CN101329228B - A peroxyacyl nitrate lipid sample injection system and detection method - Google Patents
A peroxyacyl nitrate lipid sample injection system and detection method Download PDFInfo
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- CN101329228B CN101329228B CN2008101173341A CN200810117334A CN101329228B CN 101329228 B CN101329228 B CN 101329228B CN 2008101173341 A CN2008101173341 A CN 2008101173341A CN 200810117334 A CN200810117334 A CN 200810117334A CN 101329228 B CN101329228 B CN 101329228B
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- -1 nitrate lipid Chemical class 0.000 title description 26
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Abstract
本发明涉及一种过氧酰基硝酸酯类物质进样系统及检测方法，包括：进样气路，用于输送空气样本；降解回路，用于热解去除空气样本中的过氧酰基硝酸酯类物质，降解后得到零空气；标气生成单元，用于将零空气与不同量的过氧酰基硝酸酯类物质混合，得到不同浓度的标气；检测单元，用于采集零空气、标气和空气样本的数据，得到空气样本中过氧酰基硝酸酯类物质的浓度，该检测方法通过时序控制，在同一个系统中在不使用零空气的情况下利用空气样本进行在线标定，根据标定的数据自动实现空气样本检测。本发明实现了系统进样程序和标定程序的整合，操作方便。
The invention relates to a peroxyacyl nitrate substance sampling system and a detection method, comprising: a sampling gas path for transporting air samples; a degradation circuit for pyrolyzing and removing peroxyacyl nitrates in air samples The substance is degraded to obtain zero air; the standard gas generation unit is used to mix zero air with different amounts of peroxyacyl nitrates to obtain different concentrations of standard gas; the detection unit is used to collect zero air, standard gas and The data of the air sample is used to obtain the concentration of peroxyacyl nitrates in the air sample. The detection method is controlled by time sequence, and the air sample is used for online calibration in the same system without using zero air. According to the calibration data Automated air sample testing. The invention realizes the integration of the system sampling program and the calibration program, and is easy to operate.
Description
Technical field
The present invention relates to the environmental quality monitoring field, be specifically related to a kind of peroxyacetyl nitrates class material sampling system and detection method.
Background technology
Peroxyacetyl nitrates class material (RC (O) OONO
2PANs) (comprise acetylperoxide nitrate (peroxyacetyl nitrate, PAN)) be the important products that atmospheric photochemistry is polluted, but at present, China is very few to the study on monitoring of peroxyacetyl nitrates class Substance P ANs, reason is to have difficulties on its monitoring technology: the PANs material concentration in the atmosphere is lower, from minimum several ppt to the highest tens ppb; And its decomposition easily of being heated, can not be long time stored under the room temperature, these have all brought difficulty to detection.Though can be by sample introduction after the liquid nitrogen condensation enrichment, complicated operation can't continuous monitoring, the particularly research and development of on-line monitoring instrument be in space state.Along with China's urban automobile quantity increases day by day, photochemical pollution is serious day by day, and is extremely important as the monitoring of the PANs of atmospheric oxidant important indicator.Therefore, press for a kind of can be online the sampling system and the detection method of detection PANs content.
Summary of the invention
The purpose of this invention is to provide a kind of peroxyacetyl nitrates class material sampling system and detection method; under the situation that need not introduce zero air (air that does not promptly contain PANs gas); can be according to the size that enters PANs flow in zero air; dilution obtains the gas of variable concentrations; thereby finish the on-line proving process, the result of the air sample gathered and demarcation is detected automatically the content of peroxyacetyl nitrates class material in the air sample.
For achieving the above object, the present invention adopts following technical scheme:
A kind of peroxyacetyl nitrates class material sampling system is provided, and this system comprises: the sample introduction gas circuit is used to carry air sample; The degraded loop is used for the peroxyacetyl nitrates class material that air sample is removed in pyrolysis, obtains zero air after the degraded; The gas generation unit is used for zero air is mixed with the peroxyacetyl nitrates class material of different amounts, obtains the gas of variable concentrations; Detecting unit is used to gather the data of zero air, gas and air sample, obtains the concentration of peroxyacetyl nitrates class material in the air sample.
Wherein, be connected with sampling valve and zero air valve in the described sample introduction gas circuit, described gas generation unit is made up of peroxyacetyl nitrates class material input block and calibrate valve, described sampling valve, zero air valve and calibrate valve are three-way solenoid valve, air sample is entered by the common port of sampling valve, the normal-closed end of described sampling valve is connected with degraded loop input end, and the Chang Kaiduan of described sampling valve is connected with the Chang Kaiduan of zero air valve; The normal-closed end of described zero air valve is connected with the output terminal in described degraded loop, and the common port of described zero air valve is connected with the normal-closed end of described calibrate valve; The common port of described calibrate valve is connected with peroxyacetyl nitrates class material input block; The common port of described zero air valve is connected with described detecting unit with the normal-closed end of described calibrate valve simultaneously.
Wherein, described detecting unit comprises chromatographic column and electron capture detector, the common port of described zero air valve and the normal-closed end of described calibrate valve insert one of them port of six-way injection valve simultaneously, one of them port of described six-way injection valve connects helium tube, one of them port connects vacuum pump, one of them port connects chromatographic column, and described six-way injection valve connects described control module, connects the switching that realizes that gas load and gas inject described chromatographic column by the inside that changes six go side mouths.
Wherein, before a port of described six-way injection valve is inserting described chromatographic column, also be connected with mass flow controller, be used to control the gas flow rate that enters chromatographic column.
Wherein, peroxyacetyl nitrates class material input block is a peroxyacetyl nitrates class light, and described peroxyacetyl nitrates class light is connected with pick-up unit, is used to detect the peroxyacetyl nitrates class mass flow-rate of generation.
Wherein, the common port of described zero air valve is connected with pick-up unit at the normal-closed end with calibrate valve, is used to detect the flow from zero air valve normal-closed end eluting gas.
Wherein, described degraded loop comprises: pipeline, be connected with the normal-closed end of sample introduction, and be used for admission of air sample and outwards conveying; The heating tape is wrapped on the described pipeline, is used for described pipeline heating; Temperature sensor is used to measure temperature in the described pipeline; Temperature controller is connected with temperature sensor, heating tape, is used for controlling according to temperature in the pipeline of measuring the temperature of described heating tape.
Wherein, described temperature controller is controlled the temperature of described heating tape, makes the interior temperature of described pipeline reach 125 ℃.
The present invention also provides a kind of peroxyacetyl nitrates class material detection method of above-mentioned sampling system, and the method comprising the steps of: input air sample in the sample introduction gas circuit; Utilize the peroxyacetyl nitrates class material in the degraded loop pyrolysis removal air sample, the zero air that obtains after the degraded is input to described detecting unit carries out data acquisition; Utilize the gas generation unit that zero air is mixed with the peroxyacetyl nitrates class material of different amounts, obtain the gas of variable concentrations and output to detecting unit carrying out data acquisition; Air sample to be measured is input to described detecting unit carries out data acquisition, described detecting unit obtains the concentration of peroxyacetyl nitrates class material in the air sample according to the data of zero air, gas and the air sample gathered.
The present invention also provides the peroxyacetyl nitrates class material detection method of the above-mentioned sampling system of another kind of use, the method comprising the steps of: the Chang Kaiduan of described sampling valve, the Chang Kaiduan of described zero air valve, the normal-closed end of described calibrate valve are closed, the normal-closed end of described sampling valve, the normal-closed end of described zero air valve, the Chang Kaiduan of described calibrate valve are opened; Continue to set the very first time, described detecting unit obtains zero air data; The normal-closed end of described calibrate valve is opened, the Chang Kaiduan of described calibrate valve is closed; Continue second time of setting, described detecting unit obtains the gas data; The Chang Kaiduan of described sampling valve, the Chang Kaiduan of described zero air valve and the Chang Kaiduan of described calibrate valve are opened, simultaneously the normal-closed end of described sampling valve, the normal-closed end of described zero air valve and the normal-closed end of calibrate valve are closed; Continue the 3rd time of setting, described detecting unit obtains the air sample data; According to the data of the zero air, gas and the air sample that obtain, obtain the concentration of peroxyacetyl nitrates class material in the air sample.
Utilize technical scheme of the present invention, have following beneficial effect:
1) utilizes existing three-way solenoid valve product autonomous Design time series control program;
2) can be by the control three-way solenoid valve, the switching of realization system between " sampling pattern ", " null mode " and " calibration mode " realized the integration of system's sample introduction program and calibrating procedure, and be easy to operate;
3) sampling control system comprises the degraded loop of autonomous Design, can be with the pyrolysis of airborne PANs material, thus under the situation that need not introduce zero air (air that does not promptly contain PANs gas), utilize air sample and PAN gas generation system to finish on-line proving;
4) realize the omnidistance on-line automatic control of computing machine, adjustment sampling time.
Description of drawings
Fig. 1 is a peroxyacetyl nitrates class material sampling system composition frame chart of the present invention;
Fig. 2 is a peroxyacetyl nitrates class material sampling system schematic diagram among the embodiment;
Fig. 3 is the synoptic diagram of the six-way injection valve among the embodiment;
Inner connection layout when Fig. 4 is in the gas load state for six-way injection valve among the embodiment;
Inner connection layout when Fig. 5 injects state for six-way injection valve among the embodiment is in gas;
Fig. 6 is the flow process that the switching of six-way injection valve among the embodiment realizes gas sampling;
Fig. 7 is a pyrolysis loop circuit synoptic diagram among the embodiment.
Among the figure: 1, stainless steel pipeline; 2, heating tape; 3, temperature sensor; 4, vacuum pump; 5, carrier gas He; 6, chromatographic column.
Embodiment
Peroxyacetyl nitrates class material sampling system and detection method that the present invention proposes are described as follows in conjunction with the accompanying drawings and embodiments.
Embodiment
Peroxyacetyl nitrates class material sampling system composition diagram as shown in Figure 2; be used for carrying the sample introduction gas circuit of air sample to be connected with sampling valve and zero air valve in the present embodiment; the gas generation unit is made up of PANs input block and calibrate valve; sampling valve, zero air valve and calibrate valve are three-way solenoid valve, and air sample is by the common port COM of sampling valve
1Enter the normal-closed end NC of sampling valve
1Be connected the Chang Kaiduan NO of sampling valve with degraded loop input end
1Chang Kaiduan NO with zero air valve
2Connect; The normal-closed end NC of zero air valve
2Be connected the common port COM of zero air valve with the output terminal in degraded loop
2Normal-closed end NC with calibrate valve
3Connect; The common port COM of calibrate valve
3Be connected with the PANs input block; The common port COM of zero air valve
2Normal-closed end NC with calibrate valve
3Be connected with detecting unit simultaneously.
The PANs input block is the PANs light source in the present embodiment, and detecting unit comprises interconnective chromatographic column 6 and electron capture detector ECD, the common port COM of zero air valve
2Normal-closed end NC with calibrate valve
3Insert a port of six-way injection valve simultaneously, a port of six-way injection valve connects helium tube, a port connects chromatographic column 6, a port connects vacuum pump 4, six-way injection valve connects control module, connects the switching that realizes that gas load and gas inject described chromatographic column 6 by the inside that changes six go side mouths.
Be illustrated in figure 3 as the synoptic diagram of six-way injection valve, the function of six-way injection valve is the auto injection of realization system, and its automatic switchover sample introduction is realized by sampling routine control, is commercially available six-way injection valve among the figure.Six interfaces of six-way injection valve (abbreviation six-way valve) portion within it link to each other in twos.Adopt four interfaces in the present embodiment, connected the common port COM of zero air valve
2Normal-closed end NC with calibrate valve
3One of them interface realize entering of sample gas, the interface of the interface of connection helium tube, connection vacuum pump provides power for sample introduction, the port that connects chromatographic column 6 is used to carry sample gas to carry out the chromatogram detection to chromatographic column 6, is sent to electron capture detector ECD then after chromatogram detects and detects.
Six-way injection valve has two states, a kind of is gas load " LOAD " state, a kind ofly be that gas injects " INJECT " state, as shown in Figure 4, six-way injection valve is " LOAD " state at ordinary times, by changing inner the connection, the sample gas that enters six-way injection valve is provided at vacuum pump 4 under the effect of power, with COM
2, NC
3The interface and the interface pipeline that is connected with vacuum pump that connect, be called quantity tube in the present embodiment, by " LOAD " state, in quantity tube, load sample introduction gas, when needing sampling, switched to " INJECT " state as shown in Figure 5, the handoff procedure inner connection of six-way injection valve for a change, make an end of above-mentioned quantity tube connect carrier gas He gas 5, the other end inserts chromatographic column 6, and carrier gas He gas 5 just is blown into the sample gas in the quantity tube in the chromatographic column 6 like this; Sample introduction finishes back (after 10 seconds), and six-way injection valve is got back to " LOAD " state once more.
When analyzing a sample, remaining air no longer flows into chromatographic column GC, and direct outflow system.As Fig. 2, the pipeline that comes out from sampling valve, calibrate valve or zero air valve was divided into two-way before entering chromatographic column, and one the tunnel directly inserts chromatographic column, is called the sampling gas circuit in the present embodiment, uses when sampling; Another road is by inserting chromatographic column 6 behind mass flow controller MFC2, the MFC1, the pipeline that meets MFC2 also inserts vacuum pump and is communicated with the outside then, and present embodiment is called the primary air gas circuit, uses when analytic sample.The pipeline that will enter chromatographic column in the present embodiment is called the sampling gas circuit, is called the primary air gas circuit with flowing out to outside gas circuit.Gas sampling and air sample adopt and use different pipelines, air sample to adopt use directly to enter the sampling gas circuit of chromatographic column, and the sample pipeline of described use of gas is the pipeline that MFC1 flows through MFC2 earlier, and then flows through the pipeline of MFC1.Can the service property (quality) flow controller flow velocity of control gas sample gas so that zero gas and PANs fully mix, another MFC2 controls the flow velocity of primary air gas circuit when the systematic analysis sample.
When sampling shown in Figure 6 six-way injection valve control procedure, at first set each parameter, the flow velocity of the sample gas that need control as mass flow controller, and sample introduction (INJECT) and after analysis time, click " beginning "; Six-way injection valve is inner to be connected by changing, and makes it be in " LOAD " state, and sample gas enters in the quantity tube (the sample gas here can zero air, gas and air sample); Behind the sample introduction setting-up time, switch back, setting-up time is 10s in the present embodiment, switches back to make to refer to that six-way injection valve is inner to be connected by changing, and makes it be in " INJECT " state; Behind the 5min, switch to " LOAD " state once more.More than switch and make it be in " INJECT " state, gas is blown into chromatographic column 6, triggered chromatographic column GC, carry out data acquisition and record, behind the 4.3min, stop after having gathered data, after the time that is in " INJECT " state is 5min by carrier gas He; Switch to " LOAD " state then, behind the 5min, switch to " INJECT " state once more.Therefore, present embodiment is when 5 minutes integral multiple, and six-way injection valve switches.
Be illustrated in figure 7 as the degraded loop circuit figure in the present embodiment, the degraded loop is between sampling valve and zero air valve, is the pipeline that air is converted into zero gas.Its principle is to utilize 125 ℃ high temperature, and the thermal decomposition of airborne PANs material is dispeled.This degraded loop comprises: stainless steel pipeline 1 is used for admission of air sample and outwards conveying; Heating tape 2 is wrapped on the pipeline 1, is used for pipeline 1 heating; Pt100 temperature sensor 3 is bonded on the Stainless Steel pipe by heat conductive silica gel, is used to measure temperature in the described pipeline; Temperature controller is connected with temperature sensor, heating tape, is used for the temperature according to temperature control heating tape in the pipeline of measuring.Used stainless-steel tube external diameter 6mm in the present embodiment, long 2m coils into 4 circles and is contained in the incubation chamber, makes inner air tube reach 125 ℃, and pyrolysis all will take place in the PANs material under this temperature more than 99%.
Sampling routine is by Visual Basic language compilation in the present embodiment, (data collecting card transforms by A/D, D/A and I/O control by the control data capture card, the switching of the flow velocity of control of quality flowmeter and three solenoid valves) and the trigger gas chromatography, realize the automatic sampling of system, demarcate and data recording automatically.
Data collecting card is precious wound source, Beijing Science and Technology Ltd. and produces.Wherein, model is that the data collecting card of BC431 carries out the DA conversion, realizes the flow speed control to mass flowmeter; Model is that the data collecting card of BC411L carries out AD and transforms, and the flow velocity of mass flowmeter is fed back to computer, is presented on the interface, and BC411L can also control I/O and transforms simultaneously, realizes the automatic switchover of six-way injection valve and three solenoid valves.The sampling interface is (being that whole control process can realize by this data collecting card) as shown in the figure.
Control module is by three solenoid valves of control in the present embodiment, according to different signal inputs, finish the opening/closing action of different gas circuits, realize the switching of instrument between " sampling pattern ", " null mode " and " calibration mode ", realize that PANs concentration detects in the air sample, details are as follows for concrete control procedure.
(1) sampling pattern
Sampling valve: Chang Kaiduan NO
1Open normal-closed end NC
1Close;
Zero air valve: Chang Kaiduan NO
2Open normal-closed end NC
2Close;
Calibrate valve: Chang Kaiduan NO
3Open normal-closed end NC
3Close.
Air sample enters after the system at first by entering the common port COM of sampling valve
1, by " the Chang Kaiduan NO of sampling valve
1Enter zero air valve, by the common port COM of zero air valve
2Enter detecting unit, enter chromatographic column 6 by above-mentioned switching to six-way injection valve and carry out data acquisition, chromatographic column 6 is the core components in the gas chromatography detector, and it act as the material that air is different and separates, separation detection is carried out in convenient further detection.Gas chromatograph is the GC-2010 gas chromatograph that Tianjin, island company produces in the present embodiment.
(2) null mode
Sampling valve: Chang Kaiduan NO
1Close normal-closed end NC
1Open;
Zero air valve: Chang Kaiduan NO
2Close normal-closed end NC
2Open;
Calibrate valve: Chang Kaiduan NO
3Open normal-closed end NC
3Close.
Air sample enters the common port COM that at first enters sampling valve after the system
1, by the normal-closed end NC of sampling valve
1Enter the degraded loop, the PANs in the air sample is removed by pyrolysis, enters the normal-closed end NC of zero air valve then
2, by the common port COM of zero air valve
2Enter detecting unit, enter chromatographic column 6 by above-mentioned switching and carry out data acquisition six-way injection valve.
(3) calibration mode
Sampling valve: Chang Kaiduan NO
1Close normal-closed end NC
1Open;
Zero air valve: Chang Kaiduan NO
2Close normal-closed end NC
2Open;
Calibrate valve: Chang Kaiduan NO
3Close normal-closed end NC
3Open.
Air sample enters the common port COM that at first enters sampling valve after the system
1, by the normal-closed end NC of sampling valve
1Enter the degraded loop, the PANs in the air sample is removed by pyrolysis, enters the normal-closed end NC of zero air valve then
2, by the common port COM of zero air valve
2Normal-closed end NC with calibrate valve
3The PANs gas of discharging mixes, PANs gas is to be produced by the PANs light source in the present embodiment, can utilize existing detecting device to detect the flow that produces PANs gas, detect from the flow of the zero air of zero air valve outflow by detecting device simultaneously, can obtain variable concentrations like this and get PANs calibrating gas (abbreviation gas), the composition that is mixing air in the PANs calibrating gas, as oxygen and nitrogen, also mixing a spot of acetone gas and NO gas, the concentration of PANs also is very low in the PANs calibrating gas, is about 1ppm, but this concentration can obtain by aforementioned calculation, mark enters chromatographic column 6 by above-mentioned switching to six-way injection valve and carries out data acquisition with entering detecting unit.
By the switching between " sampling pattern ", " null mode " and " calibration mode ", air to be measured, zero air and PAN gas are fed detecting unit chromatographic column 6 in the top process, enter electron capture detector (ECD) then and measure.If the sampled data of known zero air, the sampled data of gas and corresponding PANs concentration, can set up the relation of PANs concentration and character pair, then air sample data and the above-mentioned relation of gathering contrasted, the PANs concentration that can obtain air sample detects, the testing process that obtains behind zero air, gas and the air sample is a prior art, no longer describes in detail here.
Degraded loop in the present embodiment utilizes the PAN pyrolysis in the air sample, can think no longer to contain the PANs material in the air sample of sample introduction, obtains zero air.Thereby under the situation that does not need additionally to provide zero air, utilize air sample and PANs gas to finish on-line proving to instrument.
Above embodiment only is used to illustrate the present invention; and be not limitation of the present invention; the those of ordinary skill in relevant technologies field; under the situation that does not break away from the spirit and scope of the present invention; can also make various variations and modification; therefore all technical schemes that are equal to also belong to category of the present invention, and scope of patent protection of the present invention should be defined by the claims.
Claims (8)
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| CN2008101173341A CN101329228B (en) | 2008-07-29 | 2008-07-29 | A peroxyacyl nitrate lipid sample injection system and detection method |
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|---|---|---|---|
| CN2008101173341A CN101329228B (en) | 2008-07-29 | 2008-07-29 | A peroxyacyl nitrate lipid sample injection system and detection method |
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| Publication Number | Publication Date |
|---|---|
| CN101329228A CN101329228A (en) | 2008-12-24 |
| CN101329228B true CN101329228B (en) | 2010-09-15 |
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| CN101561422B (en) * | 2009-04-30 | 2012-10-03 | 北京大学 | On-line monitoring system for concentration of acetylperoxide nitrate |
| CN102507761B (en) * | 2011-10-17 | 2014-04-30 | 中国科学院大气物理研究所 | System and method for measuring nitric oxide in a small amount of gas |
| CN104267198B (en) * | 2014-07-22 | 2016-05-18 | 武汉市天虹仪表有限责任公司 | A kind of automatic calibration equipment for volatile organic matter analyzer and method |
| CN105716932B (en) * | 2014-12-02 | 2020-10-27 | 中国辐射防护研究院 | Dilution gas path control method and device for high-concentration gas measurement |
| CN105067596B (en) * | 2015-07-23 | 2018-04-13 | 山东省科学院海洋仪器仪表研究所 | Ozone-detecting element and detection method |
| CN105136934A (en) * | 2015-09-16 | 2015-12-09 | 中国科学院生态环境研究中心 | Online gas chromatographic analysis and calibration system for PANs and CC14 in atmosphere |
| CN111060589A (en) * | 2020-01-10 | 2020-04-24 | 湖北锐意自控系统有限公司 | System and method for measuring concentration of anesthetic gas |
| CN112946122A (en) * | 2021-01-28 | 2021-06-11 | 中国科学院生态环境研究中心 | Method for detecting nitrogen oxide in high-purity gas |
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