CN210572144U - Real-time measurement all-in-one of quality of water volatility organic matter - Google Patents

Real-time measurement all-in-one of quality of water volatility organic matter Download PDF

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CN210572144U
CN210572144U CN201921501276.2U CN201921501276U CN210572144U CN 210572144 U CN210572144 U CN 210572144U CN 201921501276 U CN201921501276 U CN 201921501276U CN 210572144 U CN210572144 U CN 210572144U
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module
pipe
sample gas
valve
communicated
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闫兴钰
张宁
李锋艳
张利军
李建行
郭旭
王晋
吕子啸
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Sinogreen Environmental Protection Science & Technology Co ltd
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Sinogreen Environmental Protection Science & Technology Co ltd
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Abstract

The utility model relates to a real-time measurement all-in-one of water quality volatility organic matter belongs to the environmental protection field, concretely relates to online monitoring of water volatility organic matter, the utility model aims to solve the problem that a real-time measurement all-in-one of water quality volatility organic matter is provided, can automatic sampling replace the current manual on-the-spot sampling, on-the-spot automatic cold trap sweeping is catched the thermal desorption and is replaced the laboratory manual operation and is catched the thermal desorption flow, can automatic online sweep the preliminary treatment, and the analysis of autoinjection, the data is uploaded and is preserved; the technical scheme is as follows: the device comprises an automatic sampling sealing calibration module, an online dewatering module and a cold trap trapping high-temperature analysis module; the automatic sampling sealing calibration module, the online dewatering module and the cold trap trapping high-temperature analysis module are sequentially communicated, a sampling pump is connected to the automatic sampling sealing calibration module, and after the sampling pump is dried by the online dewatering module, a sample is analyzed by the cold trap trapping high-temperature analysis module and then is monitored; the utility model discloses but wide application in environmental protection field.

Description

Real-time measurement all-in-one of quality of water volatility organic matter
Technical Field
The utility model relates to a real-time measurement all-in-one of quality of water volatility organic matter belongs to environmental protection and detects technical field.
Background
In the existing monitoring method for volatile organic compounds in water, water samples are collected, packaged and stored in a water body site manually and then are taken back to a laboratory for chromatographic analysis, and the monitoring method inevitably leads to inaccurate data caused by the volatility of monitoring factors; in addition, the sample is taken back to a laboratory after field sampling, so that the timeliness is poor, and the change condition of the water quality cannot be reflected in time; finally, the existing monitoring method needs manual participation and cannot achieve the effect of continuous online monitoring.
SUMMERY OF THE UTILITY MODEL
The utility model overcomes prior art exists not enough, provides a real-time measurement all-in-one of quality of water volatility organic matter, can automatic sampling replace current artifical on-the-spot sample, and the on-the-spot cold trap entrapment thermal desorption that sweeps replaces laboratory manual operation entrapment thermal desorption flow automatically, can sweep the preliminary treatment on line automatically to autoinjection analysis, data upload the save.
In order to solve the technical problem, the utility model discloses a technical scheme be: a real-time measurement integrated machine for water quality volatile organic compounds comprises an automatic sampling sealing calibration module, an online dewatering module and a cold trap trapping high-temperature analysis module; the automatic sampling sealing calibration module, the online dewatering module and the cold trap trapping high-temperature analysis module are sequentially communicated, a sampling pump is connected to the automatic sampling sealing calibration module, and after the sampling pump is dried by the online dewatering module, a sample is analyzed by the cold trap trapping high-temperature analysis module and then is monitored;
the automatic sampling sealing calibration module has the structure that: comprises a headspace bottle, a nine-hole valve, a purging pipe and a peristaltic pump, wherein the headspace bottle and the purging pipe are both communicated with the nine-hole valve, the peristaltic pump is connected with the purging pipe, sucking the calibration medium in the headspace bottle into a purging tube through a peristaltic pump, wherein a first liquid level sensor and a second liquid level sensor are arranged in the purging tube, the first liquid level sensor is positioned above the second liquid level sensor, the first liquid level sensor is used for calibrating the volume of the medium, the second liquid level sensor is used for overtravel level alarm, the nine-hole valve is also connected with a nitrogen source which is communicated with the purging pipe through the nine-hole valve, the device is used for blowing out volatile organic compounds in the calibration medium in the purging pipe, a two-position three-way electromagnetic valve is arranged on a pipeline between the peristaltic pump and the purging pipe, and the volatile organic compounds blown out from the purging pipe are communicated with the online dewatering module through the two-position three-way electromagnetic valve;
the structure of the online dewatering module is as follows: the device comprises a nafion tube, a hydrogen-air integrated machine, a sample gas inlet end and a sample gas outlet end, wherein one end of the nafion tube is communicated with the sample gas inlet end, the other end of the nafion tube is communicated with the sample gas outlet end, the sample gas inlet end and the sample gas outlet end are communicated through a membrane inner side channel of the nafion tube, one end of a membrane outer side channel of the nafion tube is an emptying end, the other end of the membrane outer side channel of the nafion tube is connected to the hydrogen-air integrated machine through a drying pipeline, the drying pipeline is provided with a drying tank filled with a drying agent, water in the sample gas is analyzed by utilizing the pressure gradient of water inside and outside the membrane of the nafion tube, the sample gas inlet end is communicated with an automatic sampling sealing calibration module, and the sample gas outlet end is communicated with a cold trap high-temperature analysis module;
the cold trap trapping high-temperature analysis module has the structure that: including entrapment device, heating device and gas chromatograph, the both ends of entrapment device are connected on gas chromatograph through the valve that sets up in gas chromatograph, gas chromatograph still is connected through valve and the empty all-in-one of hydrogen and online dewatering module, dry sample gas passes through the entrapment device and is caught by the entrapment device entrapment through the valve in the online dewatering module, heating device sets up on the entrapment device for the sample gas of entrapment device entrapment is decomposed in the heating, and sends into the nitrogen gas that the sample gas after will decomposing provides through the nitrogen gas source and carry out the testing and analyzing in the gas chromatograph as the power supply, the empty all-in-one of hydrogen is used for providing hydrogen and air for gas chromatograph FID detector burning to provide the energy source for inside solenoid valve.
The blowing pipe is a transparent pipe, a heating resistance wire is wound on the periphery of the blowing pipe, the blowing pipe is located in a heat insulation box made of heat insulation materials, and an observation window is formed in the position, corresponding to the blowing pipe, of the heat insulation box.
And the nine-hole valve is connected with a distilled water bottle and a waste liquid bottle, and the distilled water bottle and the waste liquid bottle are respectively used for cleaning the purging pipe and storing the cleaned waste liquid.
And the drying pipeline is provided with a flow valve and an electromagnetic valve.
And valves are arranged at two ends of the heating device, and when the valves are closed, the heating device is triggered to start heating the trapping device.
The heating device can heat the trapping device to 100-200 ℃.
Compared with the prior art, the utility model beneficial effect who has is:
1. the utility model discloses can satisfy and directly carry out continuous on-line monitoring at the water scene, relevant data is preserved in the content of volatile organic compounds and record in the real-time recording water, has avoided because the error that loaded down with trivial details manual operation caused with postpone.
2. The utility model discloses can realize the on-the-spot automatic quantitative sampling of water sample, need not artifical sample.
3. The utility model discloses a sealed calibration sample can realize calibrating the sample under the minimum condition that volatilizees of calibration standard liquid, has avoided because the degree of accuracy that the standard liquid volatilizees and causes reduces.
Drawings
The present invention will be further described with reference to the accompanying drawings.
Fig. 1 is a schematic structural diagram of the present invention.
In the figure: the device comprises an automatic sampling seal calibration module 1, a headspace bottle 11, a nine-hole valve 12, a purging pipe 13, a peristaltic pump 14, a first liquid level sensor 15, a second liquid level sensor 16, a nitrogen source 17, a two-position three-way electromagnetic valve 18, a distilled water bottle 110, a waste liquid bottle 111, an online dewatering module 2, a nafion pipe 21, a hydrogen-air all-in-one machine 22, a sample gas inlet end 23, a sample gas outlet end 24, a sample gas outlet end 25, a drain end 26, a drying pipeline 27, a drying tank 28, a flow valve 29, an electromagnetic valve 3, a cold trap high-temperature analysis module 31, a trap device 32, a heating device 33, a gas chromatograph and a sampling pump 4.
Detailed Description
As shown in fig. 1, the utility model relates to a real-time measurement all-in-one machine for water quality volatile organic compounds, which comprises an automatic sampling seal calibration module 1, an online dewatering module 2 and a cold trap trapping high temperature analysis module 3; the automatic sampling sealing calibration module 1, the online dewatering module 2 and the cold trap trapping high-temperature analysis module 3 are sequentially communicated, the automatic sampling sealing calibration module 1 is connected with a sampling pump 4, and after the sampling pump 4 is dried by the online dewatering module 2, a sample is analyzed by the cold trap trapping high-temperature analysis module 3 and then is monitored;
the automatic sampling sealing calibration module 1 has the structure that: including head space bottle 11, nine orifice valves 12, purge tube 13 and peristaltic pump 14, head space bottle 11 and purge tube 13 all communicate with nine orifice valves 12, peristaltic pump 14 is connected on purge tube 13, inhales the calibration medium in the head space bottle 11 through peristaltic pump 14 in purge tube 13, be provided with first level sensor 15 and second level sensor 16 in purge tube 13, first level sensor 15 is located the top of second level sensor 16, utilizes first level sensor 15 to mark the medium volume, utilizes second level sensor 16 to do super liquid level warning usefulness, still be connected with nitrogen source 17 on the nine orifice valves 12, nitrogen source 17 communicates with purge tube 13 through nine orifice valves 12 for blow out the volatile organic compounds in the calibration medium in purge tube 13, be provided with two three way solenoid valves 18 on the pipeline between peristaltic pump 14 and purge tube 13, the volatile organic compounds blown out of the blowing pipe 13 through the middle drum are communicated with the online dewatering module 2 through a two-position three-way electromagnetic valve 18;
the structure of the online dewatering module 2 is as follows: the device comprises a nafion tube 21, a hydrogen-air integrated machine 22, a sample gas inlet end 23 and a sample gas outlet end 24, wherein one end of the nafion tube 21 is communicated with the sample gas inlet end 23, the other end of the nafion tube 21 is communicated with the sample gas outlet end 24, the sample gas inlet end 23 is communicated with the sample gas outlet end 24 through a membrane inner side channel of the nafion tube 21, one end of a membrane outer side channel of the nafion tube 21 is an emptying end 25, the other end of the membrane outer side channel of the nafion tube 21 is connected to the hydrogen-air integrated machine 22 through a drying pipeline 26, the drying pipeline 26 is provided with a drying tank 27 filled with a drying agent, water in the sample gas is analyzed out by utilizing the pressure gradient of water in the membrane outer side of the nafion tube 21, the sample gas inlet end 23 is communicated with an automatic sampling sealing calibration module 1, and the sample gas outlet end 24 is communicated with a cold trap gas outlet high-temperature analysis module 3;
the structure of the cold trap trapping high-temperature analysis module 3 is as follows: including entrapment device 31, heating device 32 and gas chromatograph 33, the both ends of entrapment device 31 are connected on gas chromatograph 33 through the valve that sets up in gas chromatograph 33, gas chromatograph 33 still is connected with empty all-in-one of hydrogen 22 and online dewatering module 2 through the valve, dry sample gas passes through entrapment device 31 and is caught by entrapment device 31 in online dewatering module 2 through the valve, heating device 32 sets up on entrapment device 31 for the sample gas of thermal decomposition entrapment device 31 entrapment, and send into gas chromatograph 33 as the power supply with the nitrogen gas that the sample gas after will decomposing provided through nitrogen source 17 and carry out the detection and analysis in, empty all-in-one of hydrogen 22 is used for providing hydrogen and air for gas chromatograph 33FID detector burning to provide the energy source for inside solenoid valve.
The purging pipe 13 is a transparent pipe, a heating resistance wire is wound on the periphery of the purging pipe, the purging pipe 13 is located in a heat insulation box made of heat insulation materials, and an observation window is formed in the position, corresponding to the purging pipe 13, on the heat insulation box.
The nine-hole valve 12 is connected with a distilled water bottle 110 and a waste liquid bottle 111, and the distilled water bottle 110 and the waste liquid bottle 111 are respectively used for cleaning the purging tube 13 and storing the cleaned waste liquid.
The drying line 26 is provided with a flow valve 28 and a solenoid valve 29.
Valves are arranged at two ends of the heating device 32, and when the valves are closed, the heating device 32 is triggered to start heating the trapping device 31.
The heating device 32 can heat the trapping device 31 to 100-200 ℃, and can be set at any temperature.
The utility model adopts electrical elements such as a nine-hole valve 12, a peristaltic pump 14, a quantitative component, a stepping motor driver and the like to perform timing and quantitative sampling under the control of a PLC control unit; the automatic purging, trapping and analyzing process is carried out by adopting elements such as a purging component, an electromagnetic valve, a flow sensor, an adsorption and desorption module, a temperature controller and the like under the control of a PLC control unit; performing online purging pretreatment by adopting a nafion pipe water removal technology and a hydrogen-air integrated machine; the real-time communication of the PLC, the industrial personal computer software and the gas chromatograph is adopted to automatically control the analysis process, and the functions of automatic sample injection analysis and data uploading and storage are completed.
In order to solve the problem of interference and loss of a water removal link on target substances, the chemical affinity based on nafion sulfuric acid is adopted to remove moisture in gas, so that the target gas cannot be contacted with the moisture to cause loss, and the nafion pipe material cannot interfere the target gas. Because the pressure gradient of moisture needs to be formed in nafion membrane both sides to the dehydration of nafion pipe, this system gathers ambient air through the compressor, sends the dry air to the nafion membrane outside through the action of PLC control solenoid valve after the drier is dry and carries out incessant dehydration to the target substance. The method can ensure the water removal effect and eliminate the interference problem to the target substance due to the non-contact water removal mode.
The whole set of automatic sampling sealing calibration system of the structural part adopts vacuum suction force generated by the action of a peristaltic pump 14 as power, a stainless steel ceramic sealing nine-hole valve 12 as a water body sample introduction control mechanism, a visual quantitative purging pipe 13 with a liquid level control heating system, a two-position three-way electromagnetic valve 18 as an emptying device during sealing calibration sampling, and a headspace bottle 11 as a container for calibration liquid.
The control part controls the action of the peristaltic pump 14, the nine-hole valve 12 and the emptying device through a PLC program, so that the on-site water sample or the calibration standard liquid sealed in the headspace bottle 11 is sent into the purging pipe 13 for the next treatment. In the process, the standard solution in the headspace bottle 11 can directly enter a subsequent system for analysis without being exposed in the air basically, so that the volatilization loss of volatile organic compounds is reduced, and the calibration accuracy is ensured.
The utility model discloses in because target volatile organic compounds boiling point is between 50 ℃ -260 ℃, at first select the stronger TenaxGR of target material adsorption affinity and active carbon to pack as the adsorbent, rely on in addition to install in entrapment device 31 in the axial syntropy radiator fan of adsorption tube and create low temperature environment at the adsorption process, guarantee that adsorption efficiency satisfies the minimum requirement of detecting the limit of chromatograph.
After adsorption is finished, the system switches pipelines under the control of a PLC and a temperature controller, seals two sides of an adsorption tube in a trapping device 31, triggers a heating device 32 on the periphery of the adsorption tube to heat the adsorption tube to 200 ℃ instantly, and controls to carry out reverse purging on the adsorption tube through a flow path of an electromagnetic valve to ensure that the adsorbed target substance is completely analyzed, wherein the heating device 32 is a spiral heater;
selecting high-temperature-resistant TenaxGR and activated carbon as adsorbents, and adding high-temperature-resistant silanized glass wool as a filtering device on two sides of the adsorbents except for mounting a metal sealing net;
in order to avoid the loss of substances after the analysis is finished, the pipeline is heated and insulated by high temperature tracing during the period that the analysis is finished and then the chromatographic column box is filled with the substances, in addition, the inner diameter of the pipeline at the later stage of the analysis and the inner diameter of the electromagnetic valve are strictly controlled not to be more than 1/8 inch, and the dead volume of the pipeline is reduced;
in the trapping analysis process, the PLC controls a plurality of electromagnetic valves, temperature controllers, flow sensors and other components to achieve preset actions.
The present invention has been described in detail with reference to the embodiments, but the present invention is not limited to the above embodiments, and various changes can be made without departing from the gist of the present invention within the knowledge of those skilled in the art.

Claims (6)

1. The utility model provides a real-time measurement all-in-one of quality of water volatility organic matter which characterized in that: comprises an automatic sampling sealing calibration module (1), an online dewatering module (2) and a cold trap trapping high-temperature analysis module (3); the automatic sampling sealing calibration module (1), the online dewatering module (2) and the cold trap trapping high-temperature analysis module (3) are sequentially communicated, a sampling pump (4) is connected to the automatic sampling sealing calibration module (1), and after the sampling pump (4) is dried by the online dewatering module (2), a sample is analyzed by the cold trap trapping high-temperature analysis module (3) and then is monitored;
the automatic sampling sealing calibration module (1) has the structure that: the device comprises a headspace bottle (11), a nine-hole valve (12), a purging pipe (13) and a peristaltic pump (14), wherein the headspace bottle (11) and the purging pipe (13) are communicated with the nine-hole valve (12), the peristaltic pump (14) is connected onto the purging pipe (13), a calibration medium in the headspace bottle (11) is sucked into the purging pipe (13) through the peristaltic pump (14), a first liquid level sensor (15) and a second liquid level sensor (16) are arranged in the purging pipe (13), the first liquid level sensor (15) is located above the second liquid level sensor (16), the first liquid level sensor (15) is used for calibrating the volume of the medium, the second liquid level sensor (16) is used for ultra-liquid level warning, a nitrogen source (17) is further connected onto the nine-hole valve (12), the nitrogen source (17) is communicated with the purging pipe (13) through the nine-hole valve (12) and is used for blowing out the volatile organic compounds in the calibration medium in the purging pipe (13), a two-position three-way electromagnetic valve (18) is arranged on a pipeline between the peristaltic pump (14) and the purging pipe (13), and volatile organic compounds blown out from the purging pipe (13) are communicated with the online water removal module (2) through the two-position three-way electromagnetic valve (18);
the structure of the online dewatering module (2) is as follows: the device comprises a nafion pipe (21), a hydrogen-air integrated machine (22), a sample gas inlet end (23) and a sample gas outlet end (24), wherein one end of the nafion pipe (21) is communicated with the sample gas inlet end (23), the other end of the nafion pipe (21) is communicated with the sample gas outlet end (24), the sample gas inlet end (23) and the sample gas outlet end (24) are communicated through a membrane inner side channel of the nafion pipe (21), one end of a membrane outer side channel of the nafion pipe (21) is a discharge end (25), the other end of the membrane outer side channel of the nafion pipe (21) is connected to the hydrogen-air integrated machine (22) through a drying pipeline (26), a drying tank (27) filled with a drying agent is arranged on the drying pipeline (26), the water in the sample gas is separated out by utilizing the pressure gradient of water in the membrane outer side of the nafion pipe (21), and the sample gas inlet end (23) is communicated with an automatic sampling and sealing calibration module (1), the sample gas outlet end (24) is communicated with the cold trap trapping high-temperature analysis module (3);
the cold trap trapping high-temperature analysis module (3) has the structure that: including entrapment device (31), heating device (32) and gas chromatograph (33), the both ends of entrapment device (31) are connected on gas chromatograph (33) through the valve that sets up in gas chromatograph (33), gas chromatograph (33) still are connected through valve and hydrogen-air all-in-one (22) and online dewatering module (2), dry sample gas passes through entrapment device (31) and is caught by entrapment device (31) through the valve in online dewatering module (2), heating device (32) set up on entrapment device (31) for the sample gas that heating decomposition was caught by entrapment device (31) to send into gas chromatograph (33) as the power supply with the nitrogen gas that the sample gas after will decomposing provided through nitrogen source (17) and carry out the detection analysis, hydrogen-air all-in-one (22) are used for providing hydrogen and air for gas chromatograph (33) FID detector burning, and provides a source of energy for the internal solenoid valve.
2. The real-time measurement all-in-one of quality of water volatility organic matter of claim 1, characterized by: the purging pipe (13) is a transparent pipe, a heating resistance wire is wound on the periphery of the purging pipe, the purging pipe (13) is located in a heat insulation box made of heat insulation materials, and an observation window is formed in the position, corresponding to the purging pipe (13), on the heat insulation box.
3. The real-time measurement all-in-one of quality of water volatility organic matter of claim 1, characterized by: the nine-hole valve (12) is connected with a distilled water bottle (110) and a waste liquid bottle (111), and the distilled water bottle (110) and the waste liquid bottle (111) are respectively used for cleaning the purging pipe (13) and storing the cleaned waste liquid.
4. The real-time measurement all-in-one of quality of water volatility organic matter of claim 1, characterized by: and a flow valve (28) and an electromagnetic valve (29) are arranged on the drying pipeline (26).
5. The real-time measurement all-in-one of quality of water volatility organic matter of claim 1, characterized by: valves are arranged at two ends of the heating device (32), and when the valves are closed, the heating device (32) is triggered to start heating the trapping device (31).
6. The real-time measurement all-in-one of quality of water volatility organic matter of claim 1, characterized by: the heating device (32) can heat the trapping device (31) to 100-200 ℃.
CN201921501276.2U 2019-09-10 2019-09-10 Real-time measurement all-in-one of quality of water volatility organic matter Active CN210572144U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110426480A (en) * 2019-09-10 2019-11-08 中绿环保科技股份有限公司 A kind of real time on-line monitoring equipment of water quality volatile organic matter

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110426480A (en) * 2019-09-10 2019-11-08 中绿环保科技股份有限公司 A kind of real time on-line monitoring equipment of water quality volatile organic matter

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