CN107290454B - Portable soil remediation polycyclic aromatic hydrocarbon's quick detection device - Google Patents
Portable soil remediation polycyclic aromatic hydrocarbon's quick detection device Download PDFInfo
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Abstract
The invention discloses a portable rapid detection device for soil remediation polycyclic aromatic hydrocarbon, which comprises a soil sampling device, a cooling screening device, a dryness and humidity sensor, at least one Soxhlet extractor, a rapid solvent extractor, a gas chromatograph-mass spectrometer and a base, wherein the cooling screening device comprises a screening funnel, a crushing device, a cooling air injection ring pipe and a soil storage device, and the screening funnel is arranged at the top of a detachable vibrating screen and is provided with a screening rake; the Soxhlet extractors are connected to a base between the cooling screening device and the rapid solvent extractor through a fixed box body; the dry and wet sensor, the rapid solvent extractor, the gas chromatograph-mass spectrometer and the smashing device are all connected with the control panel. The rapid detection device integrates soil pre-sampling for soil polycyclic aromatic hydrocarbon detection, automatic processing of sampled soil samples, sequential Soxhlet extraction, rapid extraction and gas chromatography-mass spectrometry combined instrument processing, and improves the detection efficiency of soil polycyclic aromatic hydrocarbon.
Description
Technical Field
The invention relates to the technical field of polycyclic aromatic hydrocarbon detection for soil remediation, in particular to a portable rapid detection device for soil remediation polycyclic aromatic hydrocarbon.
Background
Polycyclic Aromatic Hydrocarbons (PAHs) are a class of persistent organic pollutants with three causes (carcinogenic, teratogenic and mutagenic), mainly in the atmosphere, water and soil. Polycyclic aromatic hydrocarbons are produced by incomplete combustion of organics and fossil fuels, and there are four main causes of global polycyclic aromatic hydrocarbon pollution today: (1) Smoke dust generated by household stoves, domestic stoves, industrial boilers and the like; (2) Various industrial processes for producing and using tar, such as coking, petroleum cracking, coal tar refining, asphalt paving, and the like; (3) various artificial open-air combustion and fires; (4) exhaust gases of various motor vehicles and internal combustion engines.
Because of the very low levels of these compounds in the environment, how to isolate and enrich them from environmental samples and further analyze them is the most important step in the overall analysis technique, as it directly affects the accuracy of the final analysis results. In particular, for the restored soil, it is still necessary to detect the content of polycyclic aromatic hydrocarbon in the soil in real time, so as to ensure the stability of the restoration of the soil and the sustainable use performance in the later period.
The analysis method of the polycyclic aromatic hydrocarbon mainly comprises the following steps: column chromatography, thin layer chromatography, ultraviolet absorption, gas Chromatography (GC), high performance liquid chromatography, mass spectrometry, etc. Column chromatography and thin layer chromatography have certain separation effects, but cannot perform accurate definite and quantitative analysis; gas Chromatography (GC), high performance liquid chromatography and mass spectrometry can perform qualitative and quantitative analysis at the same time, but the requirement for the sample is high, and pretreatment is required to remove a large amount of impurities. At present, a method for analyzing polycyclic aromatic hydrocarbon in soil generally adopts a Soxhlet extraction-column chromatography separation-gas phase mass spectrometry method, and specifically comprises the steps of placing a soil or sediment sample in a Soxhlet extractor, refluxing for 18-24 hours by using benzene/methanol or dichloromethane/acetone, adding copper powder, and concentrating; subjecting to anhydrous sodium sulfate/silica gel/alumina column chromatography, eluting with n-hexane and dichloromethane, concentrating with a concentrator, and fixing volume; qualitative and quantitative determinations were made using a gas chromatograph/mass spectrometer (GC/MS) using standards.
However, for sludge, if only the analysis method of polycyclic aromatic hydrocarbon in soil is adopted, a large amount of organic substances exist, thereby interfering the determination result of GC/MS on polycyclic aromatic hydrocarbon.
The Chinese patent No. CN101122588A, named a method for determining polycyclic aromatic hydrocarbon in sludge, discloses a method for determining polycyclic aromatic hydrocarbon in the conventional soil, which is based on the steps of Soxhlet extraction, column chromatography, gas phase mass spectrometry and the like, and adds a process of washing the eluent with concentrated sulfuric acid after column chromatography. Although the method of the invention adds one step of washing the eluent with concentrated sulfuric acid after column chromatography on the basis of the steps of Soxhlet extraction, column chromatography, gas phase mass spectrometry and the like of the conventional analysis method of polycyclic aromatic hydrocarbon in soil, the method for measuring polycyclic aromatic hydrocarbon in sludge with good accuracy and high detection efficiency is provided. However, in the process of testing soil samples by using the method, the samples are required to be collected by using a gravity column-shaped mud collector, the samples are subjected to light-proof natural air drying in a laboratory, ground and sieved by a 80-mesh sieve, the sieved samples are placed in a sealed bag for low-temperature preservation, and then the samples are subjected to pretreatment, sample extraction, sample purification, sample concentration, constant volume, recovery experiments and GC/MS analysis, and then are respectively required to be carried out by different test equipment and instruments, the carrying out period is long, and the sample is difficult to process intensively and the test data are unified, and many data are required to be manually processed, such as table comparison and the like, and the processing period is long.
Disclosure of Invention
In order to overcome the defects in the prior art, the invention provides a rapid detection device for rapidly, efficiently and integrally detecting the content of polycyclic aromatic hydrocarbon after soil remediation.
The technical scheme adopted by the invention is as follows: the utility model provides a portable soil repair polycyclic aromatic hydrocarbon's quick detection device, includes soil sampling device, cooling screening plant, dry humidity sensor, at least one soxhlet extractor, quick solvent extraction appearance, gas chromatography-mass spectrometer and base, wherein: the soil sampling device is connected to the top position of the cooling and screening device in a turnover way through the hinged support; the cooling screening device comprises a screening funnel, a crushing device, a cooling air injection ring pipe and a soil storage device which are arranged from top to bottom, a detachable vibrating screen is further arranged between the screening funnel and the crushing device, the screening rake is arranged at the top of the detachable vibrating screen, and the screening rake acquires large-particle soil at the top of the detachable vibrating screen and other impurities and removes the large-particle soil outside the screening funnel for discarding; the Soxhlet extractors are connected to a base between the cooling screening device and the rapid solvent extractor through a fixed box body; the dry and humidity sensor, the rapid solvent extractor, the gas chromatograph-mass spectrometer and the smashing device are all connected with a control panel, and the control panel controls and displays the switching states of the devices and the digital signals in each device.
Further, the screening rake includes the rake body, discharge port, vortex fan and material output tube, and wherein the rake body passes through the bracing piece to be fixed at the inner wall of screening funnel, and the discharge port is established to the central part of the rake body, and vortex fan and material output tube are connected gradually at the top of discharge port, and this material output tube extends beyond screening funnel.
Further, the bottom of the rake body of the screening rake is also provided with a plurality of metal rake teeth which collect or wind some flexible impurities.
Further, the cooling air injection ring pipe is connected to the bottom of the cooling screening device and is in a circular structure; and meanwhile, a plurality of nozzles are arranged on the inner wall of the cooling air injection circular pipe towards the central position, and the nozzles spray cold air into the cooling air injection circular pipe through a blower.
Further, a rubber damping air bag ring is further arranged at the connection position of the crushing device of the cooling screening device and the cooling air injection annular pipe, the whole rubber damping air bag ring is of a cylindrical structure, and the thickness of the damping air bag ring is 3-6cm.
Further, at least one side of the soil housing device is provided with ventilation holes which further assist in lowering the temperature of the soil within the soil housing device.
Further, the quick solvent extractor and the gas chromatograph-mass spectrometer are detachably connected to the base.
Further, the soil sampling device comprises a shovel structure and a cantilever, wherein the cantilever is detachably connected to the hinged support through a plug pin.
Further, the fixed box body is of a semi-I-shaped structure, and a plurality of damping structures are arranged between the fixed box body and the soil containing device of the cooling and screening device; several Soxhlet extractors are connected in parallel inside.
Further, the cantilever drives the digging structure to rotate through a turnover sampling cylinder or a motor and a turnover support arm, so that automatic soil sampling is realized; the overturning support arm is fixed at the output end of the overturning sampling cylinder or the motor, and the other end of the overturning support arm is hinged with the cantilever through a double-lug structure at the tail end of the overturning support arm, so that overturning is finally realized.
Compared with the prior art, the invention has the beneficial effects that: according to the rapid detection device for the soil remediation polycyclic aromatic hydrocarbon, disclosed by the invention, the soil sampling device, the cooling screening device, the dryness and humidity sensor, the at least one Soxhlet extractor, the rapid solvent extractor and the gas chromatography-mass spectrometer are connected on the base in a concentrated manner, and after the rollers, the tires or the movable power source and the power equipment are arranged on the base, the rapid detection device can be moved to the soil site to perform local sampling and rapid detection, or the steps of automatic sampling, automatic screening, grinding and cooling are directly realized on the soil at a sampling site, so that the detection time and steps of the soil remediation polycyclic aromatic hydrocarbon are shortened, and the detection efficiency of the soil remediation polycyclic aromatic hydrocarbon is improved.
In addition, the rapid detection device of the invention also connects the dryness and humidity sensor, the rapid solvent extractor, the gas chromatograph-mass spectrometer and the crushing device with the control panel, uses the control panel to control and display the on-off states of the devices and the digital signals in each device, and improves the overall coordination and control capacity of the devices.
In general, the rapid detection device for soil remediation polycyclic aromatic hydrocarbon integrates soil pre-sampling for soil polycyclic aromatic hydrocarbon detection, automatic processing of sampled soil samples, sequential Soxhlet extraction, rapid extraction and gas chromatography-mass spectrometry combined instrument processing, reduces various steps for soil polycyclic aromatic hydrocarbon detection, shortens the detection period of soil polycyclic aromatic hydrocarbon, and improves the detection efficiency of soil polycyclic aromatic hydrocarbon.
Drawings
FIG. 1 is a block diagram of one embodiment of a portable soil remediation, polycyclic aromatic hydrocarbon rapid detection device;
FIG. 2 is a schematic diagram of the soil sampling apparatus and cooling screening apparatus of the embodiment of FIG. 1;
FIG. 3 is a state diagram of the embodiment of FIG. 1 in which the fast solvent extractor 5 and the gas chromatograph-mass spectrometer 6 are detached from the base for use;
FIG. 4 is a block diagram of one embodiment of a soil sampling device;
FIG. 5 is a detailed view of the cooling screen of the rake;
wherein: 1-a soil sampling device, 101-a digging shovel structure, 102-a cantilever, 103-a turnover sampling cylinder or motor, and 104-a turnover support arm; 2-cooling screening device, 21-screening hopper, 22-crushing device, 23-cooling air injection ring pipe and 231-nozzle; 24-soil containing device, 25-detachable vibrating screen, 26-screening rake, 261-rake body, 262-metal rake teeth, 263-discharge hole, 264-vortex fan, 265-material output pipe, 266-support bar and 27-blower; 3-dry humidity sensor, 4-Soxhlet extractor, 5-quick solvent extractor, 6-gas chromatograph-mass spectrometer, 7-hinged support, 8-fixed box, 9-base, 10-control panel, 11-shock-absorbing structure, 12-rubber shock-absorbing air bag ring and 13-plug pin.
Detailed Description
The present invention will be further described with reference to the drawings and examples, which are only for the purpose of illustrating the invention and are not to be construed as limiting the scope of the invention.
As shown in fig. 1, a portable rapid detection device for soil remediation polycyclic aromatic hydrocarbon comprises a soil sampling device 1, a cooling screening device 2, a dryness and humidity sensor 3, at least one soxhlet extractor 4, a rapid solvent extractor 5, a gas chromatography-mass spectrometer 6 and a base 9, wherein: the soil sampling device 1 is connected with the top position of the cooling and screening device 2 in a reversible way through a hinged support 7; as shown in fig. 2, the cooling screening device 2 comprises a screening funnel 21, a crushing device 22, a cooling air injection circular pipe 23 and a soil accommodating device 24 which are arranged from top to bottom, a detachable vibrating screen 25 is further arranged between the screening funnel 21 and the crushing device 22, a screening rake 26 is arranged at the top position of the detachable vibrating screen 25 of the screening funnel 21, and the screening rake 26 acquires large-particle soil and other impurities at the top of the detachable vibrating screen 25 and removes the large-particle soil and other impurities outside the screening funnel for discarding; the Soxhlet extractors 4 are connected to a base 9 between the cooling screening device 2 and the rapid solvent extractor 5 through a fixed box 8; the rapid detection device of the invention also connects a dryness and humidity sensor, a rapid solvent extraction instrument, a gas chromatography-mass spectrometer and a smashing device with a control panel, uses the control panel 10 to control and display the switching states of the devices and the digital signals in each device, improves the overall coordination and control capacity of the devices, connects and transmits the data and signals among the devices through one of wired, wireless, infrared or Bluetooth, and finally displays the temperature and humidity data, smashing related voltage or control data of the repaired polycyclic aromatic hydrocarbon soil, the extraction time and temperature parameters, and the parameters of the chromatograph-mass spectrometer of the polycyclic aromatic hydrocarbon in each group of soil detected by the gas chromatography-mass spectrometer.
In the above embodiment, in order to automatically clean up the sundries or residues above the detachable vibrating screen 25 in the screening hopper 21, as shown in fig. 5, the screening rake 26 includes a rake body 261, a discharge hole 263, a vortex fan 264 and a material output pipe 265, wherein the rake body 261 is fixed on the inner wall of the screening hopper 21 through a support rod 266, the discharge hole 263 is arranged at the center of the rake body 261, the residues adsorbed by the vortex fan are discharged from the discharge hole to the outside of the device for disposal, the top of the discharge hole 263 is sequentially connected with the vortex fan and the material output pipe 265, and the material output pipe 265 extends beyond the screening hopper 21.
In the above embodiment, the bottom of the bamboo rake body 261 of the bamboo rake 26 is further provided with a plurality of metal bamboo rake teeth 262, and the metal bamboo rake teeth 262 collect or wind flexible impurities, thereby having better cleaning effect.
In the above embodiment, the cooling jet loop 23 is connected to the bottom of the cooling screening device 2 and has a circular configuration; at the same time, the inner wall of the cooling air injection loop 23 is provided with a plurality of nozzles 231 toward the center position, and the nozzles inject cool air into the cooling air injection loop 23 through the blower 27, thereby improving the capability of completely pulverizing the pulverized soil.
As shown in fig. 2 and 3, the connection position of the smashing device 22 of the cooling screening device 2 and the cooling air injection annular pipe 23 is further provided with a rubber damping air bag ring 12, the whole rubber damping air bag ring 12 is of a cylindrical structure, the thickness of the damping air bag ring 12 is 3-6cm, and the height of the damping air bag ring is 5-15cm, so that vibration transmitted from the smashing device to the soil storage device 24 is reduced, soil splashed by the soil storage device is further reduced, stability of the soil is guaranteed, waste is avoided, and efficiency of soil pretreatment is improved.
In the above embodiment, at least one side of the soil housing device 24 is provided with ventilation holes, which further assist in reducing the temperature of the soil in the soil housing device so that the soil meets the requirements of Soxhlet extraction as much as possible, saving processing time.
As shown in fig. 3, the fast solvent extractor 5 and the gas chromatography-mass spectrometer 6 are detachably connected to the base 9, and in specific use, the fast solvent extractor 5 and the gas chromatography-mass spectrometer 6 can be detached from the base, and the soil pre-sampling device and the soxhlet extractor are separately transported to a soil detection site, so that the use method is suitable for detecting large-area soil restoration, can sample multiple soil simultaneously and rapidly, and when the fast solvent extractor 5 and the gas chromatography-mass spectrometer 6 are detachably connected to the base 9, the control panel 10 is placed above the fixed box 8 of the soxhlet extractor.
In addition, as shown in fig. 4, the soil sampling device 1 comprises a shovel structure 101 and a cantilever 102, wherein the cantilever 102 is detachably connected to the hinged support 7 through a plug pin 13, and the shovel structure with the design can directly remove the soil to be sampled on site without carrying tools, so that the application range is wider. The cantilever 102 drives the digging structure 101 to rotate through the overturning sampling cylinder or the motor 103 and the overturning support arm 104, so that automatic soil sampling is realized; wherein upset support arm 104 is fixed at the output at upset sampling cylinder or motor 103, and the other end is through at its terminal ears structure and then articulated with cantilever 102, finally realizes automatic upset, need not manual operation, and sampling efficiency is higher.
In the above embodiment, the fixed box 8 has a semi-i-shaped structure, and a plurality of shock absorbing structures 11 are arranged between the fixed box and the soil containing device 24 of the cooling and screening device 2; the plurality of Soxhlet extractors 4 are connected in parallel in the soil, so that the soil which is already subjected to the Soxhlet extraction treatment process is not influenced by the soil which is being pre-treated, and the detection accuracy of polycyclic aromatic hydrocarbon of each sampled soil is improved.
In general, the rapid detection device for soil remediation polycyclic aromatic hydrocarbon integrates soil pre-sampling for soil polycyclic aromatic hydrocarbon detection, automatic processing of sampled soil samples, sequential Soxhlet extraction, rapid extraction and gas chromatography-mass spectrometry combined instrument processing, reduces various steps for soil polycyclic aromatic hydrocarbon detection, shortens the detection period of soil polycyclic aromatic hydrocarbon, and improves the detection efficiency of soil polycyclic aromatic hydrocarbon.
The embodiments of the present invention are disclosed as preferred embodiments, but not limited thereto, and those skilled in the art will readily appreciate from the foregoing description that various extensions and modifications can be made without departing from the spirit of the present invention.
Claims (8)
1. A portable soil remediation polycyclic aromatic hydrocarbon's quick detection device, its characterized in that: including soil sampling device (1), cooling screening plant (2), dry humidity sensor (3), at least one soxhlet extractor (4), quick solvent extraction appearance (5), gas chromatography-mass spectrometer (6) and base (9), wherein:
the soil sampling device (1) is connected to the top position of the cooling and screening device (2) in a reversible manner through a hinged support (7);
the cooling screening device (2) comprises a screening funnel (21), a crushing device (22), a cooling air injection ring pipe (23) and a soil accommodating device (24) which are arranged from top to bottom, a detachable vibrating screen (25) is further arranged between the screening funnel (21) and the crushing device (22), a screening rake (26) is arranged at the top position of the screening funnel (21) positioned at the detachable vibrating screen (25), and the screening rake (26) acquires large-particle soil and other impurities at the top of the detachable vibrating screen (25) and removes the large-particle soil and other impurities out of the screening funnel to be discarded;
the Soxhlet extractors (4) are connected to a base (9) between the cooling screening device (2) and the rapid solvent extractor (5) through a fixed box body (8);
the dry and wet sensor (3), the rapid solvent extractor (5), the gas chromatograph-mass spectrometer (6) and the smashing device (22) are all connected with the control panel (10), and the control panel (10) controls and displays the on-off states of the devices and the digital signals in each device;
the cooling air injection ring pipe (23) is connected to the bottom of the cooling screening device (2) and is in a circular structure; meanwhile, a plurality of nozzles are arranged on the inner wall of the cooling air injection circular pipe (23) towards the central position direction, and the nozzles spray cold air into the cooling air injection circular pipe (23) through a blower (27); the connection position of the crushing device (22) of the cooling screening device (2) and the cooling air injection ring pipe (23) is also provided with a rubber damping air bag ring (12); screening rake (26) include rake body (261), discharge port (263), vortex fan (264) and material output tube (265), and wherein rake body (261) are fixed at the inner wall of screening funnel (21) through bracing piece (266), and discharge port (263) are established at the central part of rake body (261), and vortex fan and material output tube (265) are connected gradually at the top of discharge port (263), and this material output tube (265) extend beyond screening funnel (21).
2. The portable rapid detection device for soil remediation polycyclic aromatic hydrocarbon according to claim 1, wherein: the bottom of the bamboo rake body (261) of the screening bamboo rake (26) is also provided with a plurality of metal bamboo rake teeth (262), and the metal bamboo rake teeth (262) collect or twine a plurality of flexible impurities.
3. The portable rapid detection device for soil remediation polycyclic aromatic hydrocarbon according to claim 1, wherein: the rubber shock-absorbing air bag ring (12) is of a cylindrical structure, and the thickness of the shock-absorbing air bag ring (12) is 3-6cm.
4. The portable rapid detection device for soil remediation polycyclic aromatic hydrocarbon according to claim 1, wherein: at least one side of the soil containing device (24) is provided with ventilation holes which further assist in reducing the temperature of the soil in the soil containing device.
5. The portable rapid detection device for soil remediation polycyclic aromatic hydrocarbon according to claim 1, wherein: the rapid solvent extraction instrument (5) and the gas chromatography-mass spectrometer (6) are detachably connected to the base (9).
6. The portable rapid detection device for soil remediation polycyclic aromatic hydrocarbon according to claim 1, wherein: the soil sampling device (1) comprises a digging shovel structure (101) and a cantilever (102), wherein the cantilever (102) is detachably connected to the hinged support (7) through a plug pin (13).
7. The portable rapid detection device for soil remediation polycyclic aromatic hydrocarbon according to any one of claims 1 to 6, wherein: the fixed box body (8) is of a semi-I-shaped structure, and a plurality of shock absorption structures (11) are arranged between the fixed box body and the soil containing device (24) of the cooling and screening device (2); a plurality of Soxhlet extractors (4) are connected in parallel inside thereof.
8. The portable rapid detection device for soil remediation polycyclic aromatic hydrocarbon of claim 7, wherein: the cantilever (102) drives the digging structure (101) to rotate through a turnover sampling cylinder or a motor (103) and a turnover support arm (104), so that automatic soil sampling is realized; the overturning support arm (104) is fixed at the output end of the overturning sampling cylinder or the motor (103), and the other end of the overturning support arm is hinged with the cantilever (102) through a double-lug structure at the tail end of the overturning support arm, so that overturning is finally realized.
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| CN101013114A (en) * | 2007-02-05 | 2007-08-08 | 同济大学 | Extraction purifying measuring method of polycyclic aromatic hydrocarbons in soil |
| CN101122588A (en) * | 2007-09-13 | 2008-02-13 | 复旦大学 | Method for determining polycyclic aromatic hydrocarbons in sludge |
| CN101773739B (en) * | 2009-12-23 | 2011-03-23 | 太原理工大学 | Method for extracting polyaromatic hydrocarbon from solid phase sample |
| CN103487301B (en) * | 2013-09-23 | 2016-08-10 | 福建师范大学 | Movable integrated machine is ground in a kind of soil analysis sample screening |
| CN104280485A (en) * | 2014-10-24 | 2015-01-14 | 南京大学 | Method for synchronously extracting and purifying various chlorinated polycyclic aromatic hydrocarbons in soil |
| RU2589897C1 (en) * | 2015-04-23 | 2016-07-10 | Федеральное Государственное Автономное Образовательное Учреждение Высшего Профессионального Образования "Дальневосточный Федеральный Университет" (Двфу) | Method of determining general and polycyclic aromatic hydrocarbons in components of ecosystem |
| CN105866276A (en) * | 2016-04-07 | 2016-08-17 | 河南城建学院 | Method for simultaneously extracting and purifying plurality of types of chlorinated polycyclic aromatic hydrocarbons in soil |
| CN207096182U (en) * | 2017-06-30 | 2018-03-13 | 迪天环境技术南京股份有限公司 | A kind of portable soil repairs the device for fast detecting of polycyclic aromatic hydrocarbon |
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