CN108226269B - In-situ and rapid detection method and device for volatile organic compounds in soil - Google Patents
In-situ and rapid detection method and device for volatile organic compounds in soil Download PDFInfo
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Abstract
The invention provides an in-situ and rapid detection method and a device for volatile organic compounds in soil, wherein the detection device comprises a front-end extraction device and a rear-end detection device, and the front-end extraction device and the rear-end detection device are connected through a gas path pipeline; the front end extraction device comprises a shell, a handle and pedals, wherein the handle is arranged on the shell, the lower end part of the handle extends into the shell, and the pedals are arranged on two opposite side surfaces of the shell; the lower tip of handle is provided with the geotome, and the handle can drive the geotome and prolong vertical direction motion. The detection device has simple structure and simple and convenient operation, and can carry out in-situ and rapid detection on volatile organic compounds in soils with different soil qualities and different depths at different temperatures.
Description
Technical Field
The invention relates to a method and a device for detecting volatile organic compounds in soil, in particular to a method and a device which are combined with a mass spectrum detection method and can carry out in-situ and rapid detection on volatile organic compounds in soil with different soil qualities and different depths at different temperatures.
Background
Volatile Organic Compounds (VOCs) are a class of organic compounds having a boiling point below 260 ℃ and a saturated vapor pressure at room temperature above 133.32 Pa. Most VOCs have persistence, lipophilicity, deposition and high toxicity, and a substantial portion of VOCs are even carcinogenic and genetically toxic. The soil has strong adsorption capacity to VOCs, the VOCs in the soil has concealment, toxicity, durability, diversity and volatility, and the soil polluted by the VOCs can indirectly cause great harm to the surrounding environment, animals, plants and human bodies, so the detection and treatment of the VOCs in the soil are important subjects about the national civilization.
At present, the technology for detecting VOCs in soil is mainly laboratory instrument analysis technology: the laboratory instrumental analysis technology mostly adopts Gas Chromatography (GC), Liquid Chromatography (LC), Gas Chromatography-Mass Spectrometry (GC-MS), Gas Chromatography-Flame Ionization Detector (GC-FID), Gas Chromatography-photoionization Detector (GC-PID), Gas Chromatography-Electron Capture Detector (GC-ECD) and other instruments, and is often combined with sample pretreatment methods such as static headspace, purging and trapping, solid phase microextraction, microwave extraction and the like, the device is complex, the process is complicated, the detection time is long, and the VOCs are collected, transported and stored due to the existence of the process, the Volatile Organic Compound (VOCs) can not be detected in real situations, and the VOCs can not reflect the real pollution of the soil, in-situ and timely rapid on-site detection cannot be realized.
In CN 204330674U, a blowing and trapping pretreatment method is adopted to detect VOCs in soil in combination with a Time-of-flight Mass Spectrometry (TOF-MS) technology, the blowing and trapping sample pretreatment method has the processes of collecting and freeze-drying a soil sample, volatilization and leakage of the VOCs are inevitably caused, the method belongs to an ex-situ extraction method, inert gas is required to be introduced into a sample pool through a blowing pipe, then the sample is enriched and heated and vaporized through a concentration concentrator, and finally the mixture is uniformly mixed through a gas mixing tank and then sent into the TOF-MS through a quantitative ring for analysis, although the TOF-MS can be used for accurately detecting the types and concentrations of the VOCs, the extraction device of the VOCs is more complex and the pretreatment Time is longer; in CN 104181284A, a thermal extraction method is combined with GC-FID or GC-PID or GC-ECD to detect VOCs in soil, a hydraulic transmission device is adopted by the extraction device of VOCs to insert a hollow drill bit into the soil, carrier gas is introduced into the drill bit, then a small part of the soil nearby is heated by a resistance wire to change the VOCs in the soil into gas, and finally the gas-state VOCs are carried into the GC-FID or GC-PID or GC-ECD by the carrier gas to be detected; in CN 104597143A, adopting microwave extraction pretreatment combined with GC, LC and GC-MS methods to detect different types of VOCs, wherein the microwave extraction pretreatment needs to collect soil samples in advance, weigh the soil samples, then put the weighed soil samples into a digestion tank and add extraction liquid, then using a microwave extractor to perform extraction for a long time, cooling, filtering, acid washing and drying the extracted different types of samples, and finally adopting three different methods of GC, LC and GC-MS to detect the extracted different types of samples respectively, the method has long extraction time and complex extraction process, and when adopting GC or LC or GC-MS to detect, the GC and LC have long separation time of substances, and the LC also needs to use organic solvents and auxiliary gases; in CN 201716312U, a thermal extraction method is used in combination with a flowmeter and a volatile organic compound tester to detect VOCs in soil, a large-scale drilling machine is first used to drill a probe into soil, a resistance wire arranged in the probe is then used to heat the nearby soil to volatilize the VOCs, and then the volatile organic compound is sent to the flowmeter and the volatile organic compound tester through an air duct under the action of a suction fan to detect the VOCs; in CN 205384258U, volatile pollutants in soil are detected by combining a thermal extraction method and a GC, a soil sample is firstly collected, then the soil sample is placed on a mesh screen in a sealed barrel, then the soil sample is heated and vibrated, and finally organic pollutants volatilized from the soil sample are sent into the GC through a gas conveying pipe for detection. The above patents have respective limitations more or less, and cannot simultaneously meet the requirements of in-situ, rapid and accurate detection of VOCs in soil.
With the increasing importance of countries and society on the detection of VOCs in soil, the demand on soil VOCs detection equipment is increasingly strong, and particularly, the demand on simple, rapid, in-situ and accurate detection methods and equipment is stronger.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide an in-situ and rapid detection method and device for volatile organic compounds in soil, which can be used for in-situ, rapid, accurate, simple and convenient detection of volatile organic compounds in soil at different temperatures for different soil qualities and different depths.
The technical route of the method is as follows: for field detection, direct sample injection is adopted without sample pretreatment, firstly, the soil is heated to a certain temperature by adopting a thermal extraction method to reach the boiling point of VOCs, so that the VOCs are volatilized from the soil, and then the VOCs are guided into a rear-end detection device for detection through a simple guide device; for rear-end detection, rapid, online and accurate detection and analysis can be realized, and the membrane sample introduction technology is a sample introduction technology which has the advantages of simple structure, no need of pretreatment, short response time, selective separation and enrichment functions and capability of enabling volatile organic compounds to rapidly penetrate, and can completely meet the requirements of in-situ, rapid and accurate detection on VOCs in soil by combining the advantages of trace analysis, rapid response, high sensitivity, high resolution and the like of a portable mass spectrometer.
The purpose of the invention is realized by the following technical scheme:
the invention provides an in-situ and rapid detection device for volatile organic compounds in soil, which comprises a front-end extraction device and a rear-end detection device, wherein the front-end extraction device and the rear-end detection device are connected through a gas circuit pipeline; the front end extraction device comprises a shell, a handle and pedals, wherein the handle is arranged on the shell, the lower end part of the handle extends into the shell, and the pedals are arranged on two opposite side surfaces of the shell; the lower tip of handle is provided with the geotome, and the handle can drive the geotome and prolong vertical direction motion.
Preferably, the soil sampling drill is of a hollow structure, the bottom of the soil sampling drill is open, and the side wall of the soil sampling drill is provided with a plurality of first small holes. The first small hole can enable volatile organic compounds to escape from the soil; the soil sampling drills of different types (different types of soil sampling drills are suitable for different soil textures) can be replaced according to different soil textures.
Preferably, a temperature probe is arranged below the handle and in the middle of the soil sampling drill, and the temperature probe is connected with the handle in a sealing mode.
Preferably, the shell is of a hollow structure, the bottom of the shell is open, and one or more heating devices are uniformly arranged on the inner side wall of the shell.
More preferably, the heating device is an infrared heating pipe, the number of the heating device is 4, the infrared heating pipe is matched with the temperature probe, and the soil can be heated to the set temperature in a short time under the control of the controller.
Preferably, an end cover is arranged above the shell, and the shell and the end cover are connected through a clamping hoop and a sealing ring.
When the soil surface detection device is used for detection, after the shell is contacted with soil to be detected, the shell, the end cover and the surface of the soil to be detected form a closed detection cavity together.
Preferably, the shell is of an annular structure, and the bottom of the shell is provided with an annular wedge-shaped structure with a certain height for being inserted into the soil surface layer.
Preferably, the inner surface of the end cover is provided with a dust filtering box, and the dust filtering box is connected with the end cover through threads; the dust filter box is internally provided with dustproof filter cotton, and the lower bottom surface of the dust filter box is provided with a plurality of second small holes;
and a pneumatic connector and a sealing cable connector are arranged on the outer surface of the end cover.
More preferably, the dustproof filter cotton is made of high-temperature-resistant and volatile-free materials and is used for filtering particulate matters generated in the detection process and preventing the air path pipeline from being blocked.
Preferably, the lower end part of the pneumatic connector is communicated with the dust filtering box, and the upper end part of the pneumatic connector is connected with the rear end detection device through an air channel pipeline; one end of the sealed cable joint is connected with the heating device and the temperature probe, and the other end of the sealed cable joint is connected with an external power supply and the controller.
Preferably, a spring energy storage sealing ring and a spring energy storage sealing ring gland are arranged at the joint of the handle and the end cover, and the spring energy storage sealing ring is arranged in the spring energy storage sealing ring gland. The spring energy storage sealing ring is coaxial with the connecting rod of the handle and is used for providing sealing during the up-and-down reciprocating motion and the rotating motion of the handle; the spring energy storage sealing ring gland is in threaded connection with the end cover and used for fixing the spring energy storage sealing ring.
Preferably, the rear end detection device is a portable membrane sample injection mass spectrometer and is in sealing connection with the gas path pipeline through a gas pump.
Preferably, the pedal is provided at a lower end portion of the housing for fixing the front end extraction device.
Preferably, the handle comprises a handle and a connecting rod, one end of the connecting rod is connected with the handle, and the other end of the connecting rod is connected with the soil auger; the handle is connected with the connecting rod through threads, and the handle is coated with insulating materials; aiming at different soil depths, connecting rods with different lengths can be replaced, and scales are marked on the connecting rods.
All the connecting parts of the invention are hermetically connected so as to ensure that the detection cavity can form relative seal after the shell is placed on the soil surface layer. The parts connected through the screw thread can be detached and replaced.
The invention also provides an in-situ and rapid detection method for volatile organic compounds in soil, which adopts the detection device for detection.
Preferably, the detection method comprises the following steps: arrange whole front end extraction element in the soil top layer, fixed by the footboard, form a airtight detection cavity in inside, adopt the handle to drive the geotome and get soil to airtight detection cavity middle part, through the heating, volatile organic compounds comes out from the loss in the soil, volatile organic compounds filters the back through the dirt filtering box under the air pump effect, detects in getting into portable membrane advance appearance mass spectrograph by the gas circuit pipeline.
Compared with the prior art, the invention has the following beneficial effects: the detection device has simple structure and simple and convenient operation, and can realize in-situ, rapid and accurate detection of the volatile organic compounds under different soil qualities, different soil depths and different temperatures.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1 is a schematic view of the apparatus of the present invention;
FIG. 2 is a bottom view of the front end extraction assembly of the present invention;
FIG. 3 is a top view of the front end extraction assembly of the present invention;
FIG. 4 is a right side view of the front end extraction assembly of the present invention;
FIG. 5 is a sectional view showing the internal structure of the front end extraction device according to the present invention;
wherein: 1-a shell; 2-end cap; 3-a handle; 4, clamping a hoop; 5-a pedal; 6-earth boring; 7-a dust filtration box; 8-spring energy storage sealing ring gland; 9-spring energy storage sealing ring; 10-temperature probe; 11-a heating device; 12-sealing the cable joint; 13-a pneumatic joint; 14-gas path pipeline; 15-dustproof filter cotton; 16-an air pump; 17-portable membrane sample mass spectrometer.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that it would be obvious to those skilled in the art that various changes and modifications can be made without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1
The embodiment provides an in-situ and rapid detection device for volatile organic compounds in soil, as shown in fig. 1 to 5, which includes a front end extraction device and a rear end detection device, wherein the front end extraction device and the rear end detection device are connected through a gas pipeline 14; the front end extraction device comprises a shell 1, a handle 3 and pedals 5, wherein the handle 3 is arranged on the shell 1, the lower end part of the handle 3 extends into the shell 1, and the pedals 5 are arranged on two opposite side surfaces of the shell 1; the lower tip of handle 3 is provided with soil auger 6, and handle 3 can drive soil auger 6 and extend vertical direction motion.
The soil sampling drill 6 is of a hollow structure, the bottom of the soil sampling drill is open, and a plurality of first small holes are formed in the side wall of the soil sampling drill. The first small hole can enable volatile organic compounds to escape from the soil; different types of soil drills 6 can be replaced for different soil qualities (different types of soil drills are suitable for different soil qualities).
And a temperature probe 10 is arranged below the handle 3 and in the middle of the soil sampling drill 6, and the temperature probe 10 is hermetically connected with the handle 3.
The shell 1 is of a hollow structure, the bottom of the shell is open, and one or more heating devices 11 are uniformly arranged on the inner side wall of the shell 1.
An end cover 2 is arranged above the shell 1, and the shell 1 and the end cover 2 are connected through a hoop 4 and a sealing ring.
When the soil surface detection device is used for detection, after the shell 1 is contacted with soil to be detected, the shell 1, the end cover 2 and the surface of the soil to be detected form a closed detection cavity together.
The shell 1 is of an annular structure, and the bottom of the shell is provided with an annular wedge-shaped structure with a certain height and used for being inserted into a soil surface layer.
The inner surface of the end cover 2 is provided with a dust filtering box 7, and the dust filtering box 7 is connected with the end cover 2 through threads; the dust filtering box 7 is internally provided with dustproof filtering cotton 15, and the lower bottom surface of the dust filtering box 7 is provided with a plurality of second small holes;
the outer surface of the end cover 2 is provided with a pneumatic connector 13 and a sealed cable connector 12.
The dustproof filter cotton 15 is made of high-temperature-resistant and non-volatile materials and is used for filtering particles appearing in the detection process and preventing the air path pipeline from being blocked.
The lower end part of the pneumatic connector 13 is communicated with the dust filtering box 7, and the upper end part is connected with a rear end detection device through an air passage pipeline 14; one end of the sealed cable joint 12 is connected with the heating device 11 and the temperature probe 10, and the other end is connected with an external power supply and a controller.
The handle 3 and the end cover 2 are connected through a spring energy storage sealing ring 9 and a spring energy storage sealing ring gland 8, and the spring energy storage sealing ring 9 is arranged in the spring energy storage sealing ring gland 8. The spring energy storage sealing ring 9 is coaxial with the connecting rod of the handle 3 and is used for providing sealing during the up-and-down reciprocating motion and the rotating motion of the handle 3; the spring energy storage sealing ring gland 8 is connected with the end cover 2 through threads and used for fixing the spring energy storage sealing ring 9.
The rear end detection device is a portable membrane sample injection mass spectrometer and is hermetically connected with the gas circuit pipeline 14 through a gas pump 16.
The pedal 5 is provided at the lower end of the housing 1 for fixing the front end extraction device.
The handle 3 comprises a handle and a connecting rod, one end of the connecting rod is connected with the handle, and the other end of the connecting rod is connected with the soil sampling drill 6; the handle is connected with the connecting rod through threads, and the handle is coated with insulating materials; aiming at different soil depths, connecting rods with different lengths can be replaced, and scales are marked on the connecting rods.
All the connecting parts of the invention are hermetically connected so as to ensure that the detection cavity can form relative seal after the shell 1 is placed on the soil surface layer. The parts connected through the screw thread can be detached and replaced.
The detection device is adopted to carry out in-situ and rapid detection on volatile organic compounds in the simulated soil sample, and the detection method comprises the following steps: firstly, preparing a simulated soil sample, adding 35 VOC standard samples with the concentration of 20 mug/L into 1kg of VOC-free standard soil, uniformly mixing, preparing a standard sample with the addition amount of 2 mug, placing the whole front-end extraction device on the surface layer of the soil sample, forming a closed detection cavity inside, driving a soil sampling drill by a handle to take the soil sample to the middle part of the closed detection cavity, heating to enable volatile organic compounds to escape from the soil, filtering the volatile organic compounds by a dust filter box under the action of an air pump, and then enabling the volatile organic compounds to enter a portable sample introduction mass spectrometer through an air pipeline to perform parallel detection for 5 times.
The time from sampling to detection ending is only about 5min, and the result of the standard recovery rate of 5 parallel detections is shown in table 1, the average recovery rate of 35 VOC standard samples is 91.03% -104.85%, and the allowable limit of 80% -120% is met.
TABLE 15 recovery rates of spiked replicates
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes or modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention. The embodiments and features of the embodiments of the present application may be combined with each other arbitrarily without conflict.
Claims (2)
1. An in-situ and rapid detection device for volatile organic compounds in soil is characterized by comprising a front-end extraction device and a rear-end detection device, wherein the front-end extraction device and the rear-end detection device are connected through a gas circuit pipeline; the front end extraction device comprises a shell, a handle and pedals, wherein the handle is arranged on the shell, the lower end part of the handle extends into the shell, and the pedals are arranged on two opposite side surfaces of the shell; the lower end part of the handle is provided with the soil sampling drill, and the handle can drive the soil sampling drill to move along the vertical direction;
the soil sampling drill is of a hollow structure, the bottom of the soil sampling drill is open, and a plurality of first small holes are formed in the side wall of the soil sampling drill;
a temperature probe is arranged below the handle and in the middle of the soil sampling drill and is in sealed connection with the handle;
the shell is of a hollow structure, the bottom of the shell is open, and one or more heating devices are uniformly arranged on the inner side wall of the shell;
an end cover is arranged above the shell, and the shell and the end cover are connected through a hoop and a sealing ring;
when the soil surface detection device is used for detection, after the shell is contacted with the soil to be detected, the shell, the end cover and the surface of the soil to be detected form a closed detection cavity together; the inner surface of the end cover is provided with a dust filtering box, and the dust filtering box is connected with the end cover through threads; the dust filter box is internally provided with dustproof filter cotton, and the lower bottom surface of the dust filter box is provided with a plurality of second small holes;
the outer surface of the end cover is provided with a pneumatic connector and a sealing cable connector;
the lower end part of the pneumatic connector is communicated with the dust filtering box, and the upper end part of the pneumatic connector is connected with the rear end detection device through an air path pipeline; one end of the sealed cable joint is connected with the heating device and the temperature probe, and the other end of the sealed cable joint is connected with an external power supply and a controller;
a spring energy storage sealing ring and a spring energy storage sealing ring gland are arranged at the joint of the handle and the end cover, and the spring energy storage sealing ring is arranged in the spring energy storage sealing ring gland;
the rear end detection device is a portable membrane sample injection mass spectrometer and is hermetically connected with the gas path pipeline through a gas pump;
all the connecting parts of the device are hermetically connected so as to ensure that the detection cavity can form relative sealing after the shell is placed on the soil surface layer.
2. An in-situ and rapid detection method for volatile organic compounds in soil, which is characterized in that the detection device of claim 1 is adopted for detection.
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| CN201711167231.1A CN108226269B (en) | 2017-11-21 | 2017-11-21 | In-situ and rapid detection method and device for volatile organic compounds in soil |
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| CN108226269B true CN108226269B (en) | 2021-03-23 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109738242A (en) * | 2019-01-11 | 2019-05-10 | 成都市环境保护科学研究院 | Volatile organic contaminant acquisition device in soil |
| CN109991045A (en) * | 2019-03-20 | 2019-07-09 | 中国地质大学（武汉） | A kind of gas rapid sampling attachment suitable for clayed soil |
| CN110031267B (en) * | 2019-04-01 | 2024-06-25 | 北京鹏宇昌亚环保科技有限公司 | Head space mechanism for soil VOCs treatment instrument and soil VOCs treatment instrument |
| CN111122233A (en) * | 2020-01-07 | 2020-05-08 | 浙江埃泰克环境科技有限公司 | Soil sampler for VOCs analysis |
| CN115452446B (en) * | 2022-09-07 | 2023-06-20 | 兰州空间技术物理研究所 | Lunar soil sample feeding and heating device |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN204330674U (en) * | 2015-01-08 | 2015-05-13 | 王新娟 | For detecting the equipment of Volatile Organic Compounds in Soil |
| CN204988775U (en) * | 2015-09-15 | 2016-01-20 | 湖南润丰达生态环境科技有限公司 | Device that fetches earth that is used for soil measuring in surveying soil fertilization |
| CN105954059A (en) * | 2016-06-01 | 2016-09-21 | 青岛农业大学 | Convenient undisturbed soil taking device |
| CN107063739A (en) * | 2016-11-10 | 2017-08-18 | 东北农业大学 | Sample acquisition machine |
| CN107340152B (en) * | 2017-07-08 | 2020-02-18 | 广东中协和检测有限公司 | Soil volatile organic compounds environmental protection detection device |
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