CN112033787A - Enrichment equipment for VOCs on-line monitoring, VOCs analysis system and method - Google Patents
Enrichment equipment for VOCs on-line monitoring, VOCs analysis system and method Download PDFInfo
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/405—Concentrating samples by adsorption or absorption
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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- G01N33/0004—Gaseous mixtures, e.g. polluted air
- G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
- G01N33/0027—General constructional details of gas analysers, e.g. portable test equipment concerning the detector
- G01N33/0036—General constructional details of gas analysers, e.g. portable test equipment concerning the detector specially adapted to detect a particular component
- G01N33/0047—Organic compounds
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/40—Concentrating samples
- G01N1/4022—Concentrating samples by thermal techniques; Phase changes
- G01N2001/4033—Concentrating samples by thermal techniques; Phase changes sample concentrated on a cold spot, e.g. condensation or distillation
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Abstract
The invention provides enrichment equipment, a VOCs analysis system and a method for VOCs online monitoring, and relates to air quality detection, wherein the enrichment equipment is applied to a VOCs analyzer and comprises the following components: the device comprises a water removal device, an enrichment device, flow control equipment and a high-temperature valve box; the input end of the flow control device is respectively connected with the sample gas inlet, the high-temperature valve box and the activated gas inlet; the output end of the flow control equipment is connected with the water removal device, the sample gas outlet and the high-temperature valve box; the two ends of the enrichment device are respectively connected with the high-temperature valve box. The gas to be detected is pretreated through the dewatering device and the enrichment device in the enrichment equipment, and finally input into the VOCs analyzer through the flow control equipment and the high-temperature valve box to complete detection, so that the detection limit of target pollutants of the gas to be detected is effectively improved, and the analysis precision is improved.
Description
Technical Field
The invention relates to the field of air quality detection, in particular to enrichment equipment for VOCs online monitoring, a VOCs analysis system and a VOCs analysis method.
Background
VOCs (Volatile Organic Compounds) have a great impact on environmental safety and are harmful to human health, and therefore, detection and treatment of VOCs generated in industrial activities and daily life are required. The composition of a sample matrix collected during the existing VOCs monitoring is complex, the concentration of target pollutants is generally low, and the analysis is directly carried out without any pretreatment, so that the analysis result error is large.
Disclosure of Invention
In view of the above, the present invention provides an enrichment device, a system and a method for analyzing VOCs for online monitoring of VOCs, wherein a gas to be detected is pretreated by a water removal device and an enrichment device in the enrichment device, and finally input into a VOCs analyzer through a high temperature valve box to complete detection, and for the gas to be detected with low target pollutant concentration, a process from low temperature enrichment to thermal desorption is completed through the water removal device, the enrichment device and the high temperature valve box, so that the detection limit of the target pollutants in the gas to be detected is effectively increased, and the analysis accuracy is improved.
In a first aspect, an embodiment of the present invention provides an enrichment device for online monitoring of VOCs, where the enrichment device is applied to a VOCs analyzer, and the enrichment device includes: the device comprises a water removal device, an enrichment device, flow control equipment and a high-temperature valve box;
the input end of the flow control device is respectively connected with the sample gas inlet, the high-temperature valve box and the activated gas inlet; the output end of the flow control equipment is connected with the water removal device, the sample gas outlet and the high-temperature valve box; two ends of the enrichment device are respectively connected with the high-temperature valve box;
the flow control equipment is used for controlling the initial sample gas transmitted to the water removal device through the sample gas inlet and controlling the gas flow of the activated gas inlet flowing into the enrichment device;
a water removal device for removing water vapor in the initial sample gas to obtain a gas containing CO2And a first sample gas of the VOCs component and passing the first sample gas to an enrichment device;
the enrichment device is used for carrying out enrichment and removal treatment on the first sample gas and removing carbon dioxide in the first sample gas to obtain a second sample gas;
and the high-temperature valve box is used for heating the second sample gas so as to transmit the heated second sample gas to the VOCs analyzer for detection.
In some embodiments, the flow control apparatus comprises: at least one flow stabilizer valve and at least one electronic flow sensor; wherein, the flow stabilizing valve is arranged at the sample gas inlet and the activated gas inlet; the electronic flow sensor is arranged at the sample gas outlet.
In some embodiments, a glass bead filled cold trap tube is arranged in the water removal device; the refrigeration temperature range of the cold trap pipe is as follows: 0 to-30 degrees celsius.
In some embodiments, a cold trap tube containing a plurality of adsorbents is disposed within the enrichment device.
In some embodiments, the high temperature valve box comprises a plurality of multi-way valves inside, and each multi-way valve is used for switching the working state of the enrichment equipment;
the bottom of high temperature valve box is provided with the hot plate, and the hot plate is arranged in heating the second appearance gas that contains in the multi-ported valve that is located hot plate department.
In some embodiments, when the communication mode of the plurality of multi-way valves is a sample gas enrichment mode, the input end of the enrichment device is connected with the sample gas inlet through the plurality of multi-way valves, and the output end of the enrichment device is connected with the sample gas outlet through the plurality of multi-way valves;
when the communication mode of the multi-way valves is a flash evaporation and desorption mode, the input end of the enrichment device is connected with the chromatographic sample inlet through the multi-way valves, and the output end of the enrichment device is connected with the chromatographic carrier gas outlet through the multi-way valves;
when the intercommunication mode of a plurality of multi-ported valves is activation and interval mode, the input of enrichment device is connected with the tail gas export through a plurality of multi-ported valves, and the output of enrichment device is connected with the activated gas import through a plurality of multi-ported valves.
In some embodiments, the plurality of multi-way valves comprises: 1 six-way valve and 3 three-way valves; the first three-way valve and the second three-way valve in the three-way valves are positioned at the bottom of the high-temperature valve box; the six-way valve and the third three-way valve are positioned at the top of the high-temperature valve box.
In some embodiments, the operating conditions of the enrichment device include a sample gas enrichment mode, a flash desorption mode, and an activation interval mode;
wherein, under the sample gas enrichment mode, the chromatographic sample inlet is connected with the chromatographic carrier gas outlet through a second three-way valve; the first sample gas enters an enrichment device through a six-way valve;
in a flash desorption mode, the chromatographic sample inlet and the chromatographic carrier gas outlet are connected through a third three-way valve, a six-way valve, an enrichment device, a first three-way valve and a second three-way valve in sequence; the enrichment device heats the second sample gas, and the heated second sample gas is reversely input to the chromatographic sample inlet for VOCs analysis;
in the activation interval mode, an activated gas inlet and a tail gas outlet are connected through a first three-way valve, a six-way valve, an enrichment device and a third three-way valve in sequence; the chromatographic sample inlet and the chromatographic carrier gas outlet are connected through a second three-way valve.
In a second aspect, an embodiment of the present invention provides a system for analyzing VOCs, including: enrichment equipment for online monitoring of VOCs and a VOCs analyzer as mentioned in the first aspect;
the enrichment equipment is used for enriching the sample gas containing the VOCs components;
and the VOCs analyzer is used for analyzing the enriched sample gas to obtain a VOCs analysis result of the sample gas.
In a third aspect, an embodiment of the present invention further provides a method for analyzing VOCs, where the method is applied to the system for analyzing VOCs mentioned in the second aspect, and the method includes:
inputting a sample gas containing the VOCs components into an enrichment device; wherein, the enrichment equipment is the enrichment equipment for online monitoring of VOCs mentioned in the first aspect;
according to the working mode of enrichment equipment, enriching and concentrating the VOCs sample gas; the working modes comprise a sample gas enrichment mode, a flash desorption mode and an activation interval mode;
and inputting the VOCs sample gas after enrichment and concentration into a VOCs analyzer for analysis to obtain the analysis result of the VOCs.
The embodiment of the invention has the following beneficial effects:
the invention providesThe utility model provides an enrichment equipment, VOCs analytic system and method for VOCs on-line monitoring, this enrichment equipment is applied to the VOCs analysis appearance, includes: the device comprises a water removal device, an enrichment device, flow control equipment and a high-temperature valve box; the input end of the flow control device is respectively connected with the sample gas inlet, the high-temperature valve box and the activated gas inlet; the output end of the flow control equipment is connected with the water removal device, the sample gas outlet and the high-temperature valve box; two ends of the enrichment device are respectively connected with the high-temperature valve box; and the flow control equipment is used for controlling the initial sample gas transmitted to the water removal device through the sample gas inlet and controlling the gas flow of the activated gas inlet flowing into the enrichment device. Wherein the water removing device is used for removing water vapor in the initial sample gas to obtain the product containing CO2And a first sample gas of the VOCs component and passing the first sample gas to an enrichment device; the enrichment device is used for carrying out enrichment and removal treatment on the first sample gas and removing carbon dioxide in the first sample gas to obtain a second sample gas; and the high-temperature valve box is used for heating the second sample gas so as to transmit the heated second sample gas to the VOCs analyzer for detection. Treat through dewatering device, the enrichment device in the enrichment equipment and detect gas preliminary treatment to accomplish the detection in finally inputing to the VOCs analysis appearance through the high temperature valve case, to the lower gas that waits to detect of target pollutant concentration, accomplished from low temperature enrichment to heat absorption's process through dewatering device, enrichment device and high temperature valve case, effectively promoted the detection limit of waiting to detect the target pollutant of gaseous, promoted analytical accuracy.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by the practice of the invention as set forth above.
In order to make the aforementioned and other objects, features and advantages of the present invention comprehensible, preferred embodiments accompanied with figures are described in detail below.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
Fig. 1 is a schematic structural diagram of an enrichment apparatus for online monitoring of VOCs according to an embodiment of the present invention;
FIG. 2 is a schematic structural diagram of another enrichment facility for online monitoring of VOCs according to an embodiment of the present invention;
fig. 3 is a schematic structural diagram of enrichment equipment in a flash desorption mode according to an embodiment of the present invention;
FIG. 4 is a schematic diagram of an enrichment apparatus in an activation interval mode according to an embodiment of the present invention;
fig. 5 is a schematic structural diagram of a system for analyzing VOCs according to an embodiment of the present invention;
fig. 6 is a flowchart of a method for analyzing VOCs according to an embodiment of the present invention.
Icon:
10-a water removal device; 20-an enrichment device; 30-a flow control device; 40-high temperature valve box; 31-a first ballast valve; 32-a second ballast valve; 33-an electronic flow sensor; 41-a first three-way valve; 42-a second three-way valve; 43-a third three-way valve; 44-a six-way valve; 51-sample gas inlet; 52-sample gas outlet; 53-activated gas inlet; 54-a tail gas outlet; 55-a chromatographic sample inlet; 56-chromatographic carrier gas outlet; 100-an enrichment facility; 200-VOCs analyzer.
Detailed Description
To make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings, and it is apparent that the described embodiments are some, but not all embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Along with urbanization and industrializationThe process is accelerated, the energy consumption and the production of industrial by-products are rapidly increased, and the high intensity of industrial activities and extensive production methods result in the emission of large amounts of VOCs. Various VOCs have strong toxicity and carcinogenicity and directly harm human health; under the condition of ultraviolet irradiation, VOCs and NOx generate photochemical reaction to generate O3The oxidability of the atmosphere is enhanced; VOCs are also one of the important prerequisites of secondary organic aerosols, aromatic hydrocarbons are the main substances for generating the secondary aerosols, and VOCs are converted to O3And the catalyst participates in atmospheric chemical reaction again to generate sulfate and nitrate, so that the generation of secondary organic aerosol is further promoted, the atmospheric environment is damaged, and the human health is harmed. Therefore, in order to improve the quality of the ambient air, the analysis and treatment of VOCs have been carried out in the prior art. However, in the specific implementation process, because the composition of the sample matrix collected during the monitoring of the existing VOCs is complex, the concentration of the target pollutant is generally low, and the analysis is directly performed without any pretreatment, the analysis result has a large error.
Based on this, the embodiment of the invention provides an enrichment device, a system and a method for analyzing VOCs, which are used for online monitoring of VOCs, wherein gases to be detected can be pretreated through a water removal device and an enrichment device in the enrichment device, and finally the gases are input into a VOCs analyzer through a high-temperature valve box to complete detection, and for the gases to be detected with low target pollutant concentration, the processes from low-temperature enrichment to heat absorption are completed through the water removal device, the enrichment device and the high-temperature valve box, so that the detection limit of the target pollutants in the gases to be detected is effectively improved, and the analysis precision is improved.
For the convenience of understanding of the present embodiment, a detailed description will be given to an enrichment facility for online monitoring of VOCs disclosed in the present embodiment.
Referring to fig. 1, an enrichment apparatus for online monitoring of VOCs, which is applied to a VOCs analyzer, includes: a water removal device 10, an enrichment device 20, a flow control apparatus 30, and a high temperature valve box 40.
The input end of the flow control device 30 is connected with the sample gas inlet 51, the high-temperature valve box 40 and the activated gas inlet 53 respectively; the output end of the flow control device 30 is connected with the water removal device 10, the sample gas outlet 52 and the high-temperature valve box 40; both ends of the enrichment device 20 are respectively connected with the high temperature valve box 40.
The sample gas inlet 51 is a gas inlet channel for the initial sample gas, and the whole analysis process is started after the initial sample gas to be detected and analyzed passes through the sample gas inlet 51; the sample gas outlet 52 is an exhaust passage for the removal of the sample gas; the activation gas inlet 53 is an inlet passage for activation, and activation gas is supplied through the activation gas inlet 53 for activation when VOCs are analyzed.
A flow control device 30 for controlling the initial sample gas delivered to the water removal device 10 through the sample gas inlet 51 and controlling the flow of the gas flowing into the enrichment device 20 through the activation gas inlet 53.
A water removal device 10 for removing water vapor in the initial sample gas to obtain a gas containing CO2And a first sample gas of the VOCs components and delivering the first sample gas to the enrichment device 20. As can be seen, the first sample gas is the initial sample gas from which the water vapor is removed.
And the enrichment device 20 is used for enriching and removing the first sample gas, and simultaneously removing carbon dioxide in the first sample gas to obtain a second sample gas. The second sample gas is the first sample gas from which carbon dioxide has been removed.
And the high-temperature valve box 40 is used for heating the second sample gas so as to transmit the heated second sample gas to the VOCs analyzer for detection. The heated second sample gas enters chromatographic equipment of the VOCs analyzer through a chromatographic sample inlet 55 for chromatographic analysis to obtain an analysis result of VOCs; in this process, a chromatographic carrier gas outlet 56 is required to provide carrier gas to push the initial sample gas to be measured to finally flow into the chromatographic sample inlet 55, and the related tail gas is discharged through the tail gas outlet 54.
As can be seen from the enrichment device for online monitoring of VOCs mentioned in this embodiment, the enrichment device may pre-process the gas to be detected through the built-in water removal device and enrichment device, and finally input the gas to the VOCs analyzer through the flow control device and the high temperature valve box to complete the detection. For the gas to be detected with low target pollutant concentration, the process from low-temperature enrichment to heat absorption can be completed through the dewatering device, the enrichment device and the high-temperature valve box, the detection limit of the target pollutant of the gas to be detected is effectively improved, and the analysis precision is improved.
In some embodiments, the flow control apparatus comprises: at least one flow stabilizer valve and at least one electronic flow sensor; wherein, the flow stabilizing valve is arranged at the sample gas inlet and the activated gas inlet; the electronic flow sensor is arranged at the sample gas outlet. The flow stabilizing valve and the electronic flow sensor are controlled through embedded software, flow control of the sample gas circuit is carried out through a series combination mode of the flow stabilizing valve and the electronic flow sensor, the stability of the sample gas flow is improved through double control, the flow control of the activation gas circuit is carried out through the flow stabilizing valve, and the activated gas flow is stably and reversely cleaned through the enrichment device.
In some embodiments, a glass bead filled cold trap tube is arranged in the water removal device; the refrigeration temperature range of the cold trap pipe is as follows: 0 to-30 degrees celsius.
In some embodiments, a cold trap tube containing a plurality of adsorbents is disposed within the enrichment device.
In some embodiments, the high temperature valve box comprises a plurality of multi-way valves inside, and each multi-way valve is used for switching the working state of the enrichment equipment; the bottom of high temperature valve box is provided with the hot plate, and the hot plate is arranged in heating the second appearance gas that contains in the multi-ported valve that is located hot plate department.
In some embodiments, when the communication mode of the plurality of multi-way valves is a sample gas enrichment mode, the input end of the enrichment device is connected with the sample gas inlet through the plurality of multi-way valves, and the output end of the enrichment device is connected with the sample gas outlet through the plurality of multi-way valves;
when the communication mode of the multi-way valves is a flash evaporation and desorption mode, the input end of the enrichment device is connected with the chromatographic sample inlet through the multi-way valves, and the output end of the enrichment device is connected with the chromatographic carrier gas outlet through the multi-way valves;
when the intercommunication mode of a plurality of multi-ported valves is activation and interval mode, the input of enrichment device is connected with the tail gas export through a plurality of multi-ported valves, and the output of enrichment device is connected with the activated gas import through a plurality of multi-ported valves.
The enrichment facility of the above embodiment is described with reference to another enrichment facility for online monitoring of VOCs shown in fig. 2. The plurality of multi-way valves of the enrichment apparatus shown in fig. 2 comprises: 1 six-way valve and 3 three-way valves; wherein, a first three-way valve 41 and a second three-way valve 42 of the three-way valves are positioned at the bottom of the high-temperature valve box 40; a six-way valve 44 and a third three-way valve 43 are located at the top of the high temperature valve box 40.
A three-stage refrigeration sheet is arranged in the dewatering device; wherein, a cold trap pipe filled with glass beads is arranged in the dewatering module, and the size of the cold trap pipe is as follows
The refrigerating temperature range of the refrigerating sheet is as follows: and (3) enriching the water vapor in the initial sample gas in a water removal device through low temperature at the temperature of between 0 and minus 30 ℃.
The bottom of high temperature valve box is provided with the hot plate, and the hot plate is arranged in heating the second sample gas that contains in the multi-way valve that is located hot plate department, and heatable reaches 120 ℃, guarantees that the sample gas that "flash distillation" came out passes through each gas circuit in the valve box at high temperature.
The enrichment device is refrigerated by the three-stage refrigeration piece, the temperature in the device can be reduced to minus 30 ℃, and the device is internally provided with
The cold trap tube of (1) is filled with a carbon C with the length of 13mm, a carbon B with the length of 25mm and a carbon 1000 with the length of 13 mm; the device is kept at the temperature of minus 30 ℃ for sample gas enrichment. After the enrichment is finished, the enriched sample gas is instantly gasified at the heating rate of 100 ℃/s and is carried to the inlet of an analysis instrument for sample gas analysis under the pushing of carrier gas.
The flow control apparatus described above includes: two flow stabilizing valves and an electronic flow sensor; wherein, the first flow stabilizing valve 31 is arranged at the sample gas inlet 51, and the second flow stabilizing valve 32 is arranged at the activated gas inlet 53; the electronic flow sensor 33 is disposed at the sample gas outlet 52. The first flow stabilizing valve 31, the second flow stabilizing valve 32 and the electronic flow sensor 33 are connected with the multi-way valve, and the specific connection process with the multi-way valve is controlled through embedded software according to the working state of the enrichment equipment.
Specifically, the working state of the enrichment equipment comprises a sample gas enrichment mode, a flash desorption mode and an activation interval mode.
The enrichment apparatus shown in fig. 2 is in a sample gas enrichment mode, and the chromatography sample inlet 55 and the chromatography carrier gas outlet 56 are connected by the second three-way valve 42. At this time, the sample gas at the sample gas inlet 51 sequentially passes through the first flow stabilizing valve 31 and the water removal device, enters the six-way valve 44, is enriched by the enrichment device 20, and is discharged through the sample gas outlet 52 via the six-way valve 44. At this time, the gas paths of the activated gas inlet 53, the tail gas outlet 54, the chromatography sample inlet 55 and the chromatography carrier gas outlet 56 are not communicated.
In the sample gas enrichment mode, the chromatographic sample inlet and the chromatographic carrier gas outlet are connected by a second three-way valve 42; the first sample gas enters the enrichment device 20 through a six-way valve 44. The sample gas is subjected to flow control through the first flow stabilizing valve 31 and enters the water removal device 10 at a constant flow rate, the water removal device 10 enriches water vapor in a solid state at a low temperature, the VOCs components are not affected and enter the high-temperature valve box 40 through the water removal device 10, then the VOCs components are converted through the six-way valve 44 and enter the enrichment device 20, and the enrichment device 20 enriches the sample gas at the low temperature; at the moment, the carrier gas controlled by the EPC in the chromatograph passes through the system and then returns to the chromatograph, and the activated gas path is not opened at the moment.
The connection relationship between the multi-way valves in the sample gas enrichment mode is shown in detail in fig. 2, and the channels in the six-way valve are respectively represented by 1, 2, 3, 4, 5 and 6; the passages in the three-way valve are indicated by 1, 2, 3, respectively.
The operation mode of the enrichment apparatus shown in fig. 3 is a flash desorption mode, and in the flash desorption mode, the chromatographic sample inlet and the chromatographic carrier gas outlet are connected sequentially through a third three-way valve 43, a six-way valve 44, the enrichment device 20, a first three-way valve 41 and a second three-way valve 42; the enrichment device 20 heats the second sample gas, and the heated second sample gas is reversely input to the chromatographic sample inlet 55 for VOCs analysis.
In the flash desorption mode, the water removal device 10 is heated to normal temperature, and the enriched solid water vapor is converted into gas state and is taken out of the water removal device 10 by the sample gas; the enrichment device 20 rapidly heats up to 300 ℃ at a heating rate of 100 ℃/s, the enriched VOCs are flashed out of the enrichment tube, the temperature of the flash evaporation is kept for continuous desorption, and the desorbed sample gas is reversely carried into an analysis instrument by chromatographic carrier gas for analysis; the activation gas circuit is not opened at this time.
The connection relationship between the multi-way valves in the flash desorption mode is shown in detail in fig. 3, and similarly to fig. 2, the channels in the six-way valve are respectively shown as 1, 2, 3, 4, 5 and 6; the channels in the three-way valve are respectively represented by 1, 2 and 3, and the connection relationship is not described again.
The operation mode of the enrichment facility shown in fig. 4 is an activation interval mode in which the activated gas inlet 53 and the tail gas outlet 54 are connected sequentially by the first three-way valve 41, the six-way valve 44, the enrichment device 20, and the third three-way valve 43; the chromatography sample inlet 55 and the chromatography carrier gas outlet 56 are connected by the second three-way valve 42.
In the activation mode, the sample gas is continuously drained after passing through the water removal device 10 at normal temperature, at this time, the activation gas path is introduced into the enrichment device, the enrichment pipe of the enrichment device 20 is reversely purged at the desorption temperature, the purged tail gas is drained, and at this time, the chromatographic carrier gas returns to the chromatograph after passing through the enrichment device.
Under the interval mode, the gas circuit system at this moment is unanimous under with the activation mode, and sample gas no longer is sent into enrichment facility 20 under the interval mode, cools down dewatering device 10 and enrichment facility 20 simultaneously to the preconcentration temperature that each part set for, waits for the beginning of enrichment next time.
The connection between the multi-way valves in the active interval mode is shown in detail in fig. 4, and the channels in the six-way valve are shown as 1, 2, 3, 4, 5, 6, respectively, similar to fig. 2 and 3; the channels in the three-way valve are respectively represented by 1, 2 and 3, and the connection relationship is not described again.
The temperature of the enrichment device 20 is reduced by adopting a semiconductor refrigeration technology in the temperature reduction process; the refrigerating piece is small in size, small in required space and convenient to install, and temperature control can be performed through an embedded program. The working principle of a semiconductor cooler is based on the peltier principle, i.e. when a circuit consisting of two different conductors a and B is energized with direct current, some other heat is released in addition to joule heat at the junction, while the other junction absorbs heat, and this phenomenon caused by the peltier effect is reversible, with the change of the direction of the current, the junction which releases and absorbs heat also changing.
In the low-temperature enrichment process, the adsorption performance of activated carbon is utilized, C2-C18 compounds are subjected to low-temperature enrichment by adopting a three-combination mode of Carbopack C, Carbopack B and Carboxen 1000, samples are enriched and concentrated at the enrichment temperature of minus 30 ℃, and the detection limit is improved on the premise of not modifying an analysis device.
In a second aspect, an embodiment of the present invention provides a system for analyzing VOCs, a schematic structural diagram of which is shown in fig. 5, where the system includes: the enrichment device 100 for online monitoring of VOCs and the VOCs analyzer 200 as mentioned in the first aspect;
the enrichment device 100 is used for enriching a sample gas containing VOCs components; the relevant technical parameters of the enrichment facility 100 are as follows:
temperature of the water removal device: 0 ℃;
temperature of the enrichment device: -30 ℃;
temperature of the high-temperature valve box: 120 ℃;
temperature of chromatographic sample introduction pipeline: 120 ℃;
temperature rise rate of the enrichment device: not less than 100 ℃/s;
the refrigeration technology comprises the following steps: and (5) refrigerating by using a semiconductor.
The VOCs analyzer 200 is configured to analyze the enriched sample gas to obtain a VOCs analysis result of the sample gas.
The enrichment equipment for online monitoring of the VOCs in the embodiment has the same technical characteristics as the enrichment equipment for online monitoring of the VOCs provided in the above method embodiment, so that the same technical problems can be solved, and the same technical effects can be achieved. For the sake of brevity, where not mentioned in the examples section, reference may be made to the corresponding matter in the preceding method examples.
In a third aspect, an embodiment of the present invention further provides a method for analyzing VOCs, where the method is applied to the system for analyzing VOCs mentioned in the second aspect, and as shown in fig. 6, the method includes:
step S601, inputting a sample gas containing the VOCs components into an enrichment facility.
The enrichment equipment is used for VOCs on-line monitoring mentioned in the embodiment, and the sample gas is input into the enrichment equipment through the sample gas inlet and the flow stabilizing valve and the water removal device in sequence.
Step S602, according to the working mode of enrichment equipment, enriching and concentrating the VOCs sample gas; the working modes comprise a sample gas enrichment mode, a flash desorption mode and an activation interval mode.
The water removal device is cooled to the pre-concentration temperature sequentially through the three modes, and the atmospheric sample enters the water removal device at a constant flow rate under the condition of mass flow control. The cold trap in the water removal device is filled with glass beads, water vapor is enriched in the water removal device in a solid state, and most of VOCs components pass through the water removal device without being affected (the water vapor is removed by freezing the water removal device to 0 ℃).
The enrichment device is cooled to the pre-concentration temperature, the gas passing through the water removal device enters the enrichment device, adsorbents in a three-combination mode of Carbopack B, Carbopack C and Carboxen 1000 are arranged in the enrichment device, VOCs components are completely adsorbed, and at the moment, gaseous CO2 is taken out of the system, so that CO2 is removed.
The enrichment device is rapidly heated to 300 ℃, the trapped compounds are instantaneously gasified, and the compounds are transferred to an analysis instrument for analysis in a flash evaporation mode.
And step S603, inputting the VOCs sample gas after enrichment and concentration into a VOCs analyzer for analysis to obtain the analysis result of the VOCs.
After the sample with lower concentration of the target pollutant is subjected to low-temperature enrichment-thermal desorption, the detection limit of the target pollutant can be effectively improved, and meanwhile, the interference of a matrix on the measurement can be eliminated. On the premise of not changing the analyzer, the detection limit of the target compound is effectively improved by pretreating the sample gas.
The VOCs analysis system in this embodiment has the same technical features as the VOCs analysis system provided in the above method embodiment, so that the same technical problems can be solved, and the same technical effects can be achieved. For the sake of brevity, where not mentioned in the examples section, reference may be made to the corresponding matter in the preceding method examples.
In the several embodiments provided in the present application, it should be understood that the disclosed system, apparatus, and method may be implemented in other ways. The above-described embodiments of the apparatus are merely illustrative, and for example, the division of the units is only one logical division, and there may be other divisions when actually implemented, and for example, a plurality of units or components may be combined or integrated into another system, or some features may be omitted, or not executed. In addition, the shown or discussed mutual coupling or direct coupling or communication connection may be an indirect coupling or communication connection of devices or units through some communication interfaces, and may be in an electrical, mechanical or other form.
The units described as separate parts may or may not be physically separate, and parts displayed as units may or may not be physical units, may be located in one place, or may be distributed on a plurality of network units. Some or all of the units can be selected according to actual needs to achieve the purpose of the solution of the embodiment.
In addition, functional units in the embodiments of the present invention may be integrated into one processing unit, or each unit may exist alone physically, or two or more units are integrated into one unit.
The functions, if implemented in the form of software functional units and sold or used as a stand-alone product, may be stored in a non-volatile computer-readable storage medium executable by a processor. Based on such understanding, the technical solution of the present invention or a part thereof, which essentially contributes to the prior art, can be embodied in the form of a software product stored in a storage medium and including instructions for causing a computer device (which may be a personal computer, a server, or a network device) to execute all or part of the steps of the method according to the embodiments of the present invention. And the aforementioned storage medium includes: a U-disk, a removable hard disk, a Read-Only Memory (ROM), a Random Access Memory (RAM), a magnetic disk or an optical disk, and other various media capable of storing program codes.
Finally, it should be noted that: the above-mentioned embodiments are only specific embodiments of the present invention, which are used for illustrating the technical solutions of the present invention and not for limiting the same, and the protection scope of the present invention is not limited thereto, although the present invention is described in detail with reference to the foregoing embodiments, those skilled in the art should understand that: any person skilled in the art can modify or easily conceive the technical solutions described in the foregoing embodiments or equivalent substitutes for some technical features within the technical scope of the present disclosure; such modifications, changes or substitutions do not depart from the spirit and scope of the embodiments of the present invention, and they should be construed as being included therein. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (10)
1. An enrichment device for online monitoring of VOCs, the enrichment device being applied to a VOCs analyzer, the enrichment device comprising: the device comprises a water removal device, an enrichment device, flow control equipment and a high-temperature valve box;
the input end of the flow control device is respectively connected with the sample gas inlet, the high-temperature valve box and the activated gas inlet; the output end of the flow control equipment is connected with the water removal device, the sample gas outlet and the high-temperature valve box; two ends of the enrichment device are respectively connected with the high-temperature valve box;
the flow control device is used for controlling the initial sample gas transmitted to the water removal device through the sample gas inlet and controlling the gas flow of the activated gas inlet flowing into the enrichment device;
the water removal device is used for removing water vapor in the initial sample gas to obtain the gas containing CO2And a first sample gas of the VOCs component and passing the first sample gas to the enrichment device;
the enrichment device is used for carrying out enrichment and removal treatment on the first sample gas and removing carbon dioxide in the first sample gas to obtain a second sample gas;
and the high-temperature valve box is used for heating the second sample gas so as to transmit the heated second sample gas to the VOCs analyzer for detection.
2. The enrichment apparatus of claim 1, wherein the flow control apparatus comprises: at least one flow stabilizer valve and at least one electronic flow sensor; the flow stabilizing valve is arranged at the sample gas inlet and the activated gas inlet; the electronic flow sensor is arranged at the sample gas outlet.
3. The enrichment apparatus of claim 1, wherein a glass bead filled cold trap is provided within the water removal device; the refrigeration temperature range of the cold trap pipe is as follows: 0 to-30 degrees celsius.
4. The enrichment apparatus of claim 1, wherein a cold trap tube containing a plurality of adsorbents is disposed within the enrichment device.
5. The enrichment apparatus of claim 1, wherein the interior of the high temperature valve box contains a plurality of multi-way valves, each for switching the operating state of the enrichment apparatus;
the bottom of high temperature valve case is provided with the hot plate, the hot plate is used for to being located the multi-ported valve of hot plate department contains the second sample gas heats.
6. The enrichment apparatus of claim 5,
when the communication mode of the multi-way valves is a sample gas enrichment mode, the input end of the enrichment device is connected with the sample gas inlet through the multi-way valves, and the output end of the enrichment device is connected with the sample gas outlet through the multi-way valves;
when the communication mode of the multi-way valves is a flash evaporation and desorption mode, the input end of the enrichment device is connected with the chromatographic sample inlet through the multi-way valves, and the output end of the enrichment device is connected with the chromatographic carrier gas outlet through the multi-way valves;
when the communication mode of the multi-way valves is the activation and interval mode, the input end of the enrichment device is connected with the tail gas outlet through the multi-way valves, and the output end of the enrichment device is connected with the activated gas inlet through the multi-way valves.
7. The enrichment apparatus of claim 6, wherein the plurality of multi-way valves comprises: 1 six-way valve and 3 three-way valves; wherein a first three-way valve and a second three-way valve of the three-way valves are located at the bottom of the high-temperature valve box; the six-way valve and the third three-way valve are positioned at the top of the high-temperature valve box.
8. The enrichment apparatus of claim 7, wherein the operational state of the enrichment apparatus comprises a sample gas enrichment mode, a flash desorption mode, and an activation interval mode;
wherein, in the sample gas enrichment mode, the chromatographic sample inlet and the chromatographic carrier gas outlet are connected through the second three-way valve; the first sample gas enters the enrichment device through the six-way valve;
in a flash desorption mode, the chromatographic sample inlet and the chromatographic carrier gas outlet are connected through the third three-way valve, the six-way valve, the enrichment device, the first three-way valve and the second three-way valve in sequence; the enrichment device heats the second sample gas, and the heated second sample gas is reversely input to the chromatographic sample inlet for VOCs analysis;
in the activation interval mode, the activation gas inlet and the tail gas outlet are connected sequentially through the first three-way valve, the six-way valve, the enrichment device and the third three-way valve; the chromatogram injection port and the chromatogram carrier gas outlet are connected through the second three-way valve.
9. A system for analyzing VOCs, the system comprising: the enrichment device and VOCs analyzer for online monitoring of VOCs of any of claims 1 to 8;
the enrichment equipment is used for enriching sample gas containing VOCs components;
and the VOCs analyzer is used for analyzing the enriched sample gas to obtain a VOCs analysis result of the sample gas.
10. A method for analyzing VOCs, the method being applied to the system for analyzing VOCs according to claim 9, the method comprising:
inputting a sample gas containing the VOCs components into an enrichment device; wherein the enrichment facility is the enrichment facility for online monitoring of VOCs according to any one of claims 1 to 8;
according to the working mode of the enrichment equipment, enriching and concentrating the VOCs sample gas; the working modes comprise a sample gas enrichment mode, a flash desorption mode and an activation interval mode;
and inputting the VOCs sample gas after enrichment and concentration into a VOCs analyzer for analysis to obtain the analysis result of VOCs.
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