CN219496275U - Environment-friendly on-line monitoring and sampling equipment for organic matters in waste gas with fixed pollution sources - Google Patents
Environment-friendly on-line monitoring and sampling equipment for organic matters in waste gas with fixed pollution sources Download PDFInfo
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- CN219496275U CN219496275U CN202320238167.6U CN202320238167U CN219496275U CN 219496275 U CN219496275 U CN 219496275U CN 202320238167 U CN202320238167 U CN 202320238167U CN 219496275 U CN219496275 U CN 219496275U
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Abstract
The utility model relates to the technical field of on-line monitoring and sampling equipment, and particularly discloses environment-friendly on-line monitoring and sampling equipment for organic matters in waste gas with a fixed pollution source. The utility model can collect cold and hot flue gas and gas with larger humidity, and ensure the effective representativeness of the sample; the accumulated ash and residues of the pipeline are conveniently cleaned; the device is provided with a gas sampling flow path and a measuring flow path, so that the sampling of the sampling adsorption tube and the sampling bag and the on-line monitoring of organic matters in the waste gas can be realized respectively; the device detector can be calibrated and calibrated in time, the data quality is ensured, and the detection of the hydrogen flame ionization detector of most organic matters and the detection of the electron capture detector of the electric polar compounds such as the heteroatom compounds such as N, O, S and the halohydrocarbon can be respectively realized through the selective and applicable detection of the hydrogen flame ionization detector and the electron capture detector.
Description
Technical Field
The utility model relates to the technical field of on-line monitoring and sampling equipment, and particularly discloses environment-friendly on-line monitoring and sampling equipment for organic matters in waste gas with a fixed pollution source.
Background
With the development of economy and the expansion of the production scale of chemical enterprises, the emission of various organic matters is also increasing year by year. The components of organic matters in the exhaust gas discharged by different industries are complex, and the sampling difficulty is increased due to the characteristics of high temperature, high humidity and the like of the exhaust gas discharge. The on-line monitoring and sampling equipment is provided, so that workers can conveniently master the emission conditions of organic matters of different enterprises, and the monitoring and treatment of the organic matters in the exhaust of the fixed pollution sources are enhanced.
The current main stream organic matter monitoring equipment on the market cannot simultaneously display various parameters of the flue gas at one time, and when the temperature of the flue gas is too high or the humidity is too high, the problems that samples cannot be collected or residual liquid in a sampling flow path is easy to cause sample pollution and sample collection and analysis representative distortion are lacked exist; after the equipment is used for a long time, the problems of dust accumulation and difficult residual cleaning exist. Most of the devices in the market also have the problems that the functions are single, the sampling and analyzing functions cannot be realized at the same time, and the quality of the monitored data cannot be perfectly guaranteed due to the lack of the calibration function. In addition, most of the devices on the market at present can only measure a few organic matters with simple structures, cannot separately measure complex compounds containing N, O, S and other heteroatoms and electrode compounds such as halogenated hydrocarbons, and cannot meet the current monitoring requirements of a plurality of organic matters with various numbers.
Disclosure of Invention
Aiming at the defects in the prior art, the utility model provides the environment-friendly on-line monitoring and sampling equipment for the organic matters in the exhaust gas of the fixed pollution source, which can display parameters such as the temperature, the pressure, the flow rate, the humidity and the like of the exhaust gas of the fixed pollution source in real time; the cold and hot flue gas and the gas with larger humidity can be collected, so that the effective representativeness of the sample is ensured; the accumulated ash and residues of the pipeline are conveniently cleaned; the device is provided with a gas sampling flow path and a measuring flow path, and can respectively realize the sampling of the sampling adsorption tube and the sampling bag and the on-line monitoring of organic matters in the waste gas. In addition, the device can calibrate and calibrate the equipment detector in time to ensure the data quality, and can realize FID detection of most organic matters and ECD detection of heteroatom compounds containing N, O, S and electric polar compounds such as halohydrocarbon through selective application detection of a hydrogen Flame Ionization Detector (FID) and an Electron Capture Detector (ECD) respectively.
The technical scheme adopted for solving the technical problems is as follows:
the utility model relates to an environment-friendly on-line monitoring and sampling device for organic matters in fixed pollution source waste gas, which comprises a gas sampling flow path, a measuring flow path, a sampling head back-blowing flow path and a calibration flow path.
The gas sampling flow path comprises a sampling head, a semiconductor refrigerator, an electric ball valve, a traction pump, a first mass flowmeter, a four-way ball valve, a third three-way ball valve, a second ball valve, a third ball valve, a sampling adsorption tube and a gas collecting bag, wherein the sampling head is connected with the semiconductor refrigerator through a sampling pipeline, the semiconductor refrigerator is sequentially connected with the electric ball valve, the traction pump, the first mass flowmeter, the four-way ball valve and the third three-way ball valve through a heat tracing sampling tube, the third three-way ball valve is respectively connected with the second ball valve and the third ball valve through the heat tracing sampling tube, the second ball valve is connected with the sampling adsorption tube, and the third ball valve is connected with the gas collecting bag;
the measuring flow path comprises a sampling head, a semiconductor refrigerator, an electric ball valve, a traction pump, a first mass flowmeter, a four-way ball valve, a sample quantitative ring, a vent valve, a third three-way ball valve, a first ball valve, an electric heating box and a fourth three-way ball valve which are sequentially connected, wherein the fourth three-way ball valve is connected with two paths of parallel gas paths; one path of parallel gas path is that a fourth three-way ball valve is sequentially connected with a first sample inlet, a first glass liner tube, a first column temperature box, a hydrogen flame ionization detector, a first photomultiplier and a computer, and the other path of parallel gas path is that the fourth three-way ball valve is sequentially connected with a second sample inlet, a second glass liner tube, a second column temperature box, an electron capture detector, a second photomultiplier and a computer. The sample quantifying ring is connected with the vent valve, the third three-way ball valve, the first ball valve, the electric heating box and the pipeline between the fourth three-way ball valve and the first and second sample inlets through the heat tracing sampling pipe.
The sampling head blowback flow path comprises a high-purity nitrogen bottle, a first pressure reducing valve, a first pressure gauge, a first three-way ball valve and a sampling head which are connected in sequence.
The calibration flow path comprises a calibration gas cylinder, a second pressure reducing valve, a second pressure gauge, a second three-way ball valve, a second mass flowmeter, a four-way ball valve, a sample quantitative ring, a vent valve, a third three-way ball valve, a first ball valve, an electric heating box and a fourth three-way ball valve which are sequentially connected, wherein the fourth three-way ball valve is connected with two paths of parallel gas paths; the two parallel gas paths are the same as the two parallel gas paths in the measuring flow path; the calibration flow path further comprises a high-purity nitrogen cylinder, a first pressure reducing valve, a first pressure gauge and a first three-way ball valve which are sequentially connected, and the first three-way ball valve is further connected with a second three-way ball valve.
The sampling head is externally covered with a heating belt, the heating belt is connected with a first temperature sensor, the heating belt and the first temperature sensor are simultaneously connected with a first temperature controller, and the heating belt is externally covered with an insulating layer, so that the temperature in the sampling head is controlled to be kept at 120 ℃. The sampling head is also provided with an on-line analysis device for temperature, pressure, flow rate and humidity.
A semiconductor condensing sheet is arranged in the semiconductor refrigerator, a second temperature sensor is arranged between the semiconductor condensing sheet and the semiconductor refrigerator, and the semiconductor condensing sheet and the second temperature sensor are simultaneously connected with a second temperature controller to control the temperature of the semiconductor refrigerator to be 4 ℃ so as to achieve the purpose of water removal; the lower end of the semiconductor refrigerator is provided with a condensate liquid level observation cylinder so as to observe the liquid level condition of condensate.
The heat tracing sampling tube between the electric ball valve and the traction pump is connected with a third temperature sensor and a third temperature controller, the third temperature sensor is connected with the third temperature controller, and the temperature of the control pipeline is 60 ℃.
An adsorption cold trap is arranged in the electric heating box and is respectively connected with the first ball valve and the fourth three-way ball valve; the adsorption cold trap is used for concentrating and enriching the sample gas and reducing the detection limit of gas pollutants.
The first sample inlet and the first glass liner tube are simultaneously connected with a fourth temperature controller, and the second sample inlet and the second glass liner tube are simultaneously connected with a fifth temperature controller, so that the effect of controlling the gas temperature is achieved.
The function of the sample quantitative ring is to measure a fixed volume of sample gas or standard gas, then the measured sample gas or standard gas sequentially passes through a third three-way ball valve and a first ball valve under the power of high-purity nitrogen gas to reach an adsorption cold trap, is enriched and concentrated in the adsorption cold trap, and then after the electric heating box rapidly heats and instantaneously thermally desorbs, enters a first sample inlet or a second sample inlet of gas chromatography through a fourth three-way ball valve, sequentially passes through a first glass liner tube, a first column temperature box, or a second glass liner tube and a second column temperature box, and then enters a hydrogen Flame Ionization Detector (FID) or an Electron Capture Detector (ECD) for analysis. The sampling adsorption tube is mainly used for collecting sample gas by an adsorption tube method, the gas collecting bag is mainly used for collecting sample gas by a gas bag method, and the sampling adsorption tube and the gas collecting bag can be used for efficiency comparison analysis of organic matter detection among different instruments or different analysis methods.
A first chromatographic column and a second chromatographic column are respectively arranged in the first column incubator and the second column incubator; the hydrogen Flame Ionization Detector (FID) connected to the first column incubator can measure most organic matters in a universal way, has high linearity, and the Electron Capture Detector (ECD) connected to the second column incubator can measure compounds containing N, O, S and other heteroatoms and halogenated hydrocarbon and other electric polar compounds. The hydrogen Flame Ionization Detector (FID) and the Electron Capture Detector (ECD) are respectively connected with a computer through a first photomultiplier and a second photomultiplier, and the computer is connected with the concentration alarm, so that the over-standard early warning can be realized. The computer can display parameters such as flue gas temperature, pressure, flow rate, humidity and the like in real time; the method comprises the steps that after calibration through calibration flow path equipment, an organic matter standard curve to be tested, calculation of sample gas and concentration of the sample gas are established and displayed in a computer; the temperature of each temperature controller, the opening and closing of each electric ball valve, the opening and closing of the pump and the adjustment of the flow of the flowmeter are controlled.
The opening and closing of the first three-way ball valve and the electric ball valve in the gas flow path can facilitate the selection of whether to open the back flushing flow path according to actual conditions; the four-way ball valve can control and select a gas sampling flow path, a measuring flow path or a calibration flow path; the first ball valve can control whether a measurement flow path is selected; the second ball valve and the third ball valve can control the selection of sampling adsorption tubes or gas collection bags for sampling; the fourth three-way ball valve can control gas to enter the first sample inlet or the second sample inlet.
The second mass flowmeter in the calibration flow path can measure the flow and the volume of the standard gas, and can measure the volume of the consumed high-purity nitrogen serving as power after the standard gas passes through the sample quantitative ring to quantify the volume in the equipment calibration process.
The high-purity nitrogen in the high-purity nitrogen bottle can be used as a power carrier gas to carry the sample gas in the sample quantitative ring in the calibration flow path, is adsorbed, enriched and concentrated in an adsorption cold trap, and enters a first sample inlet and a second sample inlet of gas chromatography after being quickly heated and desorbed by an electric heating box; and cleaning deposited ash and residues in the sampling flow path as back blowing in the back blowing flow path of the sampling head.
The working principle and the process of the utility model are as follows:
(1) Collection of waste gas of a fixed pollution source:
before sample collection, according to the sampling requirement, clean sampling adsorption tube or gas collecting bag is connected with second ball valve and third ball valve pipeline respectively. And starting the temperature control of the heating belt, the first temperature controller and the first temperature sensor, and accurately heating the temperature of the sampling head to 120 ℃ so as to prevent the adsorption of the objects in the sampling head during the sampling, wherein the temperature of the sampling head is synchronously displayed in a computer. The sampling head is also provided with a temperature, pressure, flow speed and humidity on-line analysis device, and a filter device is arranged inside the sampling head. When the first temperature controller displays that the temperature of the sampling head is heated to 120 ℃ and kept stable, the sampling head is inserted into a given flue sampling point, and at the moment, the temperature, humidity, pressure and flow rate parameters of the waste gas in the flue can be directly read from a computer. After the waste gas is filtered, the semiconductor refrigerator is judged to be started or not according to the flue gas moisture content value displayed by the computer in real time. When the moisture content of the flue gas is higher, the semiconductor refrigerator is started, the semiconductor refrigerator starts to refrigerate quickly, and the temperature of the semiconductor refrigerator is controlled to be maintained at 4 ℃ by the second temperature controller, so that the moisture in the flue gas can be condensed and removed quickly during sampling. If the moisture content of the flue gas meets the sampling requirement, the semiconductor refrigerator can be kept in a closed state. Opening the electric ball valve to open the gas flow path, starting the traction pump, and starting sampling. The temperature of the heat tracing sampling tube is maintained at 60 ℃ by a third temperature sensor and a third temperature controller. The rotary four-way ball valve is communicated with the third three-way ball valve, the flow of the first mass flowmeter and the sampling time are set through a computer, and the first ball valve is in a closed state. Under the control of the traction pump and the first mass flowmeter, the waste gas sequentially passes through the sampling head, the electric ball valve, the traction pump, the first mass flowmeter and the four-way ball valve, and according to actual sampling requirements, the waste gas sample collection of the sampling adsorption tube or the gas collecting bag is respectively realized through the opening and closing control of the second ball valve and the third ball valve. And storing the collected waste gas sample into a sampling adsorption tube or a gas collection bag, and controlling the sampling volume of the gas sample through the flow and the sampling time of the first mass flowmeter. After the first sample is collected, another clean sampling adsorption tube or a gas collection bag can be replaced to collect the next sample, or the traction pump can be directly turned off, the sampling head is taken out from the flue, and the sampling is completed.
(2) On-line monitoring of organic matters in waste gas of a fixed pollution source:
when the on-line monitoring of organic matters in the waste gas is implemented, the early-stage collection operation of the waste gas sample in the flue is the same as that of the step (1), at the moment, the four-way ball valve is turned to a measuring flow path, the left end and the right end of the four-way ball valve are communicated with each other and are communicated with a sample quantifying ring, and the second ball valve and the third ball valve are in a closed state. And through the pumping traction of the traction pump and the flow control of the first mass flowmeter, the sample gas enters the sample quantitative ring after passing through the four-way ball valve, a certain volume of waste gas sample is measured through the sample quantitative ring, and the upper end of the emptying valve is closed after the redundant sample gas is emptied through the emptying valve. The method comprises the steps of opening a high-purity nitrogen bottle, adjusting the flow rate of gas through a first pressure reducing valve and a first pressure gauge, opening a first three-way ball valve, enabling high-purity nitrogen to serve as carrier gas to enter a sample quantitative ring through the lower end and the left end of the first three-way ball valve, a second mass flowmeter and a four-way ball valve in sequence, enabling a waste gas sample with a good fixed volume in the sample quantitative ring to sequentially pass through a third three-way ball valve and the first ball valve under the power of the high-purity nitrogen, reaching an adsorption cold trap, concentrating and enriching in the adsorption cold trap, and enabling the waste gas sample to enter a first sample inlet or a second sample inlet through the fourth three-way ball valve after instant high-temperature thermal desorption through rapid heating of an electric heating box. According to the actual need of on-line monitoring, if the device is used for measuring most organic matters for universality, after entering a first sample inlet, sample gas sequentially flows through a first glass liner tube and a first chromatographic column and then enters a hydrogen Flame Ionization Detector (FID), and a fourth temperature controller and a first column temperature box can control the reaction temperature to be in a measurement requirement range. The FID detection signal enters a computer after passing through a first photomultiplier, and the concentration of the sample is calculated according to a standard curve established before measurement. If the sample gas is used for measuring the compounds containing N, O, S and other heteroatoms and the electrically polar compounds such as halogenated hydrocarbon, the sample gas sequentially flows through the second glass liner tube and the second chromatographic column and then enters an Electron Capture Detector (ECD), and the fifth temperature controller and the second column temperature box can be used for controlling the column temperature of the second chromatographic column to be in the organic matter measurement requirement range in a gradient manner. And (3) the ECD detection signals enter a computer after passing through a second photomultiplier, and the concentration of different organic matters in each sample gas sample is calculated according to a standard curve established before measurement. The computer is connected with the concentration alarm, and when the concentration of the organic matters in the waste gas exceeds the standard, the concentration alarm sounds to give out an alarm and displays the alarm on the computer.
(3) Cleaning a sampling head:
before the collection of the waste gas sample, after the completion of the sampling and when the dust deposit cleaning is needed after the equipment is used for a long time, the utility model can open the back-blowing flow path to carry out the cleaning operation of the sampling head. Closing the electric ball valve, opening the high-purity nitrogen bottle, adjusting the flow rate of high-purity nitrogen through the first pressure reducing valve and the first pressure gauge, opening the first three-way ball valve, and communicating the upper end and the lower end of the first three-way ball valve, so that the high-purity nitrogen enters the sampling head through the gas pipeline and is emptied through the sampling head, and convenient cleaning of dust accumulation and residue of the sampling head is realized.
(4) Calibration of the detector and establishment of different standard curves of various substances:
and the four-way ball valve is rotated, so that the lower end pipeline of the four-way ball valve is communicated with the right end pipeline, the first ball valve is opened, and the second ball valve and the third ball valve are closed. And opening a calibration module or a standard curve establishment module in the computer program. Opening the standard gas cylinder, controlling the standard gas flow rate through a second pressure reducing valve and a second pressure gauge, rotating the second three-way ball valve, enabling the right end and the upper end of the second three-way ball valve to be communicated, and controlling the standard gas flow rate through setting second mass flowmeter parameters through a computer. And (3) the standard gas enters a quantitative ring of the sample to obtain a fixed volume of standard gas, the redundant standard gas is emptied through an emptying valve, and then the upper end of the emptying valve is closed. The second three-way ball valve is rotated to enable the lower end and the upper end of the second three-way ball valve to be communicated, then a high-purity nitrogen bottle is opened, the gas flow rate is regulated through a first pressure reducing valve and a first pressure gauge, the first three-way ball valve is opened, high-purity nitrogen gas is enabled to be used as carrier gas to enter a sample quantitative ring through the lower end and the left end of the first three-way ball valve, the second mass flow meter and the four-way ball valve in sequence, and the standard gas with the measured fixed volume in the sample quantitative ring sequentially passes through the third three-way ball valve and the first ball valve under the power of the high-purity nitrogen gas to reach an adsorption cold trap, and is enriched and concentrated in the adsorption cold trap. And then, after the electric heating box rapidly heats the instant high-temperature thermal desorption, the desorption enters the first sample inlet or the second sample inlet through a fourth three-way ball valve. And (3) then, entering gas chromatography FID and ECD measurement processes of different organic matters in the same sample gas as in the step (2), and completing calibration and calibration of corresponding FID and ECD equipment of different organic matters and establishment of different standard curves of different matters.
The beneficial effects of the utility model are as follows:
1. the sampling head is provided with the temperature, pressure, flow speed and humidity on-line analysis device, and displays in real time on a computer, the sampling head can be heated at high temperature and is heat-resistant, cold and hot flue gas can be collected, and effective representativeness of a collected flue gas sample is ensured.
2. The utility model adopts the semiconductor refrigerator to efficiently condense and remove water, and the condensate liquid level observation cylinder is arranged at the bottom of the semiconductor refrigerator, so that the utility model is applicable to measuring volatile organic compounds in the flue gas with high humidity.
3. The utility model is provided with the back-blowing flow path of the sampling head, and can realize convenient cleaning of dust deposit residues of the sampling head and the sampling pipeline.
4. The utility model is provided with a gas sampling flow path and a measuring flow path after the flue gas passes through the four-way ball valve. The gas sampling flow path is provided with a sampling adsorption tube and a sampling bag, so that the gas can be sampled easily; the measuring flow path can analyze different types of organic matters by selecting a hydrogen Flame Ionization Detector (FID) or an Electron Capture Detector (ECD) which are suitable for each measuring flow path.
5. The utility model is provided with a calibration flow path, and can calibrate and calibrate the hydrogen Flame Ionization Detector (FID) and the Electron Capture Detector (ECD) in time so as to ensure the data quality.
6. The utility model can measure most organic compounds by using a hydrogen Flame Ionization Detector (FID) in a universal way, and can also measure compounds containing N, O, S and other heteroatoms and electric polar compounds such as halogenated hydrocarbon by using an Electron Capture Detector (ECD).
Drawings
FIG. 1 is a schematic diagram of the structure of the present utility model;
wherein: 1. a sampling head; 2. a heating belt; 3. a first temperature controller; 4. a heat preservation layer; 5. a first temperature sensor; 6. a semiconductor refrigerator; 7. a semiconductor condensing sheet; 8. a condensate liquid level observation cylinder; 9. a sampling line; 10. a second temperature controller; 11. a second temperature sensor; 12. an electric ball valve; 13. a heat tracing sampling tube; 14. a third temperature controller; 15. a traction pump; 16. a third temperature sensor; 17. a first mass flow meter; 18. a four-way ball valve; 19. a sample quantification ring; 20. a third three-way ball valve; 21. a first ball valve; 22. a second ball valve; 23. sampling adsorption tube; 24. a third ball valve; 25. a gas collection bag; 26. an electric heating box; 27. adsorbing a cold trap; 28. a fourth three-way ball valve; 29. a first sample inlet; 30. a fourth temperature controller; 31. a first glass liner; 32. a first column incubator; 33. a first chromatographic column; 34. a hydrogen flame ionization detector; 35. a first photomultiplier tube; 36. a second sample inlet; 37. a fifth temperature controller; 38. a second glass liner; 39. a second column incubator; 40. a second chromatographic column; 41. an electron capture detector; 42. a second photomultiplier tube; 43. a computer; 44. a high purity nitrogen cylinder; 45. a first pressure reducing valve; 46. a first pressure gauge; 47. a first three-way ball valve; 48. a gas marking cylinder; 49. a second pressure reducing valve; 50. a second pressure gauge; 51. a second three-way ball valve; 52. a second mass flow meter; 53. a concentration alarm; 54. and a vent valve.
Detailed Description
The utility model is further described below with reference to examples.
Example 1
As shown in FIG. 1, the environment-friendly on-line monitoring and sampling device for organic matters in the waste gas of the fixed pollution source comprises a gas sampling flow path, a measuring flow path, a sampling head blowback flow path and a calibration flow path.
The gas sampling flow path comprises a sampling head 1, a semiconductor refrigerator 6, an electric ball valve 12, a traction pump 15, a first mass flowmeter 17, a four-way ball valve 18, a third three-way ball valve 20, a second ball valve 22, a third ball valve 24, a sampling adsorption tube 23 and a gas collection bag 25, wherein the sampling head 1 is connected with the semiconductor refrigerator 6 through a sampling pipeline 9, the semiconductor refrigerator 6 is sequentially connected with the electric ball valve 12, the traction pump 15, the first mass flowmeter 17, the four-way ball valve 18 and the third three-way ball valve 20 through a heat tracing sampling tube 13, the third three-way ball valve 20 is respectively connected with the second ball valve 22 and the third ball valve 24 through the heat tracing sampling tube 13, the second ball valve 22 is connected with the sampling adsorption tube 23, and the third ball valve 24 is connected with the gas collection bag 25;
the measuring flow path comprises a sampling head 1, a semiconductor refrigerator 6, an electric ball valve 12, a traction pump 15, a first mass flowmeter 17, a four-way ball valve 18, a sample quantifying ring 19, an emptying valve 54, a third three-way ball valve 20, a first ball valve 21, an electric heating box 26 and a fourth three-way ball valve 28 which are sequentially connected, wherein the fourth three-way ball valve 28 is connected with two paths of parallel gas paths; one parallel gas path is that the fourth three-way ball valve 28 is sequentially connected with the first sample inlet 29, the first glass liner tube 31, the first column temperature box 32, the hydrogen flame ionization detector 34, the first photomultiplier 35 and the computer 43, and the other parallel gas path is that the fourth three-way ball valve 28 is sequentially connected with the second sample inlet 36, the second glass liner tube 38, the second column temperature box 39, the electron capture detector 41, the second photomultiplier 42 and the computer 43. Wherein, the pipeline between the sample ration ring 19 and the emptying valve 54, the third three-way ball valve 20, the first ball valve 21, the electric heating box 26 and the fourth three-way ball valve 28, and the pipeline between the fourth three-way ball valve 28 and the first sample inlet 29 and the second sample inlet 36 are all connected by the heat tracing sampling tube 13.
The sampling head blowback flow path comprises a high purity nitrogen cylinder 44, a first pressure reducing valve 45, a first pressure gauge 46, a first three-way ball valve 47 and the sampling head 1 which are connected in sequence.
The calibration flow path comprises a calibration gas cylinder 48, a second pressure reducing valve 49, a second pressure gauge 50, a second three-way ball valve 51, a second mass flowmeter 52, a four-way ball valve 18, a sample quantifying ring 19, an emptying valve 54, a third three-way ball valve 20, a first ball valve 21, an electric heating box 26 and a fourth three-way ball valve 28 which are sequentially connected, and the fourth three-way ball valve 28 is connected with two paths of parallel gas paths; the two parallel gas paths are the same as the two parallel gas paths in the measuring flow path; the calibration flow path further comprises a high-purity nitrogen cylinder 44, a first pressure reducing valve 45, a first pressure gauge 46 and a first three-way ball valve 47 which are sequentially connected, and the first three-way ball valve 47 is further connected with a second three-way ball valve 51.
The sampling head 1 is externally covered with a heating belt 2, the heating belt 2 is connected with a first temperature sensor 5, the heating belt 2 and the first temperature sensor 5 are simultaneously connected with a first temperature controller 3, and the heating belt 2 is externally covered with an insulating layer 4, so that the temperature in the sampling head 1 is controlled to be kept at 120 ℃. The sampling head 1 is also provided with an on-line analysis device for temperature, pressure, flow rate and humidity.
The semiconductor refrigerator 6 is internally provided with a semiconductor condensation piece 7, a second temperature sensor 11 is arranged between the semiconductor condensation piece 7 and the semiconductor refrigerator 6, the semiconductor condensation piece 7 and the second temperature sensor 11 are simultaneously connected with a second temperature controller 10, and the temperature of the semiconductor refrigerator 6 is controlled to be 4 ℃ so as to achieve the purpose of water removal; a condensate liquid level observation cylinder 8 is arranged at the lower end of the semiconductor refrigerator 6 so as to observe the liquid level condition of condensate.
The heat tracing sampling tube 13 between the electric ball valve 12 and the traction pump 15 is connected with a third temperature sensor 16 and a third temperature controller 14, the third temperature sensor 16 is connected with the third temperature controller 14, and the temperature of a control pipeline is 60 ℃.
An adsorption cold trap 27 is arranged in the electric heating box 26, and the adsorption cold trap 27 is respectively connected with the first ball valve 21 and the fourth three-way ball valve 28; the adsorption cold trap 27 acts to concentrate the enriched sample gas and reduce the detection limit of gaseous contaminants.
The first sample inlet 29 and the first glass liner tube 31 are simultaneously connected with the fourth temperature controller 30, and the second sample inlet 36 and the second glass liner tube 38 are simultaneously connected with the fifth temperature controller 37, so that the effect of controlling the gas temperature is achieved.
The function of the sample quantifying ring 19 is to measure a fixed volume of sample gas or standard gas, then the measured sample gas or standard gas is pushed by high-purity nitrogen to sequentially pass through the third three-way ball valve 20 and the first ball valve 21, reach the adsorption cold trap 27, be enriched and concentrated in the adsorption cold trap 27, then rapidly heat the instant high temperature desorption in the electric heating box 26, then enter the first sample inlet 29 or the second sample inlet 36 of the gas chromatograph through the fourth three-way ball valve 28, sequentially pass through the first glass liner 31, the first column incubator 32, or the second glass liner 38, the second column incubator 39, and then enter the hydrogen Flame Ionization Detector (FID) 34 or the Electron Capture Detector (ECD) 41 for analysis. The sampling adsorption tube 23 is mainly used for collecting sample gas by an adsorption tube method, the gas collection bag 25 is mainly used for collecting sample gas by a gas bag method, and the sampling adsorption tube 23 and the gas collection bag 25 can be used for efficiency comparison analysis of organic matter detection between different instruments or different analysis methods.
The first chromatographic column 33 and the second chromatographic column 40 are respectively arranged in the first column temperature box 32 and the second column temperature box 39; the hydrogen Flame Ionization Detector (FID) 34 connected to the first column incubator 32 can measure most organic substances in a universal manner, and has high linearity, and the Electron Capture Detector (ECD) 41 connected to the second column incubator 39 can measure a compound containing a heteroatom such as N, O, S and an electrically polar compound such as halogenated hydrocarbon. The hydrogen Flame Ionization Detector (FID) 34 and the Electron Capture Detector (ECD) 41 are connected to the computer 43 through the first photomultiplier tube 35 and the second photomultiplier tube 42, respectively, and the computer 43 is connected to the concentration alarm 53, so that the over-standard warning can be realized. The computer 43 can display parameters such as flue gas temperature, pressure, flow rate, humidity and the like in real time; the organic matter standard curve to be measured, the calculation of the sample gas and the concentration of the sample gas which are established after the calibration of the calibration flow path equipment are displayed in the computer 43; the temperature of each temperature controller, the opening and closing of each electric ball valve, the opening and closing of the pump and the adjustment of the flow of the flowmeter are controlled.
The opening and closing of the first three-way ball valve 47 and the electric ball valve 12 in the gas flow path can facilitate the selection of whether to open the blowback flow path according to the actual situation; the four-way ball valve 18 can control and select a gas sampling flow path, a measuring flow path or a calibration flow path; the first ball valve 21 can control whether or not a measurement flow path is selected; the second ball valve 22 and the third ball valve 24 can control the sampling adsorption tube 23 or the gas collection bag 25 to sample; the fourth three-way ball valve 28 can control the gas to enter the first sample inlet 29 or the second sample inlet 36.
The second mass flowmeter 52 in the calibration flow path can measure the flow and volume of the standard gas, and can also measure the volume of the consumed high-purity nitrogen serving as power after the standard gas is quantified by the sample quantifying ring 19 in the equipment calibration process.
The high-purity nitrogen in the high-purity nitrogen bottle 44 can be used as a power carrier gas to carry the sample gas in the sample quantitative ring 19 in a calibration flow path, is adsorbed, enriched and concentrated in the adsorption cold trap 27, and enters the first sample inlet 29 and the second sample inlet 36 of the gas chromatograph after being quickly heated and desorbed by the electric heating box 26; and cleaning deposited ash and residues in the sampling flow path as back blowing in the back blowing flow path of the sampling head.
(1) Collection of waste gas of a fixed pollution source:
before sample collection, a clean sampling adsorption tube 23 or a gas collection bag 25 is respectively connected with the second ball valve 22 and the third ball valve 24 in a pipeline mode according to sampling requirements. And starting the temperature control of the heating belt 2, the first temperature controller 3 and the first temperature sensor 5, and precisely heating the temperature of the sampling head 1 to 120 ℃ so as to prevent organic matters from being adsorbed on the sampling head 1 during sampling, wherein the temperature of the sampling head 1 is synchronously displayed on the computer 43. The sampling head 1 is also provided with an on-line analysis device for temperature, pressure, flow rate and humidity, and a filter device is arranged inside the sampling head 1 (the shaded part in the sampling head 1 in fig. 1 represents the filter device). When the first temperature controller 3 displays that the temperature of the sampling head 1 is heated to 120 ℃ and kept stable, the sampling head 1 is inserted into a given flue sampling point, and the temperature, humidity, pressure and flow rate parameters of the exhaust gas in the flue can be directly read from the computer 43. After the exhaust gas is filtered, it is judged whether to turn on the semiconductor refrigerator 6 or not based on the flue gas moisture content value displayed in real time by the computer 43. When the moisture content of the flue gas is high, the semiconductor refrigerator 6 is started, the semiconductor refrigerator 7 starts to rapidly refrigerate, and the temperature of the semiconductor refrigerator 6 is controlled to be maintained at 4 ℃ by the second temperature controller 10, so that the moisture in the flue gas can be rapidly condensed and removed during sampling. If the moisture content of the flue gas meets the sampling requirement, the semiconductor refrigerator 6 can be kept in the off state. The electric ball valve 12 is opened to open a gas flow path, the traction pump 15 is started, and sampling is started. The temperature of the heat trace sampling tube 13 is maintained at 60 ℃ by the third temperature sensor 16 and the third temperature controller 14. The rotary four-way ball valve 18 is communicated with the third three-way ball valve 20, the flow of the first mass flowmeter 17 and the sampling time are set through the computer 43, and the first ball valve 21 is in a closed state. Under the control of the traction pump 15 and the first mass flowmeter 17, the waste gas sequentially passes through the sampling head 1, the electric ball valve 12, the traction pump 15, the first mass flowmeter 17 and the four-way ball valve 18, and according to actual sampling requirements, the waste gas sample collection of the sampling adsorption tube 23 or the gas collecting bag 25 is respectively realized through the opening and closing control of the second ball valve 22 and the third ball valve 24. The collected exhaust gas sample is stored in the sampling adsorption tube 23 or the gas collection bag 25, and the sampling volume of the gas sample is controlled by the flow rate and sampling time of the first mass flowmeter 17. After the first sample is collected, another clean sampling adsorption tube 23 or a gas collection bag 25 can be replaced to collect the next sample, or the traction pump 15 can be directly turned off, the sampling head 1 is taken out from the flue, and the sampling is completed.
(2) On-line monitoring of organic matters in waste gas of a fixed pollution source:
when the on-line monitoring of organic matters in the waste gas is implemented, the earlier-stage collection operation of the waste gas sample in the flue is the same as that of the step (1), at the moment, the four-way ball valve 18 turns to a measuring flow path, the left end and the right end of the four-way ball valve 18 are communicated with the sample quantifying ring 19, and the second ball valve 22 and the third ball valve 24 are in a closed state. Through the pumping traction of the traction pump 15 and the flow control of the first mass flowmeter 17, the sample gas enters the sample quantifying ring 19 after passing through the four-way ball valve 18, a certain volume of waste gas sample is measured through the sample quantifying ring 19, and after the surplus sample gas is emptied through the emptying valve 54, the upper end of the emptying valve 54 is closed. The high-purity nitrogen cylinder 44 is opened, the gas flow rate is regulated through the first pressure reducing valve 45 and the first pressure gauge 46, the first three-way ball valve 47 is opened, high-purity nitrogen is used as carrier gas to enter the sample quantifying ring 19 through the lower end and the left end of the first three-way ball valve 47, the second three-way ball valve 51, the second mass flowmeter 52 and the four-way ball valve 18 in sequence, the measured waste gas sample with fixed volume in the sample quantifying ring 19 sequentially passes through the third three-way ball valve 20 and the first ball valve 21 under the power of the high-purity nitrogen, reaches the adsorption cold trap 27, is concentrated and enriched in the adsorption cold trap 27, and then enters the first sample inlet 29 or the second sample inlet 36 through the fourth three-way ball valve 28 after the instantaneous high-temperature thermal desorption is heated through the electric heating box 26. According to the actual requirement of on-line monitoring, if the device is a general device for measuring most organic matters, the sample gas flows through the first glass liner tube 31 and the first chromatographic column 33 in sequence after entering the first sample inlet 29, and then enters the hydrogen Flame Ionization Detector (FID) 34, and the fourth temperature controller 30 and the first column temperature box 32 can control the reaction temperature to be within the measurement requirement range. The FID detection signal passes through the first photomultiplier 35 and enters the computer 43, and the concentration of the sample is calculated according to a standard curve established before measurement. In order to measure the compounds containing N, O, S and other hetero atoms and the electrically polar compounds such as halogenated hydrocarbon, the sample gas enters the second sample inlet 36, flows through the second glass liner 38 and the second chromatographic column 40 in sequence, and then enters the Electron Capture Detector (ECD) 41, and the fifth temperature controller 37 and the second column temperature box 39 can control the column temperature of the second chromatographic column 40 in a gradient manner within the organic matter measurement requirement range. The ECD detection signal passes through the second photomultiplier tube 42 and then enters the computer 43, and the concentration of different organic matters in each sample gas sample is calculated according to a standard curve established before measurement. The computer 43 is connected with the concentration alarm 53, and when the concentration of the organic matters in the waste gas exceeds the standard, the concentration alarm 53 sounds an exceeding standard early warning and is displayed on the computer 43.
(3) Cleaning a sampling head:
before the collection of the waste gas sample, after the completion of the sampling and when the dust deposit cleaning is needed after the equipment is used for a long time, the utility model can open the back-blowing flow path to carry out the cleaning operation of the sampling head 1. The electric ball valve 12 is closed, the high-purity nitrogen bottle 44 is opened, the flow rate of high-purity nitrogen is regulated through the first pressure reducing valve 45 and the first pressure gauge 46, the first three-way ball valve 47 is opened, the upper end and the lower end of the first three-way ball valve 47 are communicated, so that the high-purity nitrogen enters the sampling head 1 through a gas pipeline and is emptied through the sampling head 1, and convenient cleaning of dust accumulation and residue of the sampling head 1 is realized.
(4) Calibration of the detector and establishment of different standard curves of various substances:
the four-way ball valve 18 is rotated to enable the lower end pipeline of the four-way ball valve 18 to be communicated with the right end pipeline, the first ball valve 21 is opened, and the second ball valve 22 and the third ball valve 24 are closed. The calibration module or standard curve creation module in the computer 43 program is turned on. The standard gas cylinder 48 is opened, the standard gas flow rate is controlled through the second pressure reducing valve 49 and the second pressure gauge 50, the second three-way ball valve 51 is rotated, the right end and the upper end of the second three-way ball valve 51 are communicated, and the standard gas flow rate is controlled through the parameters of the second mass flowmeter 52 set by the computer 43. The standard gas enters the sample dosing ring 19 to measure a fixed volume of standard gas, and the excess standard gas is emptied through the vent valve 54, after which the upper end of the vent valve 54 is closed. The second three-way ball valve 51 is rotated to enable the lower end and the upper end of the second three-way ball valve 51 to be communicated, then the high-purity nitrogen bottle 44 is opened, the gas flow rate is regulated through the first pressure reducing valve 45 and the first pressure gauge 46, the first three-way ball valve 47 is opened, high-purity nitrogen is enabled to be used as carrier gas to enter the sample quantifying ring 19 through the lower end and the left end of the first three-way ball valve 47, the second three-way ball valve 51, the second mass flowmeter 52 and the four-way ball valve 18 in sequence, and the measured standard gas with fixed volume in the sample quantifying ring 19 sequentially passes through the third three-way ball valve 20 and the first ball valve 21 under the power of the high-purity nitrogen to reach the adsorption cold trap 27 and is enriched and concentrated in the adsorption cold trap 27. Then after the electric heating box 26 rapidly heats the instant high temperature thermal desorption, the desorption enters the first sample inlet 29 or the second sample inlet 36 through the fourth three-way ball valve 28. And (3) then, entering gas chromatography FID and ECD measurement processes of different organic matters in the same sample gas as in the step (2), and completing calibration and calibration of corresponding FID and ECD equipment of different organic matters and establishment of different standard curves of different matters.
Claims (10)
1. The utility model provides an environmental protection on-line monitoring and sampling equipment of organic matter in fixed pollution source waste gas, includes gas sampling flow path, measurement flow path, sampling head blowback flow path and demarcation flow path, its characterized in that: the gas sampling flow path comprises a sampling head (1), a semiconductor refrigerator (6), an electric ball valve (12), a traction pump (15), a first mass flowmeter (17), a four-way ball valve (18), a third three-way ball valve (20), a second ball valve (22), a third ball valve (24), a sampling adsorption tube (23) and a gas collection bag (25), wherein the sampling head (1) is connected with the semiconductor refrigerator (6) through a sampling pipeline (9), the semiconductor refrigerator (6) is sequentially connected with the electric ball valve (12), the traction pump (15), the first mass flowmeter (17), the four-way ball valve (18) and the third three-way ball valve (20) through a heat tracing sampling tube (13), the third three-way ball valve (20) is respectively connected with the second ball valve (22) and the third ball valve (24), the second ball valve (22) is connected with the sampling adsorption tube (23), and the third ball valve (24) is connected with the gas collection bag (25);
the measuring flow path comprises a sampling head (1), a semiconductor refrigerator (6), an electric ball valve (12), a traction pump (15), a first mass flowmeter (17), a four-way ball valve (18), a sample quantitative ring (19), a vent valve (54), a third three-way ball valve (20), a first ball valve (21), an electric heating box (26) and a fourth three-way ball valve (28) which are sequentially connected, wherein the fourth three-way ball valve (28) is connected with two paths of parallel gas paths; one path of parallel gas path is that a fourth three-way ball valve (28) is sequentially connected with a first sample inlet (29), a first glass liner tube (31), a first column incubator (32), a hydrogen flame ionization detector (34), a first photomultiplier tube (35) and a computer (43), and the other path of parallel gas path is that the fourth three-way ball valve (28) is sequentially connected with a second sample inlet (36), a second glass liner tube (38), a second column incubator (39), an electron capture detector (41), a second photomultiplier tube (42) and the computer (43).
2. The environmental protection on-line monitoring and sampling device for organic matters in exhaust gas with fixed pollution sources according to claim 1, wherein: the sampling head blowback flow path comprises a high-purity nitrogen cylinder (44), a first pressure reducing valve (45), a first pressure gauge (46), a first three-way ball valve (47) and a sampling head (1) which are connected in sequence.
3. The environmental protection on-line monitoring and sampling device for organic matters in exhaust gas with fixed pollution sources according to claim 2, wherein: the calibration flow path comprises a calibration gas cylinder (48), a second pressure reducing valve (49), a second pressure gauge (50), a second three-way ball valve (51), a second mass flowmeter (52), a four-way ball valve (18), a sample quantifying ring (19), a vent valve (54), a third three-way ball valve (20), a first ball valve (21), an electric heating box (26) and a fourth three-way ball valve (28) which are sequentially connected, wherein the fourth three-way ball valve (28) is connected with two paths of parallel gas paths; the two parallel gas paths are the same as the two parallel gas paths in the measuring flow path; the calibration flow path further comprises a high-purity nitrogen cylinder (44), a first pressure reducing valve (45), a first pressure gauge (46) and a first three-way ball valve (47), wherein the high-purity nitrogen cylinder, the first pressure reducing valve, the first pressure gauge and the first three-way ball valve (47) are sequentially connected, and the first three-way ball valve (47) is further connected with a second three-way ball valve (51).
4. The environmental protection on-line monitoring and sampling device for organic matters in exhaust gas with fixed pollution sources according to claim 1, wherein: the sampling head (1) is covered with a heating belt (2), the heating belt (2) is connected with a first temperature sensor (5), the heating belt (2) and the first temperature sensor (5) are simultaneously connected with a first temperature control instrument (3), and the heating belt (2) is covered with a heat preservation layer (4).
5. The environmental protection on-line monitoring and sampling device for organic matters in exhaust gas with fixed pollution sources according to claim 1, wherein: a semiconductor condensing sheet (7) is arranged in the semiconductor refrigerator (6), a second temperature sensor (11) is arranged between the semiconductor condensing sheet (7) and the semiconductor refrigerator (6), and the semiconductor condensing sheet (7) and the second temperature sensor (11) are simultaneously connected with a second temperature controller (10); the lower end of the semiconductor refrigerator (6) is provided with a condensate liquid level observation cylinder (8).
6. The environmental protection on-line monitoring and sampling device for organic matters in exhaust gas with fixed pollution sources according to claim 1, wherein: the heat tracing sampling tube (13) between the electric ball valve (12) and the traction pump (15) is connected with a third temperature sensor (16) and a third temperature controller (14), and the third temperature sensor (16) is connected with the third temperature controller (14).
7. The environmental protection on-line monitoring and sampling device for organic matters in exhaust gas with fixed pollution sources according to claim 1, wherein: an adsorption cold trap (27) is arranged in the electric heating box (26), and the adsorption cold trap (27) is respectively connected with the first ball valve (21) and the fourth three-way ball valve (28).
8. The environmental protection on-line monitoring and sampling device for organic matters in exhaust gas with fixed pollution sources according to claim 1, wherein: the first sample inlet (29) and the first glass liner tube (31) are connected with the fourth temperature control instrument (30) at the same time, and the second sample inlet (36) and the second glass liner tube (38) are connected with the fifth temperature control instrument (37) at the same time.
9. The environmental protection on-line monitoring and sampling device for organic matters in exhaust gas with fixed pollution sources according to claim 1, wherein: the first chromatographic column (33) and the second chromatographic column (40) are respectively arranged in the first column incubator (32) and the second column incubator (39).
10. The environmental protection on-line monitoring and sampling device for organic matters in exhaust gas with fixed pollution sources according to claim 1, wherein: the computer (43) is connected with the concentration alarm (53).
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| CN202320238167.6U CN219496275U (en) | 2023-02-17 | 2023-02-17 | Environment-friendly on-line monitoring and sampling equipment for organic matters in waste gas with fixed pollution sources |
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