CN113865945A - Unpowered hood type passive sampling device for semi-volatile organic compounds and using method thereof - Google Patents
Unpowered hood type passive sampling device for semi-volatile organic compounds and using method thereof Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 10
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- 229910052751 metal Inorganic materials 0.000 claims abstract description 34
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- 238000001179 sorption measurement Methods 0.000 claims abstract description 16
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- YMWUJEATGCHHMB-UHFFFAOYSA-N Dichloromethane Chemical compound ClCCl YMWUJEATGCHHMB-UHFFFAOYSA-N 0.000 claims description 12
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- 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
- G01N1/2294—Sampling soil gases or the like
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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
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Abstract
The invention belongs to the technical field of atmospheric environmental pollutant monitoring, and provides a passive sampling device for unpowered hood type semi-volatile organic compounds and a using method thereof. A passive sampling device of unpowered hood type semi-volatile organic compounds comprises a hood, a connecting cylinder, a metal support, a sampling box, an adsorption material, a silicone tube, a gasket and a metal screen. The upper end opening of the connecting cylinder is butted with a blast cap, and the lower end of the connecting cylinder is connected with a gas pipe connector; the sampling box is connected with an air pipe joint at the bottom of the connecting cylinder through a silicone tube; the bottom of the sampling box is provided with an opening, and a coarse screen, a fine screen and a gasket are sequentially arranged at the opening from bottom to top. The hood is driven to rotate under the action of wind power, so that the air flow in the vertical direction is increased, the gas circulation speed in the sampling boxes is increased, the sampling rate is increased, the sampling time is shortened, the sampling rate of pollutants in the adsorbing materials of each sampling box is approximate to the same rate, and the difference of passive sampling rates caused by the difference of different high environmental conditions is corrected.
Description
Technical Field
The invention relates to the technical field of atmospheric environmental pollutant monitoring, in particular to a passive sampling device for unpowered hood type semi-volatile organic compounds and a using method thereof.
Background
The semi-volatile organic pollutants (SVOCs for short) refer to compounds with relatively strong volatility, insolubility in water, and solubility in organic solvents, and the boiling point is 170-350 ℃. Compared with volatile organic compounds, SVOCs are more difficult to degrade and exist in the environment for a longer time. The compounds are easy to persist in air, water, soil and other environments, can be transported for long distance, and most of the compounds have certain toxicity and bioaccumulation properties. Recently, soil and air pollution caused by SVOCs has been receiving increasing attention. The monitoring of the near-surface SVOCs concentration is helpful for knowing the concentration change and migration trend between soil and atmosphere, is helpful for mastering the soil-gas migration rule of SVOCs, and provides a theoretical basis for controlling and reducing SVOCs pollutants in soil and atmosphere.
There are two kinds of active and passive sampling methods for monitoring the concentration of SVOCs in air. The active sampler mainly utilizes a power air pump to extract air, has the advantages of short sampling time and accurate monitoring of instantaneous concentration, is expensive in manufacturing cost and large in size, needs a power supply during working, and is not beneficial to long-term sampling of multiple points in the field. In addition, the active sampler has disturbance to the surrounding air, which is not beneficial to the simultaneous acquisition of samples with different heights in a short distance. The passive sampler mainly adopts polyurethane foam and other adsorbing materials, and absorbs SVOCs in the air onto the adsorbing materials when the air flow passes through the adsorbing materials by utilizing the concentration gradient between the air and the adsorbing materials. The passive sampler has the advantages of low manufacturing cost, no need of a power supply and small interference to surrounding air, and is widely used for monitoring semi-volatile organic pollutants in atmospheric environments in field and other regional ranges, but the conventional polyurethane foam (PUF) passive sampler has long sampling time and low sampling rate, is easily influenced by environmental changes such as wind speeds at different heights and the like in the field sampling process, and the sampling rate is changed along with the change of the sampling rate, so that the deviation between the measured pollutant concentration and the actual concentration is large.
Disclosure of Invention
The invention aims to provide a passive sampling device for volatile organic compounds of an unpowered hood and a using method thereof, which are used for solving the problems in the prior art, accelerating the air circulation speed in a sampling box by rotating the hood, properly improving the sampling rate, shortening the sampling time, realizing the rapid acquisition of medium and short time of semi-volatile organic compounds in the atmosphere, and realizing the monitoring of the concentration of the vertical section of the soil of SVOCs by placing the sampling boxes at different heights. The device has applicability to continuous passive sampling of the soil with atmospheric gaseous semi-volatile organic compounds at different vertical heights and for a long time.
In order to achieve the purpose, the invention provides the following technical scheme:
a passive sampling device of unpowered hood type semi-volatile organic compounds comprises a hood 8, a connecting cylinder 9, a metal bracket 11, a sampling box 2, an adsorption material 7, a silicone tube 10, a gasket 3, a fine screen 4 and a coarse screen 5; the upper end of the connecting cylinder 9 is opened and is in threaded connection with the blast cap 8, the lower end of the connecting cylinder is closed and is provided with a plurality of air pipe joints 1, the air pipe joints and the blast cap are screwed tightly through threads, and the bottom of the connecting cylinder 9 is connected with the metal bracket 11; the top of the sampling box 2 is provided with a threaded round hole and is in threaded connection with the air pipe joint 1, and the air pipe joint 1 on the connecting cylinder 9 is connected with the air pipe joint 1 on the sampling box 2 through a silicone tube 10; a bottom cover 6 with a hole is arranged at the opening at the bottom of the sampling box 2; a coarse screen 5, a fine screen 4, a gasket 3 and an adsorbing material 7 are sequentially arranged in the sampling box 2 from bottom to top, and a gap is formed between the gasket 3 and the adsorbing material 7; the metal support 11 is perpendicular to the ground, the bottom of the metal support is in a tip shape, the height direction of the metal support is provided with openings, and the sampling box 2 is fixed on the metal support 11 through the openings on the metal support 11 by the metal bandage 12.
The diameter of the opening of the bottom cover 6 is smaller than that of the sampling box 2, and the opening is used for supporting the adsorbing material 7 in the sampling box 2, fixing the coarse screen 5, the fine screen 4 and the gasket 3 and facilitating the inflow of sampling gas.
Adsorbing material 7 is circular shape polyurethane foam, and its diameter is greater than the 2 internal diameters of sampling box, guarantees that the two closely laminates, and its highly is less than 2 high 2cm of sampling box, and adsorbing material 7 bottom is apart from bottom 62cm during the installation, further avoids the interference of granule looks.
The coarse screen 5 is 10 meshes; the fine screen 4 is 200 meshes; the two materials are both stainless steel, the shape is circular, and the diameter is consistent with the inner diameter of the bottom cover 6; the gasket 3 plays a role in sealing, is made of polytetrafluoroethylene and is in a ring shape, the outer diameter of the gasket is consistent with the inner diameter of the bottom cover 6, and the inner diameter of the gasket is consistent with the inner diameter of the opening of the bottom cover 6.
The connecting cylinder 9 is cylindrical and mainly made of stainless steel, threads are arranged inside an opening at the top of the connecting cylinder 9, and the blast cap 8 is butted with the connecting cylinder 9 through the threads; the sampling box 2 is made of stainless steel.
Five threaded circular holes are uniformly distributed at the bottom of the connecting cylinder 9 or the number of the circular holes is adjusted according to the actual sampling condition; the air pipe joint 1 is screwed with the connecting cylinder 9 through a threaded round hole.
A using method of a passive sampling device of unpowered hood type semi-volatile organic compounds is characterized by comprising the following steps:
before sampling, sequentially carrying out Soxhlet extraction on an adsorbing material 7 by using acetone and dichloromethane, wherein the adsorbing material 7 is polyurethane foam;
step two, drying the extracted adsorbing material 7 in vacuum to remove residual solvent, wrapping with aluminum foil and sealing with a compact bag, and storing in a refrigerator at-20 ℃;
step three, assembling the passive sampling device of the unpowered hood semi-volatile organic compound, vertically inserting the metal bracket 11 into a position which is 10-15cm below the ground of the sampling point, and installing each sampling box 2 according to the specific height of the sampling requirement to ensure that the air inlet at the bottom of each sampling box 2 is parallel to the ground;
and step four, after sampling for 6-24 days, taking out the adsorbing material 7, and performing subsequent treatment, measurement and calculation to obtain a final concentration result.
Compared with the prior art, the invention has the following advantages:
1) the hood is driven to rotate under the action of wind power, so that the air flow in the vertical direction is increased, the gas circulation speed in the sampling boxes is increased, the sampling rate is increased, the sampling time is shortened, the sampling rate of pollutants in the adsorbing materials of each sampling box is approximate to the same rate, and the difference of passive sampling rates caused by the difference of different high environmental conditions is corrected.
2. The air flow in the vertical direction generated by the rotation of the blast cap is weak, so that the disturbance to the air around the sampling point is very small and is far lower than the influence of the active sampler.
3. The passive sampling device has the advantages of simple structure, portability, simple installation, convenient operation, no need of a power supply, and capability of continuously sampling field air at multiple points, multiple heights, medium and short periods.
4. The passive sampling device mainly adsorbs gaseous pollutants, and the existence of the screen further avoids the interference of particles, so that the result is more accurate and reliable.
5. The passive sampling devices are placed at different heights from the ground, so that the air concentration information of the SVOCs at different heights in the vertical direction of the soil is obtained, and the soil-atmosphere diffusion tendency and flux of the SVOCs are further estimated.
6. According to different sampling purposes, the sampling height and the number of the sampling boxes are flexibly set and proper adsorption materials are selected.
Drawings
FIG. 1 is a schematic diagram of a passive sampling device for unpowered hood-type semi-volatile organic compounds according to the present invention;
FIG. 2(a) is a schematic view of a cartridge according to the present invention;
FIG. 2(b) is a schematic view of an adsorbent material according to the present invention;
FIG. 3 is a schematic bottom view of the connector barrel of the present invention;
FIG. 4(a) is a schematic diagram showing the comparison of the sampling rates of the unpowered hood-type semi-volatile organic compound passive sampling device of the present invention and a common passive sampling device for different OPE monomers;
fig. 4(b) is a schematic diagram showing the comparison of the sampling rates of the unpowered hood type semi-volatile organic compound passive sampling device of the present invention and a common passive sampling device for different PAE monomers.
In the figure: 1. the air pipe joint, 2, a sampling box, 3, a gasket, 4, a fine screen, 5, a coarse screen, 6, a bottom cover, 7, an adsorption material, 8, a wind cap, 9, a connecting cylinder, 10, a silicone tube, 11, a metal bracket and 12, a metal binding band.
Detailed Description
The present invention is further described with reference to the accompanying drawings and specific embodiments, and the technical solutions in the embodiments of the present invention are clearly and completely described, it is obvious that the described embodiments are only examples, and do not represent all embodiments of the present invention, and other embodiments of the present invention also belong to the protection scope of the present invention.
The unpowered hood-type passive sampling device for semi-volatile organic compounds shown in fig. 1, fig. 2(a) and fig. 2(b) comprises a hood 8, a connecting cylinder 9, a metal bracket 11, a sampling box 2, an adsorption material 7, a silicone tube 10, a gasket 3, a fine screen 4 and a coarse screen 5. 8 lower extremes of hood link to each other with connecting cylinder 9, 9 bottoms of connecting cylinder link to each other with metal support 11, connecting cylinder bottom installation air pipe joint 1 passes through silicone tube 10 with the air pipe joint 1 at 2 tops of sampling box and is connected, plays the effect of air circulation with higher speed.
The sampling boxes 2 are fixed on the metal bracket 11 at different heights; 2 bottom openings of sampling box, and bottom clasp tightly take the bottom 6 of circular trompil, supreme the installing on bottom 6 is followed down in proper order to coarse screen 5, fine screen 4, gasket 3, and coarse screen 5 and fine screen 4 have the effect of holding back atmospheric particulates and other impurity, and gasket 3 plays sealed effect, prevents that the particulate matter from getting into inside sampling box 2 from screen cloth and lid gap. The adsorbing material 7 is in close contact with the inner wall of the sampling box 2, so that a gap is prevented from being left; the adsorption material 7 is polyurethane foam, has a good adsorption effect on semi-volatile organic compounds, and can well reflect the concentration of the semi-volatile organic compounds in ambient air.
In a preferred embodiment, the diameter of the hood 8 is 15cm, the diameter of the joint of the bottom of the hood and the connecting cylinder 9 is 10cm, and the hood and the connecting cylinder are made of stainless steel.
The connecting cylinder 9 is cylindrical, is made of stainless steel, has the diameter of 10cm and the height of 15cm, is provided with an opening at the top end, is provided with threads at the opening, is connected with the bottom of the blast cap 8, and is connected with five stainless steel gas pipe joints 1 at the bottom. Meanwhile, the lower end of the connecting cylinder 9 is welded with a rectangular steel plate with a hole, so that the connecting cylinder is convenient to fix on the metal bracket 11.
The sampling box 2 and the connecting cylinder 9 in the embodiment are connected through a silicone tube 10, and the inner diameter of the silicone tube 10 is 8cm and the outer diameter is 12 cm.
FIG. 2(a) is a schematic view of the internal structure of a sampling box 2, wherein the sampling box 2 is made of stainless steel, has an inner diameter of 8cm and a height of 8cm, and is covered with a threaded opening for connecting with a gas pipe connector 1; the lower end of the stainless steel bottom cover is open, the stainless steel bottom cover 6 is fastened, the inner diameter of the bottom cover 6 is 8cm, the bottom cover 6 is provided with a circular opening with the diameter of 7cm, the bottom cover 6 is provided with a side edge with the thickness of 0.5cm and is used for mounting a coarse screen 5, a fine screen 4 and a polytetrafluoroethylene gasket 3 from bottom to top; wherein the coarse screen 5 is 10 meshes and has the diameter of 8 cm; the fine screen 4 is 200 meshes and has the diameter of 8 cm; the gasket 3 is annular, the outer diameter is 8cm, and the inner diameter is 7.5 cm; the trompil of bottom 6 is convenient for the air current to get into 2 inside and the contact of adsorption material 7 of sampling box, and the inside polyurethane foam adsorption material of closely installing of sampling box 2 prevents that it from leaving the gap with the sampling box inner wall. Coarse screen 5 and fine screen cloth 4 material are the stainless steel, and the two all plays support, filtering action, prevents particulate matter, soil, raise dust, insect and other solid impurity etc. and gets into sampling box 2 in, makes the air evenly get into inside sampling box 2 simultaneously, and gasket 3 plays sealed effect, prevents that the particulate matter from passing through screen cloth and 6 gaps in the bottom and getting into inside sampling box 2.
The sampling adsorption material 7 material is polyurethane foam, and the shape is cylindrical, and the size is diameter 8cm, and height 6cm, and 2cm bottom apart from the sampling box in adsorption material 7 bottom during the installation, further prevent the interference of particulate matter and rainwater etc..
The metal support 11 selects an angle iron support with the height of 165cm, holes are uniformly distributed in the two side pieces, the sampling box 2 is fixed by the metal binding belt 12, the bottom 15cm of the metal support 11 is sharpened, and the metal support is inserted into soil for 15cm deep and used for fixing the sampling device.
The sampling method of the unpowered hood type semi-volatile organic matter passive sampling device comprises the following steps:
before sampling, the sampling box 2, the coarse screen 5, the fine screen 4, the gasket 3 and the like are placed in water added with detergent for soaking for 24 hours, then are washed clean by flowing tap water, are rinsed for 3 times by ultrapure water, are placed in an oven for drying, and the cleanness of the sampler is ensured.
Before sampling, the polyurethane foam of the adsorption material 7 is subjected to Soxhlet extraction for 72 hours by sequentially adopting acetone and dichloromethane, and the sampling material is purified to remove a background value; and after extraction, putting the polyurethane foam into a vacuum drier, vacuumizing and drying to volatilize the solvent, finally wrapping with aluminum foil paper, putting into a sealing bag, and storing in a refrigerator at the temperature of minus 20 ℃.
Before the sampling begins, assemble sampling device according to the form of figure 1, insert 15cm in the soil with metal support 11 bottom pointed end, make sampling device keep stable, the sample box is assembled according to figure 2(a) mode, utilize tweezers to hug closely adsorption material 7 inner wall and put into each sample box 2, fix sample box 2 to metal support 11 on the different height according to the demand, sample box 2 lower extreme is on a parallel with ground, begin the sampling.
After sampling, the adsorbing material 7 is taken out by tweezers, wrapped by aluminum foil, put into a sealing bag and stored in a refrigerator.
Extracting the semi-volatile organic pollutants collected by the adsorption material 7 by using an accelerated solvent extraction instrument after sampling is finished, blowing extraction liquid nitrogen to less than 1ml, then enabling an extracting solution to pass through a silica gel column, filling the silica gel column with anhydrous sodium sulfate and 3% deactivated silica gel, and mixing n-hexane: eluting with solvent of 1:1 dichloromethane, collecting eluate, concentrating under nitrogen blowing, replacing solvent, adding internal standard substance, and detecting on machine.
And (3) analyzing and detecting the sample, and quantifying by using an internal standard method according to the collected molecular ion peak of each semi-volatile organic pollutant.
The beneficial effect of the unpowered hood-type passive sampler for semi-volatile organic compounds in practical application is verified through a specific embodiment of the invention.
The experimental site is the outdoor roof of the environmental institute of university of great university of great university of great university of great university of university, the great university of great university of great university of great university of great university of great.
Two passive sampling devices of the unpowered hood and the semi-volatile organic compounds are placed at the same height, sampling is carried out for 30 days, and no shielding is generated around the placement environment. Sampling device for semi-volatile organic compounds of each unpowered hoodFive passive samples are collected, a common non-improved passive sampler is arranged at the same height to collect the passive samples, the passive samples and the common passive samples of the unpowered hood type semi-volatile organic matter passive sampling device are respectively recovered every six days, meanwhile, a large-flow active sampler (with the flow rate of 100L/min) is used for synchronously collecting the total suspended particulate matter TSP (GF/A glass filter membrane which is calcined at 450 ℃ for 4h) and the gaseous samples (PUF with the diameter of 6.5cm and the height of 7.5cm) at the same height at the position 3m away from the passive sampling device, the filter membrane and the PUF samples which are actively sampled at a large flow are collected every 6 days, and each sample approximately collects 1000m3Air. And calculating the sampling rates of the unpowered hood semi-volatile organic matter passive sampler and the ordinary passive sampler by comparing the concentrations of the passive sampler and the active sampler.
The experiment respectively calculates the average sampling rate of 11 OPE monomers and 10 PAE monomers of two samplers within 30 days, for comparison, the sampling rate is the average sampling rate of all the monomers, and the result shows that the sampling rate of the improved unpowered hood semi-volatile organic matter passive sampling device is increased by 25% compared with the sampling rate of a common passive sampler.
TABLE 1 unpowered funnel cap comparison of sampling rates (OPE) for semi-volatile organic passive sampler and ordinary passive sampler
TABLE 2 unpowered funnel cap comparison of sampling rate of semi-volatile organic passive sampler with ordinary passive sampler (PAE)
Claims (6)
1. A passive sampling device of unpowered hood type semi-volatile organic compounds is characterized by comprising a hood (8), a connecting cylinder (9), a metal bracket (11), a sampling box (2), an adsorption material (7), a silicone tube (10), a gasket (3), a fine screen (4) and a coarse screen (5); the upper end of the connecting cylinder (9) is opened and is in threaded connection with the blast cap (8), the lower end of the connecting cylinder is closed and is provided with a plurality of air pipe connectors (1), the air pipe connectors and the blast cap are screwed tightly through threads, and the bottom of the connecting cylinder (9) is connected with the metal bracket (11); the top of the sampling box (2) is provided with a threaded round hole and is in threaded connection with the air pipe joint (1), and the air pipe joint (1) on the connecting cylinder (9) is connected with the air pipe joint (1) on the sampling box (2) through a silicone tube (10); a bottom cover (6) with a hole is arranged at an opening at the bottom of the sampling box (2); a coarse screen (5), a fine screen (4), a gasket (3) and an adsorbing material (7) are sequentially arranged in the sampling box (2) from bottom to top, and a gap exists between the gasket (3) and the adsorbing material (7); the metal support (11) is perpendicular to the ground, the bottom of the metal support is in a tip shape, the height direction of the metal support is provided with openings, and the sampling box (2) is fixed on the metal support (11) through the openings in the metal support (11) by the metal binding bands (12).
2. The passive sampling device for semi-volatile organic compounds with unpowered hood as claimed in claim 1, wherein the diameter of the opening of the bottom cover (6) is smaller than that of the sampling box (2) for holding the adsorbing material (7) in the sampling box (2), and fixing the coarse screen (5), the fine screen (4) and the gasket (3) and simultaneously facilitating the inflow of the sampling gas.
3. The passive sampling device for semi-volatile organic compounds of unpowered hood as claimed in claim 1, wherein the adsorbing material (7) is circular polyurethane foam, the diameter of the polyurethane foam is larger than the inner diameter of the sampling box (2) to ensure that the polyurethane foam and the sampling box are tightly attached, the height of the polyurethane foam is smaller than the height of 2cm of the sampling box (2), the bottom of the adsorbing material (7) is 2cm away from the bottom cover (6) during installation, and therefore interference of particle phases is further avoided.
4. The unpowered hood semi-volatile organic matter passive sampling device of claim 1, wherein the coarse screen (5) is 10 mesh; the fine screen (4) is 200 meshes; the two materials are both stainless steel, the shape is circular, and the diameter is consistent with the inner diameter of the bottom cover (6); the gasket (3) is made of polytetrafluoroethylene and is in a ring shape, the outer diameter of the gasket is consistent with the inner diameter of the bottom cover (6), and the inner diameter of the gasket is consistent with the inner diameter of the opening of the bottom cover (6).
5. The unpowered hood-type passive sampling device for semi-volatile organic compounds according to claim 1, characterized in that the connecting cylinder (9) is cylindrical and is mainly made of stainless steel; the sampling box 2 is made of stainless steel.
6. The use method of the unpowered hood type passive sampling device for semi-volatile organic compounds according to any one of claims 1 to 5, characterized by comprising the following steps:
firstly, before sampling, sequentially carrying out Soxhlet extraction on an adsorbing material (7) by using acetone and dichloromethane, wherein the adsorbing material (7) is polyurethane foam;
step two, drying the extracted adsorbing material (7) in vacuum to remove residual solvent, wrapping with aluminum foil and sealing with a compact bag, and storing in a refrigerator at-20 ℃;
step three, assembling the passive sampling device for the unpowered hood semi-volatile organic compounds, vertically inserting the metal support (11) into a position which is 10-15cm below the ground of a sampling point, installing each sampling box (2) according to the specific height required by sampling, and ensuring that an air inlet at the bottom of each sampling box (2) is parallel to the ground;
and step four, after sampling for 6-24 days, taking out the adsorption material (7), and performing subsequent treatment, measurement and calculation to obtain a final concentration result.
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