission-control equipment is connected to vacuum pump by stainless steel tube
Outlet end, digital flowmeter 22 are mounted between second switch valve 20 and vacuum pump 21.
Further, the probe is vitreous silica microprobe, and surface is coated with polyimide coating.
The present invention also provides a kind of laboratory flames intermediate product sampling and analyzing method, it the following steps are included:
S1. after burner generates stable flame, the tip of microprobe is deeply reached into a certain target position in flame, is passed through
The gaseous sample that vacuum pump extracts target position makes it respectively enter two channels, and one of channel is that sample 1 takes from first
Site E, F of sample valve valve sequentially enter the first quantitative loop, site C, D emptying；Another channel is sample 2 from the second sampling valve 3
Site O, P enter the second quantitative loop, successively arrive site M, N and be vented, to realize in gas sampling valve gas in quantitative loop
The displacement and filling of sample；
S2. after sample fills two quantitative loops, after operation when 0.01min, the first sampling valve and the second sampling valve are clockwise
Rotation switching site, valve 1 is closed when 1min, completes the gas sample introduction movement of the first sampling valve passage, and sample gas starts
It is successively separated by the first capillary column, starts to be analyzed into mass detector, temperature program is set as when operation starts: 60
DEG C keep 8min, 15 DEG C/min is warming up to 100 holding 2min, 15 DEG C/min and is warming up to 150 DEG C of holding 10min, finally with 15 DEG C/
Min, which is warming up to 180 DEG C, to be continued to keep 8min；
Thermal conductivity detector (TCD) negative polarity is opened when S3.1.8min, when 2.8min closes negative polarity；The second sampling is closed when 3min
Valve completes the sample introduction of permanent gas in the second sampling valve passage, while carrier gas 3 carries extra hydrocarbon component by the first filling
Column blowback is vented to exhaust pipe road；Permanent gas component initially enters further separation at this time, H2, O2, N2, CH4, CO according to
It is secondary enter third packed column after, H2 and O2 appearance, and CO2 is not entered also at this time, nebulizer gas pressure is set as 35-40psi；
When S4.3.8min, switches switching valve, so that CO2 is not entered third packed column (molecular sieve column), be directly over out
Site V, U, the T for closing switching valve enter TCD analysis appearance, switching valve are turned off the switch within 6 minutes, so as to avoid third packed column pair
The absorption of CO2 and fail, the CH4 and CO being now in third packed column successively separate continue appearance, in this way by two lead to
Road to the different plant species of same flame gas sample carried out separation and it is qualitative；
S5. after obtaining the chromatogram of each substance appearance, by principal component and the calibrating gas of concentration in flame
Lighter hydrocarbons species and permanent gas species are demarcated in advance, and the area at each peak, peak area response are calculated by work station
Corresponding relationship is established with known target concentration, establishes a calibration curve by multiple points that the calibrating gas of multiple concentration generates,
And then the concentration value of each sample component is obtained by the area response value and calibration curve of sample component.
Compared with prior art, the beneficial effects of the present invention are:
1. real-time monitoring is carried out to the pressure in sampling quantitative loop using pressure sensor, to ensure that each sample volume
Consistency；
2. using particulate filter and removing water screen pipe to carbon soot particles and moisture etc. in sample, avoid to chromatograph
The damage of device；
3. using five logical starting rotary valves, and using vitreous silica microprobe, reduce the replacement number of experiment middle probe,
Ensure to change the reproducibility of probe post-sampling point, while vitreous silica microprobe reduces the interference to flame；
4. can be separated more substances using the setting of the gradient of new analysis method time and temperature, do not weigh
Folded, analyzing various hydro carbons present in flame includes the intermediate products such as isomer and permanent gas, is the combustor of flame
Reason analysis provides more sufficiently reliable foundation.
Detailed description of the invention
Fig. 1 is overall structure diagram of the invention；
Fig. 2 is probe and five logical Pneumatic rotary valve partial structural diagrams of the invention；
Fig. 3 is water removal screen pipe structural schematic diagram of the invention；
Fig. 4 is A-A view in Fig. 3 of the present invention；
Fig. 5 is five logical Pneumatic rotary valve three-dimensional figure of the invention；
Fig. 6 is five logical Pneumatic rotary valve cross-sectional views of the invention；
Fig. 7 is line analysis module sampling valve occupied state structural schematic diagram of the invention；
Fig. 8 is line analysis module sample introduction valve injection status architecture schematic diagram of the invention；
Fig. 9 is line analysis module sampling valve exploded perspective schematic diagram of the invention；
In figure: 1- burner, 101- oxidant end, 102- fuel end, 2- microprobe, the first reducing of 3- adapter, 4- five
The fixed bracket of logical Pneumatic rotary valve, 5- cross connecting piece, 6- particulate filter, 7-, 8- water removal screen pipe, 9- first switch valve,
10- thermostat, the second reducing of 11- adapter, 12- carrier gas bottle, the first quantitative loop of 13-, 14- pressure sensor, 15- second are quantitative
Ring, the first sampling valve of 16-, the second sampling valve of 17-, 18- switching valve, 19- pressure vacuum gauge, 20- second switch valve, 21-
Vacuum pump, 22- digital flowmeter, 23- emission-control equipment, 24- chromatography of gases mass spectrograph, 25- computer, 26- current limiter, 27-
First capillary column, the first packed column of 28-, the second packed column of 29-, 30- third packed column.
Specific embodiment
The present invention provides a kind of laboratory flames intermediate product sampling system and analysis method.The embodiment of the present invention is provided
Technical solution in order to solve the above technical problems, in order to better understand the above technical scheme, below in conjunction with Figure of description
And the above described technique is demenstrated in detail for specific embodiment.
As shown in Figure 1, testing room flame intermediate product sampling system includes gas sample module and on-line analysis module, wherein
Gas sample module include burner 1, microprobe 2, particulate filter 6, water removal screen pipe 8, the microprobe 2 pass through it is first different
Diameter adapter is mounted on five logical Pneumatic rotary valves 4, the five logical Pneumatic rotary valve 4 and particulate filter 6, water removal screen pipe 8,
On-line detecting system is sequentially connected by stainless steel tube, is set on the pipeline that the water removal screen pipe 8 is connect with on-line detecting system
There is the front end of first switch valve 9, the on-line detecting system to connect by the second reducing adapter 11 with stainless steel tube.
As Figure 7-9, on-line analysis module includes the first quantitative loop 13, the second quantitative loop 15, the first sampling valve 16, the
Two sampling valves 17, switching valve 18, vacuum pump 21, analysis instrument, carrier gas bottle 12, wherein first sampling valve 16 and open
Pass switching valve 18 is six-way valve, and the second sampling valve 17 is ten-way valve, and first sampling valve 16, the second sampling valve 17, switch are cut
It changes valve 18 to be arranged successively, first sampling valve 16 is set along clockwise direction there are six interface A-F, and the second sampling valve 17 is along up time
Needle direction is equipped with ten interface G-P, and switching valve 18 is set along clockwise direction there are six interface Q-V, and sample is sampled by first
The interface E of valve 16 is passed through, between first sampling valve 16 and the second sampling valve 17 by stainless steel pipeline be connected to interface D and
Between O, the stainless steel tube road between the interface D and O is equipped with pressure sensor 14, the second sampling valve 17 and switching valve
It is connected between interface H and Q between 18 by stainless steel pipeline and is equipped with the second packed column, the first quantitative loop 13 is connected to F and C
Between, the second quantitative loop 15 is connected between interface P and N, and the first packed column 28 is equipped between I and L, and carrier gas bottle 12 is separately connected
Three road-load gas are separately connected interface A, J and G, are equipped with third packed column 30 between R and S, B linking parsing instrument and between be equipped with the
One capillary column 27, T linking parsing instrument, 21 inlet end connecting interface N of vacuum pump, and vacuum pump 21 connects with switching valve 18
It is equipped with second switch valve 20 and pressure vacuum gauge 19 between mouth N, current limiter 26 is equipped between V and U.In the above-described embodiments, divide
Analyzer device is gas chromatography mass spectrometer 24, wherein interface B connection mass detector, interface T connection thermal conductivity detector (TCD).
In the above-described embodiments, the Capacity Selection 0.25ml of the first quantitative loop, the Capacity Selection 1ml of the second quantitative loop.
Further preferred scheme, on-line analysis module further include computer 25, heat tape and thermostat 10, the gas phase
By electrical connection, the heat tape passes through with thermostat 10 to be electrically connected for chromatographic mass spectrometry instrument 24 and computer 25, from microprobe 2 to the
Two quantitative loops, 15 end is wound by heat tape, and carries out control setting to its temperature by thermostat 10, heat and permanent
The purpose of temperature is that part sample component condenses in pipeline in order to prevent, and sample volume is inconsistent, impact analysis result.
In the above-described embodiments, pressure sensor 14 can be monitored in real time between the first quantitative loop 13 and the second quantitative loop 15
Pressure and its holding situation, are connected with pressure vacuum gauge 19 and second switch valve between the second sampling valve 17 and vacuum pump 21
20, pressure vacuum gauge 19 is used for the pressure of Measuring Vacuum arrival end, then accesses one end of vacuum pump 21, digital flowmeter 22
It is mounted between second switch valve 20 and vacuum pump 21, for judging whether probe tip blocks, determination is digital flowmeter 22
No to need replacing other microprobes 3, emission-control equipment 23 is accessed in 22 outlet end of digital flowmeter, so that sample enters at exhaust gas
Reason device is handled.
As shown in Fig. 2,5,6, further preferred scheme is, the bottom end circle valve port of five logical Pneumatic rotary valves 4 with it is stainless
Steel pipe is connected, the four additional circle valve port of the five logical Pneumatic rotary valve 4 respectively with the first reducing adapter 3 and microprobe
2 are sequentially connected by stainless steel tube, and the center line of the four additional circle valve port of the five logical Pneumatic rotary valve 4 is located at same water
In plane, and the center line of two adjacent round valve ports is mutually perpendicular to, and controls to adjust position using external pneumatic.This is five logical
Gas rotating valve is in order to avoid tissue damage caused by factor accidental in experiment, blocking, and thawing etc. causes in sampling process
Probe replacement process, and then avoid the micron-sized variation of the position in one group of experiment, influence experimental result.Its internal junction
Structure is as shown above, is equipped with 4 valve sites altogether, i.e. once mounting can carry out the rotation replacement of No. four probes, it is made to keep former
Position sampling, when the probe in the site b needs replacing, then valve controls to adjust position using external pneumatic, rotates clockwise valve body
90 °, i.e. the probe in the original site b has been replaced with the probe in the site a now, and such sample position point can keep in situ.
As shown in Figure 3 and Figure 4, further preferred scheme is that water removal screen pipe 8 is on the basis of the above embodiments
There is the orifice filter for being covered with uniform ventilation hole at bright quartz ampoule, both ends respectively, and sealed entry is equipped at top for loading water removal
Material and plug for seal, wherein filling water removal material, the water removal material silica gel particle dry agent of arrival end filling, outlet end filling
Water removal material be molecular sieve desiccant, wherein what the silica gel particle was selected is the A type spherical silica-gel of 5mm diameter, described point
Son sieve desiccant is the 3A molecular sieve that diameter is 5mm, aperture≤5mm of the orifice filter.
In the above-described embodiments, water removal screen pipe 8 is quartz ampoule, and quartz ampoule has the characteristics such as high temperature resistant, inertia, while thoroughly
Whether bright material is convenient for observing its color change and being replaced, wherein the water removal material filled is left side (arrival end) silicon
Glue particle dry agent, right side (outlet end) be molecular sieve desiccant because the water-scavenging capability of molecular sieve is stronger, using the time compared with
It is long, then silica gel is placed on the saturation degree that left side is used to tentatively remove water and indicate water suction, when change colour half when should be replaced, and
Molecular sieve is placed on right side for further removing water.Due to being required to remove the water in flame sample gas in this sampling system
Point, there cannot be suction-operated simultaneously for other hydro carbons and permanent gas, therefore silica gel particle should choose the silica gel in appropriate aperture
Desiccant and molecular sieve desiccant.What the silica gel particle in this system was selected is the A type spherical silica-gel of 5mm diameter, the type silicon
Glue aperture is smaller, and large specific surface area, adsorption rate is very fast, suitable for relative humidity RH be 20-50 when environment.For the ease of gas
Faster by desiccant, then choose the particle of 5mm diameter, therefore the orifice plate of the left end two sides answers≤5mm, this is
System chooses the aperture 4.5mm.Molecular sieve desiccant water absorption is influenced very little by relative humidity, even if when relative humidity is 10%,
There are also very high adsorbance, what this system was selected is 3A molecular sieve, and aperture 3A, the diameter of hydrone is about 2.6A, therefore
It is mainly used for adsorbing water, any molecule of 3A is greater than without diameter in adsorption sample gas, this guarantees other objects
Kind will not be adsorbed.For the ease of consistency, it is also 5mm that molecular sieve, which is chosen, and the orifice plate of water removal drying tube right end outlet is then chosen
The aperture 4.5mm is advisable.When surveying lighter hydrocarbons and permanent gas, then heating sampling line is not had to, therefore then use silica gel and molecular sieve
Combination type removes water mode, and when surveying aromatic component, pipeline, which needs to heat, prevents component from condensing, its general temperature is set as 150 DEG C, silicon
Glue can not high temperature resistant, at this time remove water drying tube left and right sides fill 3A molecular sieve desiccant.Particulate filter 6 may filter that sample
Carbon soot particles in product.
The scheme advanced optimized on the basis of the above embodiments be further include fixed mechanism and emission-control equipment,
Middle fixed mechanism includes cross connecting piece 5 and fixed bracket 7, and microprobe 2 is fixed on fixed bracket 7 by cross connecting piece 5,
Keep stabilization of the microprobe 2 in sampling process.Emission-control equipment is connected to the outlet end of vacuum pump by stainless steel tube, number
Word flowmeter 22 is mounted between second switch valve 20 and vacuum pump 21.Digital flowmeter 22 is for judging whether probe tip blocks up
Plug, it is determined whether need replacing other microprobes 2, access emission-control equipment 23, so that remaining sample enters exhaust-gas treatment dress
It sets and is handled.
The scheme advanced optimized on the basis of the above embodiments is that microprobe is vitreous silica microprobe, and surface is coated with
Polyimide coating, its object is to increase its toughness.
The present invention also provides a kind of laboratory flames intermediate product analysis method, it the following steps are included:
S1. after burner generates stable flame, the tip of microprobe is deeply reached into a certain target position in flame, is passed through
The gaseous sample that vacuum pump extracts target position makes it respectively enter two channels, and one of channel is that sample 1 takes from first
Site E, F of sample valve valve sequentially enter the first quantitative loop, site C, D emptying；Another channel is sample 2 from the second sampling valve 3
Site O, P enter the second quantitative loop, successively arrive site M, N and be vented, to realize in gas sampling valve gas in quantitative loop
The displacement and filling of sample；
S2. after sample fills two quantitative loops, after operation when 0.01min, the first sampling valve and the second sampling valve are clockwise
Rotation switching site, valve 1 is closed when 1min, completes the gas sample introduction movement of the first sampling valve passage, and sample gas starts
It is successively separated by the first capillary column, starts to be analyzed into mass detector, temperature program is set as when operation starts: 60
DEG C keep 8min, 15 DEG C/min is warming up to 100 holding 2min, 15 DEG C/min and is warming up to 150 DEG C of holding 10min, finally with 15 DEG C/
Min, which is warming up to 180 DEG C, to be continued to keep 8min；
Thermal conductivity detector (TCD) negative polarity is opened when S3.1.8min, when 2.8min closes negative polarity；The second sampling is closed when 3min
Valve completes the sample introduction of permanent gas in the second sampling valve passage, while carrier gas 3 carries extra hydrocarbon component by the first filling
Column blowback is vented to exhaust pipe road；Permanent gas component initially enters further separation at this time, H2, O2, N2, CH4, CO according to
It is secondary enter third packed column after, H2 and O2 appearance, and CO2 is not entered also at this time；
When S4.3.8min, switches switching valve, so that CO2 is not entered third packed column (molecular sieve column), be directly over out
Site V, U, the T for closing switching valve enter TCD analysis appearance, switching valve are turned off the switch within 6 minutes, so as to avoid third packed column pair
The absorption of CO2 and fail, the CH4 and CO being now in third packed column successively separate continue appearance, in this way by two lead to
Road to the different plant species of same flame gas sample carried out separation and it is qualitative；
S5. after obtaining the chromatogram of each substance appearance, by principal component and the calibrating gas of concentration in flame
Lighter hydrocarbons species and permanent gas species are demarcated in advance, and the area at each peak, peak area response are calculated by work station
Corresponding relationship is established with known target concentration, establishes a calibration curve by multiple points that the calibrating gas of multiple concentration generates,
And then the concentration value of each sample component is obtained by the area response value and calibration curve of sample component.
In above-mentioned steps S1, the position of burner is first adjusted, one end of vitreous silica microprobe is made to be located at burner
Between oxidant end 101 and fuel end 102, and close to fuel end exit end face center position, fired using digital camera focusing
Burner outlet end center, is finely adjusted vitreous silica microprobe center and upper and lower position, makes vitreous silica microprobe position
In exit end face center point.As shown in fig. 7, being filled out in sample occupied state figure, the first quantitative loop 13 and the second quantitative loop 15
Fill sample, filled in the first quantitative loop 13 and the second quantitative loop 15 switch after sample the first sampling valve 16 and the second sampling valve 16 into
Row rotation switching site, is attached and disconnects with adjacent sites respectively, as shown in figure 8, valve 1 is closed when 1min, complete first
The gas sample introduction movement of valve passage is sampled, sample gas begins to pass through the first capillary column and successively separates, examines into mass spectrum
Device is surveyed to start to be analyzed；When 3.8min, switch switching valve 18, (divides as shown in figure 9, CO2 is made not enter third packed column
Son sieve column), site V, U, the T for being directly over switching valve enter TCD analysis appearance, turn off the switch switching valve within 6 minutes, thus
It avoids third packed column to fail to the absorption of CO2, the CH4 and CO being now in third packed column, which are successively separated, to be continued
Peak, in this way by different plant species of two channels to same flame gas sample carried out separation and it is qualitative.
In above-mentioned steps S2, in order to guarantee efficiently separating for low-carbon the hydrocarbon component (C1-C4) in the first sampling valve passage,
One capillary column flow is set as 1ml, and split ratio 20-40, separating degree and peak shape are preferable, then only needs 50 DEG C of -60 DEG C of guarantors of room temperature
It holds a period of time, after 8min, can separate, for C4 isomer and C4-C7 hydrocarbon component in the column of non-appearance, herein
Can not be completely separable under room temperature, situations such as to avoid the occurrence of overlap peak, then temperature is increased to 100 DEG C with the speed of 15 DEG C/min,
2min is kept, which has separated moieties, for the component after 12.667min, continues to be increased to 150 with 15 DEG C/min
DEG C, 10min is kept, C1-C7 component has disengaged from capillary column separation appearance at this time, only remaining benzene and toluene, because it belongs to virtue
Hydrocarbon, boiling point is higher, separates for this capillary column relatively slowly, in order to save analysis time, then continues with 15 DEG C/min speed
It is warming up to 170-180 DEG C, benzene and toluene can be separated appearance from chromatographic column.For permanent gas component in 3 channel of valve
Separation separates, i.e., 35-60 DEG C holding 12.667min is i.e. separable, carrier gas because it is permanent gas ingredient under room temperature
Pressure and valve event tool there are certain requirements, and nebulizer gas pressure and Vavle switching time are to need to cooperate to can be only achieved test condition, carrier gas
Pressure is set as 35-40psi, and when running 3min, switching valve 3 is then just by other moisture, lighter hydrocarbons and polycyclic aromatic hydrocarbon group
Divide complete blowback to go out, so that subsequent column 3,4 and thermal conductivity detector (TCD) will not be entered, while guaranteeing that target permanent constituents are complete
Into column 3.Because only that a heating post case, then temperature setting combines the component and condition in channel 1 and channel 2, most passes through afterwards
Cross verifying, temperature program is set as: 60 DEG C of holding 8min, 15 DEG C/min are warming up to 100 holding 2min, 15 DEG C/min and are warming up to 150
DEG C keep 10min, finally with 15 DEG C/min be warming up to 180 DEG C continue keep 8min, analysis time is most short and effect is best.
Specific embodiment are as follows:
The position for first adjusting burner, makes one end of vitreous silica microprobe be located at the oxidant end and fuel end of burner
Between, and close to fuel end exit end face center position, using digital camera focusing burner outlet end center, to molten
Fused silica microprobe center and upper and lower position are finely adjusted, and vitreous silica microprobe is made to be located at exit end face center point.
1, calibrating gas is each led into fuel end (permanent gas, lighter hydrocarbons and fuel) and oxidant using flowmeter control
It holds (oxygen), protection gas nitrogen (preventing from the air of surrounding from flowing to cause to disturb to it) is continually fed into around burner annulus,
The gas in combustor cavity can be displaced after 5min completely, so that its outlet end is remained continuously the flowing of calibrating gas, at this time
It is sampled at the 0mm of fuel end face.
2, it opens vacuum pump and carries out gas displacement sampling, it is constant to show that pressure drops to for pressure vacuum gauge about after half a minute
When, second switch valve and vacuum pump are closed, stops vacuumizing, about 3min is waited to show pressure sensor in pipeline and quantitative loop
Pressure be upgraded to initial atmospheric pressure and it is constant when, close first switch valve, then start sample introduction, run point editted in advance
Analysis method is analyzed.
3, the calibrating gas for being continuously passed through 3-5 various concentration is needed in step 2, it is analyzed.
4, after end of run obtains 3-5 group correlation spectrogram, integrating peak areas is carried out to spectrogram, and then obtain different component
The gas of various concentration enters the peak area that instrument measures and maps to standard ingredient concentration, forms the mark of different related coefficients (RF)
Directrix curve (straight line).
5, in experiment condition, fuel end gas is 50%C2H4 and 50%N2, and oxidant end is 20%O2 and 80%N2, point
Do not controlled by flowmeter, then using polyfluortetraethylene pipe access two ports of burner (between the upper and lower away from for 8mm),
It lights a fire in the middle part of two-port, then opens the protection gas of upper and lower port, form it into a stable one-dimensional circular flat fire
Flame.After fire endurance period burning is until stablize, the sampling of first sample point (0mm) is carried out at this time, is opened vacuum pump and is carried out gas
Displacement sampling when pressure vacuum gauge shows that pressure drops to constant about after half a minute, is closed second switch valve and vacuum pump, is stopped
It vacuumizes, waits about 3min that the pressure that pressure sensor is shown in pipeline and quantitative loop is made to be upgraded to initial atmospheric pressure and constant
When, first switch valve is closed, burner is removed, probe is avoided to be under continuous high temperature environment, then starts sample introduction, operation is pre-
The analysis method first editted is analyzed.After the point analysis, sample point is adjusted by the first position and moves up one
Fixed spacing (spacing 0.5mm, totally 17 sample points, settable difference), then repeats above-mentioned sampling and analysis process, until 17
A point sampling is completed.When flame gas sample measures, then need to draw it is accurate under the identical chromatographic condition of standard curve
Sample introduction calculates the content of tested component from curve according to resulting peak area (or peak height).
6, using outer marking quantitative method (ESTD), circular is as follows:
CS=Cr×AS/Ar
Wherein: Cs is sample concentration；
Cr is standard ingredient concentration；
As is sample peak area；
Ar is standard ingredient peak area.
Using above-mentioned calculation formula can by the concentration value and respective peak area opening relationships of sample and calibrating gas, when
Known Cr, As and Ar, the Cs value of you can get it different sample points, i.e. Target Sample Concentrations value.
In above-mentioned implementation process, each parameter setting is as follows:
In above-mentioned parameter setting table, it is the first sampling valve 16 that valve 1 is corresponding, corresponding valve 3 is the second sampling valve 17, valve
2 is corresponding for switching valve 18.
The calibrating gas of 3 groups of various concentrations and one group of sample are measured respectively in above-mentioned experimental procedure.Two
Channel obtains Chromatographic information, finally by integral, data processing, so as to detect hydrocarbon component and permanent gas in flame respectively
Body component obtains qualitative and quantitative result researching and analysing for Soot Formation mechanism.Finally obtained experimental result is as follows:
The relative error magnitudes of calculating are as follows:
Note: "-" indicates that the operating condition flame or the sample position point exist without component.
To sum up, the laboratory flames intermediate product sampling system and analysis method provided through the invention, can will be big absolutely
Some hydrocarbon substance is separated, and the content error very little of each substance finally measured.
Specific embodiments of the present invention are described in detail above, but it is intended only as one such embodiment,
The present invention is not restricted to particular embodiments described above.To those skilled in the art, any couple of present invention carries out
Equivalent modifications and substitution also all among scope of the invention.Therefore, made without departing from the spirit and scope of the invention
Equal transformation and modification, all should be contained within the scope of the invention.
Claims (10)
1. a kind of laboratory flames intermediate product sampling system, including gas sample module and on-line analysis module, feature exist
In: the gas sample module includes burner, microprobe, particulate filter, water removal screen pipe, the microprobe by first
Reducing adapter is mounted on five logical Pneumatic rotary valves, the five logical Pneumatic rotary valve and particulate filter, water removal screen pipe,
Line detection system is sequentially connected by stainless steel tube, and the pipeline that connect with on-line detecting system of water removal screen pipe is equipped with the
One switch valve, the on-line detecting system front end connect with stainless steel tube by the second reducing adapter.
2. a kind of laboratory flames intermediate product sampling system according to claim 1, it is characterised in that: described online point
Analysing module includes the first quantitative loop, the second quantitative loop, the first sampling valve, the second sampling valve, switching valve, vacuum pump, analysis
Instrument, carrier gas bottle, wherein first sampling valve and switching valve are six-way valve, and the second sampling valve is ten-way valve, described the
One sampling valve, the second sampling valve, switching valve are arranged successively, and first sampling valve is set along clockwise direction there are six interface
A-F, the second sampling valve are equipped with ten interface G-P along clockwise direction, and switching valve sets that there are six interfaces along clockwise direction
Q-V, sample are passed through by the interface E of the first sampling valve, pass through stainless steel pipeline between first sampling valve and the second sampling valve
Be connected between interface D and O, stainless steel tube between the interface D and O road is equipped with pressure sensor, the second sampling valve and
The second packed column, the connection of the first quantitative loop are connected between interface H and Q and are equipped between switching valve by stainless steel pipeline
Between F and C, the second quantitative loop is connected between interface P and N, and the first packed column is equipped between I and L, and carrier gas bottle is separately connected
Three road-load gas are separately connected interface A, J and G, between R and S be equipped with third packed column, B linking parsing instrument and between be equipped with first
Capillary column, T linking parsing instrument, vacuum pump inlet end connecting interface N, and set between vacuum pump and switching valve interface N
There are second switch valve and pressure vacuum gauge, current limiter is equipped between V and U.
3. a kind of laboratory flames intermediate product sampling system according to claim 2, it is characterised in that: the analyzer
Device is gas chromatography mass spectrometer, wherein interface B connection mass detector, interface T connection thermal conductivity detector (TCD).
4. a kind of laboratory flames intermediate product sampling system according to claim 3 and analysis method, it is characterised in that:
The on-line analysis module further includes computer, heat tape and thermostat, and the gas chromatography mass spectrometer and computer are by being electrically connected
It connecing, the heat tape passes through with thermostat to be electrically connected, it is wound from microprobe to the second quantitative loop end by heat tape, and
Control setting is carried out to its temperature by thermostat.
5. a kind of laboratory flames intermediate product sampling system according to claim 1, it is characterised in that: five ventilation
The bottom end circle valve port of dynamic rotary valve is connected with stainless steel tube, the four additional circle valve port point of the five logical Pneumatic rotary valve
It is not sequentially connected with the first reducing adapter and microprobe by stainless steel tube, the four additional circle of the five logical Pneumatic rotary valve
The center line of shape valve port is located in same level, and the center line of adjacent two round valve ports is mutually perpendicular to, using outer
Portion's pneumatic control adjusting position.
6. a kind of laboratory flames intermediate product sampling system according to claim 1, it is characterised in that: described to remove water
Chimney filter is transparent quartz tube, and both ends have the orifice filter for being covered with uniform ventilation hole respectively, are used at top equipped with sealed entry
Water removal material and plug for seal are loaded, wherein filling water removal material, the water removal material silica gel particle dry agent of arrival end filling, out
The water removal material of mouth end filling is molecular sieve desiccant, wherein what the silica gel particle was selected is the spherical silicon of A type of 5mm diameter
Glue, the molecular sieve desiccant are the 3A molecular sieve that diameter is 5mm, aperture≤5mm of the orifice filter.
7. a kind of laboratory flames intermediate product sampling system according to claim 1, it is characterised in that: further include fixing
Mechanism, the fixed mechanism include cross connecting piece and fixed bracket, and microprobe is fixed on fixed bracket by cross connecting piece
On.
8. a kind of laboratory flames intermediate product sampling system according to claim 1, it is characterised in that: further include exhaust gas
Processing unit, the emission-control equipment are connected to the outlet end of vacuum pump by stainless steel tube, the vacuum pump outlet end with
Digital flowmeter is equipped between emission-control equipment.
9. a kind of laboratory flames intermediate product sampling system according to claim 1, it is characterised in that: the microprobe
For vitreous silica microprobe, surface is coated with polyimide coating.
10. using the laboratory flames intermediate product analysis method of any one sampling system in claim 1-9, feature exists
In it the following steps are included:
S1. after burner generates stable flame, the tip of microprobe is deeply reached into a certain target position in flame, passes through vacuum
Pumping takes the gaseous sample of target position that it is made to respectively enter two channels, and one of channel is sample 1 from the first sampling valve
Site E, F of valve sequentially enter the first quantitative loop, site C, D emptying；Another channel is sample 2 from the position of the second sampling valve 3
Point O, P enter the second quantitative loop, successively arrive site M, N and are vented, to realize in gas sampling valve gaseous sample in quantitative loop
Displacement and filling；S2. after sample fills two quantitative loops, after operation when 0.01min, the first sampling valve and the second sampling valve are suitable
Hour hands rotation switching site, valve 1 is closed when 1min, completes the gas sample introduction movement of the first sampling valve passage, sample gas
It begins to pass through the first capillary column successively to separate, starts to be analyzed into mass detector, temperature program is set when operation starts
Are as follows: 60 DEG C of holding 8min, 15 DEG C/min are warming up to 100 holding 2min, 15 DEG C/min and are warming up to 150 DEG C of holding 10min, finally with
15 DEG C/min, which is warming up to 180 DEG C, to be continued to keep 8min；
Thermal conductivity detector (TCD) negative polarity is opened when S3.1.8min, when 2.8min closes negative polarity；The second sampling valve is closed when 3min,
The sample introduction of permanent gas in the second sampling valve passage is completed, while carrier gas 3 carries extra hydrocarbon component by the first packed column
Blowback is vented to exhaust pipe road；Permanent gas component initially enters further separation at this time, and H2, O2, N2, CH4, CO are successively
Into after third packed column, H2 and O2 appearance, and CO2 is not entered also at this time, nebulizer gas pressure is set as 35-40psi；
When S4.3.8min, switches switching valve, so that CO2 is not entered third packed column (molecular sieve column), be directly over switch and cut
Site V, U, the T for changing valve enter TCD analysis appearance, switching valve are turned off the switch within 6 minutes, so as to avoid third packed column to CO2
Absorption and fail, the CH4 and CO being now in third packed column, which are successively separated, continues appearance, in this way by two channels pair
The different plant species of same flame gas sample carried out separation and it is qualitative；
S5. after obtaining the chromatogram of each substance appearance, by principal component and the calibrating gas of concentration to the lighter hydrocarbons in flame
Species and permanent gas species are demarcated in advance, calculate the area at each peak by work station, peak area response with
Know that aimed concn establishes corresponding relationship, establishes a calibration curve by multiple points that the calibrating gas of multiple concentration generates, in turn
The concentration value of each sample component is obtained by the area response value and calibration curve of sample component.
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| CN112461607A (en) * | 2020-11-12 | 2021-03-09 | 南京理工大学 | Opposite-impact diffusion flame soot particle sampling device and sampling method thereof |
| CN113433259A (en) * | 2021-05-20 | 2021-09-24 | 东南大学 | Method and device for collecting and testing stable combustion intermediate products |
| CN113588861A (en) * | 2020-04-30 | 2021-11-02 | 南京理工大学 | Method for researching and regulating generation mechanism of combustion soot of aviation alternative fuel |
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