CN109444009B - On-line direct test equipment for benzopyrene in atmospheric environment - Google Patents
On-line direct test equipment for benzopyrene in atmospheric environment Download PDFInfo
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- CN109444009B CN109444009B CN201811505337.2A CN201811505337A CN109444009B CN 109444009 B CN109444009 B CN 109444009B CN 201811505337 A CN201811505337 A CN 201811505337A CN 109444009 B CN109444009 B CN 109444009B
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- conical flask
- air duct
- switch
- front air
- tube
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- FMMWHPNWAFZXNH-UHFFFAOYSA-N Benz[a]pyrene Chemical compound C1=C2C3=CC=CC=C3C=C(C=C3)C2=C2C3=CC=CC2=C1 FMMWHPNWAFZXNH-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 238000012360 testing method Methods 0.000 title description 9
- 238000005070 sampling Methods 0.000 claims abstract description 38
- 239000012528 membrane Substances 0.000 claims abstract description 22
- 239000003365 glass fiber Substances 0.000 claims abstract description 20
- 238000005259 measurement Methods 0.000 claims abstract description 18
- 238000001802 infusion Methods 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims description 24
- 238000007789 sealing Methods 0.000 claims description 3
- 238000004458 analytical method Methods 0.000 abstract description 8
- 239000002245 particle Substances 0.000 abstract description 8
- 238000000034 method Methods 0.000 abstract description 5
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 9
- 239000010419 fine particle Substances 0.000 description 6
- 238000001514 detection method Methods 0.000 description 3
- 239000000443 aerosol Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 210000003491 skin Anatomy 0.000 description 2
- 206010028980 Neoplasm Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 230000000295 complement effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 210000001035 gastrointestinal tract Anatomy 0.000 description 1
- 210000000987 immune system Anatomy 0.000 description 1
- 230000003116 impacting effect Effects 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 210000004072 lung Anatomy 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000002503 metabolic effect Effects 0.000 description 1
- 239000013618 particulate matter Substances 0.000 description 1
- 210000004994 reproductive system Anatomy 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N15/00—Investigating characteristics of particles; Investigating permeability, pore-volume, or surface-area of porous materials
- G01N15/06—Investigating concentration of particle suspensions
- G01N15/0606—Investigating concentration of particle suspensions by collecting particles on a support
- G01N15/0618—Investigating concentration of particle suspensions by collecting particles on a support of the filter type
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/2273—Atmospheric sampling
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/24—Suction devices
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/08—Preparation using an enricher
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
Abstract
The invention discloses on-line direct measurement equipment for benzopyrene in an atmospheric environment, which comprises a sampling port, a sampling tube, a front air duct, a water vapor filter element, a vacuum pump and a flowmeter; the sampling port is communicated with a sampling tube, and the sampling tube is communicated with the first end of the front air duct; the water vapor filter element, the vacuum pump and the flowmeter are arranged in the front air guide pipeline; the device also comprises a first switch, a conical flask, a glass fiber filter membrane, a separating funnel, a rear air duct, an ultrasonic extractor, a transfusion tube, a second switch, a diaphragm pump, a filter and a sample bottle; the glass fiber filter membrane is arranged in the conical flask; the first switch is arranged in a pipeline of the front air duct; the rear air duct communicates the interior of the conical flask with the external atmosphere; the ultrasonic extractor is arranged outside the conical flask; the first end of the infusion tube is inserted into the conical flask, and the second end is connected with the sample bottle. By utilizing the method, online continuous automatic sampling and direct measurement analysis of benzopyrene particles are realized, so that the measured concentration value is more accurate and effective.
Description
Technical Field
The invention relates to an online detection technology of benzopyrene, in particular to online direct detection equipment of benzopyrene in an atmospheric environment.
Background
Benzopyrene can be combined with particles in the atmosphere to form aerosol, and is absorbed by human body through skin, respiratory tract, digestive tract and the like, and metabolic activation products in the human body can cause tumors at liver, skin, lung and other parts, so that the benzopyrene has certain toxicity to reproductive system and immune system, and has important significance for accurately detecting the content of the benzopyrene.
The traditional fine particulate matter sampling device measures the flow rate of gas through a self-contained flowmeter, the flow rate is displayed through a floater of the flowmeter, a filter membrane in a filter membrane sampler can complement particulate matters in air, a collected filter membrane sample is put into a sample bottle for solvent extraction and then a subsequent experiment is carried out, and if the distance is far, the sample is required to be refrigerated and stored and is brought back to a laboratory for analysis, and the method is commonly called an off-line sampling analysis method. The method has long sampling time, mainly analyzes the collected sample for a time interval, inevitably contacts air during the time interval, if the sample is required to be stored and transported for a long distance, the chemical components of the fine particles are more easily destroyed, and the analysis sample is greatly affected by human factors and takes manpower and material resources, so that the off-line sampling analysis method is more and more difficult to meet the requirements of the observation and research of the fine particles. The development of new on-line aerosol particle sampling and analysis devices and methods has become critical to atmospheric particulate research.
Disclosure of Invention
The invention aims to provide online direct test equipment for benzopyrene in an atmospheric environment, so as to solve the problems in the prior art and improve the test efficiency and accuracy.
The invention provides online direct measurement equipment of benzopyrene in an atmospheric environment, which comprises a sample acquisition module and a pretreatment module;
the sample collection module comprises a sampling port, a sampling tube, a front air duct, a water vapor filter element, a vacuum pump and a flowmeter; the sampling port is communicated with the sampling tube, and the sampling tube is communicated with the first end of the front air duct; the water vapor filter element, the vacuum pump and the flowmeter are all arranged in the pipeline of the front air duct;
the pretreatment module comprises a first switch, a conical flask, a glass fiber filter membrane, a separating funnel, a rear air duct, an ultrasonic extractor, a transfusion tube, a second switch, a diaphragm pump, a filter and a sample bottle; the glass fiber filter membrane is arranged in the conical flask; the separating funnel is used for adding an extracting solution into the conical flask; the first switch is arranged in a pipeline of the front air duct, and the second end of the front air duct is inserted below the liquid level in the conical flask and above the glass fiber filter membrane; the rear air duct communicates the interior of the conical flask with the external atmosphere; the ultrasonic extractor is arranged outside the conical flask; the first end of the infusion tube is inserted below the liquid level in the conical flask, and the second end of the infusion tube is connected with the sample bottle; the second switch, the diaphragm pump and the filter are all arranged in the pipeline of the infusion tube.
Preferably, the bottle mouth of the conical flask is provided with a rubber plug for sealing, and the front air guide pipe, the rear air guide pipe and the infusion tube are inserted into the conical flask through holes formed in the rubber plug.
Preferably, the separating funnel has a liquid outlet pipe which is inserted into the conical flask through a hole opened in the rubber plug.
Preferably, a third switch is arranged on the liquid outlet pipe.
Preferably, the second end of the leading airway is provided with a dilator.
Preferably, the flaring device is horn-shaped.
Preferably, a fourth switch is arranged on the rear air duct.
The on-line direct measurement device provided by the invention has a simple structure, the collected sample particles are subjected to pretreatment in a closed environment, the interference of external environment and human factors is avoided, the high-efficiency capturing and conversion of fine particles are realized, the pretreatment time is saved, the interference of human factors is eliminated, the on-line direct measurement device can be directly used for continuous measurement, and the on-line continuous automatic sampling and direct measurement analysis of benzopyrene particles are realized in an automatic mode, so that the measured concentration value is more accurate and effective.
Drawings
Fig. 1 is a schematic structural diagram of an online direct measurement device for benzopyrene provided by an embodiment of the invention.
Reference numerals illustrate:
1-sampling port 2-sampling tube 3-front air guide tube 4-water vapor filter element 5-vacuum pump 6-flowmeter 7-first switch 8-conical flask 9-glass fiber filter membrane 10-separating funnel 11-rear air guide tube 12-ultrasonic extractor 13-infusion tube 14-second switch 15-diaphragm pump 16-filter 17-bottle 18-third switch 19-liquid outlet tube 20-fourth switch
Detailed Description
Embodiments of the present invention are described in detail below, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to like or similar elements or elements having like or similar functions throughout. The embodiments described below by referring to the drawings are illustrative only and are not to be construed as limiting the invention.
As shown in FIG. 1, the embodiment of the invention provides on-line direct test equipment for benzopyrene in an atmospheric environment, which comprises a sample acquisition module and a pretreatment module.
The sample collection module comprises a sampling port 1, a sampling tube 2, a front air duct 3, a water vapor filter element 4, a vacuum pump 5 and a flowmeter 6; the sampling port 1 is communicated with the sampling tube 2, and the sampling tube 2 is communicated with the first end of the front air duct 3; the water vapor filter element 4, the vacuum pump 5 and the flowmeter 6 are all arranged in the pipeline of the front air duct 3.
The pretreatment module comprises a first switch 7, a conical flask 8, a glass fiber filter membrane 9, a separating funnel 10, a rear air duct 11, an ultrasonic extractor 12, a transfusion tube 13, a second switch 14, a diaphragm pump 15, a filter 16 and a sample bottle 17; the glass fiber filter membrane 9 is arranged in the conical flask 8; the separating funnel 10 is used for adding an extracting solution into the conical flask 8; the first switch 7 is arranged in the pipeline of the front air duct 3, and the second end of the front air duct 3 is inserted below the liquid level in the conical flask 8 and above the glass fiber filter membrane 9; the rear air duct 11 communicates the interior of the conical flask 8 with the outside atmosphere; the ultrasonic extractor 12 is arranged outside the conical flask 8; a first end of the infusion tube 13 is inserted below the liquid level in the conical flask 8, and a second end of the infusion tube 13 is connected with the sample bottle 17; the second switch 14, the diaphragm pump 15 and the filter 16 are all arranged in the pipeline of the infusion tube 13.
The sampling port 1 is connected with a benzopyrene pollution source in the atmosphere, the central position of the bottom of the sampling port 1 is vertically connected with the middle part of the sampling tube 2, collected air flows pass through the front air guide pipe 3 and the water vapor filter element 4, the outlet of the water vapor filter element 4 is connected with the air inlet of the vacuum pump 5, and a flowmeter 6 is arranged on a pipeline of the air outlet of the vacuum pump 5.
Preferably, a rubber plug for sealing is arranged at the bottleneck of the conical flask 8, the rubber plug is movably connected with the bottleneck, and the front air guide pipe 3, the rear air guide pipe 11 and the infusion tube 13 are inserted into the conical flask 8 through holes formed in the rubber plug. The rubber plug has excellent heat resistance, cold resistance and atmospheric aging resistance, and has good insulativity and wear resistance.
The front air duct 3 is inserted into the conical flask 8, and preferably, a mouth expander is provided at the air outlet (second end) of the front air duct 3, and the mouth expander may be horn-shaped or may be of other shapes. The mouth expander is fixedly connected with the second end of the front air guide pipe 3, a glass fiber filter membrane 9 in the conical flask 8 is arranged right below the mouth expander, the center of the glass fiber filter membrane 9 is vertical to the center of the mouth expander, and the outlet of the mouth expander uniformly distributes collected air on the surface of the glass fiber filter membrane 9 in an impacting manner; a conduit is additionally arranged at the bottleneck of the conical flask 8 and is communicated with the atmosphere, namely a rear air duct 11, and a fourth switch 20 is arranged on the rear air duct 11. A separating funnel 10 is also arranged at the mouth of the conical flask 8, and an extraction liquid, such as acetonitrile solution, is filled in the separating funnel 10. The separating funnel 10 has a liquid outlet pipe 19, and a third switch 18 is preferably provided on the liquid outlet pipe 19. The outlet pipe 19 is inserted into the conical flask 8 through a hole made in the rubber plug.
The conical flask 8 is placed entirely inside the ultrasonic extractor 12, the liquid level of the ultrasonic extractor 12 being maintained at a level that fully submerges the liquid in the conical flask 8; the bottle mouth of the conical flask 8 is connected with a conduit through a rubber plug, namely, a transfusion tube 13 is connected to the right side, a second switch 14 is arranged on the transfusion tube 13, a micro diaphragm pump 15 is connected behind the second switch 14, and the micro diaphragm pump 15 pumps liquid to be detected; the outlet of the micro diaphragm pump 15 is connected with a replaceable filter 16 through a pipeline of the infusion tube 13, the right side of the filter 16 is connected with a sample bottle 17, and the sample bottle 17 filled with the liquid to be detected is externally connected with a sample tube of a liquid chromatograph.
The sampling port 1 can also be provided with a mouth expander, polluted gas enters the sampling tube 2 through the mouth expander of the sampling port 1 under the suction effect of the vacuum pump 5, the collected atmosphere enters the micro vacuum pump 5 after being filtered by the water vapor filter element 4, the flow meter 6 can display the flow value of the collected atmosphere, the collected atmosphere enters the conical flask 8 and is uniformly sprayed on the surface of the glass fiber filter membrane 9 at the horn-shaped mouth expander at the tail end of the front air duct 3, the enrichment of benzopyrene particles on the glass fiber filter membrane 9 is fully completed, the glass fiber filter membrane 9 is placed at the bottom in the conical flask 8, a separating funnel 10 filled with acetonitrile solution is arranged above the conical flask 8, the whole conical flask 8 device is placed in the ultrasonic extractor 12, and the benzopyrene fine particles on the glass fiber filter membrane 9 are uniformly dispersed in the extracting solution by utilizing ultrasonic waves, so that soluble components in the fine particles are rapidly dissolved in the extracting solution. The absorbed absorption liquid is sucked into the sample bottle 17 by the micro diaphragm pump 15.
The sample collection process by adopting the on-line direct test equipment is as follows:
when on-line collection measurement is needed, firstly, a switch at the front end of the micro diaphragm pump 15 is closed, a first switch 7 and a second switch 14 at the front and the rear of the conical flask 8 are opened, the micro vacuum pump 5 is started, and when the value of the flowmeter 6 reaches a stable value, the sampling starting time is recorded. After sampling for a period of time, the micro vacuum pump 5 is stopped, the first switch 7 and the second switch 14 of the conical flask 8 are closed, the rotary switch of the separating funnel 10 is opened to allow acetonitrile solution to enter the conical flask 8 to submerge glass fiber filter paper, the ultrasonic extractor 12 is started, the time, the temperature and the frequency are set, the ultrasonic extractor 12 is closed after a period of time, the ultrasonic extractor 12 is closed, the second switch 14 and the micro diaphragm pump 15 are opened, the liquid to be detected flows through the replaceable filter 16 to enter the sample bottle 17 under the suction of the micro diaphragm pump 15, and the liquid to be detected in the sample bottle 17 is introduced into the liquid chromatograph through the sample tube for detection. The rest liquid to be measured can be poured out from the mouth of the conical flask 8, and after the liquid to be measured is completely emptied, one-time enrichment measurement is completed.
The on-line direct test equipment provided by the embodiment of the invention has a simple structure, the collected sample particles are subjected to pretreatment in a closed environment, the interference of external environment and human factors is avoided, the high-efficiency capturing and conversion of fine particles are realized, the pretreatment time is saved, the interference of human factors is eliminated, the on-line direct test equipment can be directly used for continuous measurement, and the on-line continuous automatic sampling and direct test analysis of benzopyrene particles are realized in an automatic mode, so that the measured concentration value is more accurate and effective.
While the foregoing is directed to embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow.
Claims (7)
1. The on-line direct measurement equipment for benzopyrene in the atmospheric environment is characterized by comprising a sample acquisition module and a pretreatment module;
the sample collection module comprises a sampling port, a sampling tube, a front air duct, a water vapor filter element, a vacuum pump and a flowmeter; the sampling port is communicated with the sampling tube, and the sampling tube is communicated with the first end of the front air duct; the water vapor filter element, the vacuum pump and the flowmeter are all arranged in the pipeline of the front air duct;
the pretreatment module comprises a first switch, a conical flask, a glass fiber filter membrane, a separating funnel, a rear air duct, an ultrasonic extractor, a transfusion tube, a second switch, a diaphragm pump, a filter and a sample bottle; the glass fiber filter membrane is arranged in the conical flask; the separating funnel is used for adding an extracting solution into the conical flask; the first switch is arranged in a pipeline of the front air duct, and the second end of the front air duct is inserted below the liquid level in the conical flask and above the glass fiber filter membrane; the rear air duct communicates the interior of the conical flask with the external atmosphere; the ultrasonic extractor is arranged outside the conical flask; the first end of the infusion tube is inserted below the liquid level in the conical flask, and the second end of the infusion tube is connected with the sample bottle; the second switch, the diaphragm pump and the filter are all arranged in the pipeline of the infusion tube.
2. The on-line direct measurement device according to claim 1, wherein a rubber stopper for sealing is provided at a mouth of the conical flask, and the front air duct, the rear air duct and the infusion tube are inserted into the conical flask through holes opened in the rubber stopper.
3. The on-line direct measurement apparatus according to claim 2, wherein the separating funnel has a liquid outlet pipe inserted into the conical flask through a hole opened in the rubber stopper.
4. An on-line direct measurement device according to claim 3, wherein a third switch is provided on the outlet pipe.
5. The on-line direct measurement device of claim 1, wherein the second end of the leading airway is provided with a dilator.
6. The on-line direct measurement device of claim 5, wherein the mouth expander is horn-shaped.
7. The on-line direct measurement device according to claim 1, wherein a fourth switch is provided on the rear airway.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811505337.2A CN109444009B (en) | 2018-12-10 | 2018-12-10 | On-line direct test equipment for benzopyrene in atmospheric environment |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811505337.2A CN109444009B (en) | 2018-12-10 | 2018-12-10 | On-line direct test equipment for benzopyrene in atmospheric environment |
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| CN109444009A CN109444009A (en) | 2019-03-08 |
| CN109444009B true CN109444009B (en) | 2024-02-20 |
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| CN108872445A (en) * | 2018-08-27 | 2018-11-23 | 四川省疾病预防控制中心 | The analysis pre-treating method of 16 kinds of polycyclic aromatic hydrocarbons in a kind of airborne fine particulate matter PM2.5 |
| CN209513527U (en) * | 2018-12-10 | 2019-10-18 | 红云红河烟草(集团)有限责任公司 | The online straight measurement equipment of BaP in atmospheric environment |
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