CN110542599A - device and method for collecting plant source volatile organic compounds - Google Patents
device and method for collecting plant source volatile organic compounds Download PDFInfo
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- CN110542599A CN110542599A CN201910795008.4A CN201910795008A CN110542599A CN 110542599 A CN110542599 A CN 110542599A CN 201910795008 A CN201910795008 A CN 201910795008A CN 110542599 A CN110542599 A CN 110542599A
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- G01N1/22—Devices for withdrawing samples in the gaseous state
- G01N1/2202—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling
- G01N1/2214—Devices for withdrawing samples in the gaseous state involving separation of sample components during sampling by sorption
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Abstract
The invention belongs to the technical field of detection, and particularly relates to a device and a method for collecting plant-derived volatile organic compounds. The collecting device comprises a gas circulation system formed by sequentially connecting an atmosphere sampling instrument, a sealing bag for wrapping plants, a allochroic silica gel drying tower and an active carbon drying tower; wherein, the air outlet of the atmosphere sampling instrument is connected with the air inlet pipe at the top of the active carbon drying tower; the bottom air outlet of the activated carbon drying tower is connected with the top air inlet pipe of the allochroic silica gel drying tower; the bottom air outlet of the allochroic silica gel drying tower is connected with the bottom hole pipe of the sealing bag for wrapping the plants; and the top hole of the sealing bag for wrapping the plants is connected with an air inlet pipe of the atmosphere sampling instrument. The method has the advantages of being more convenient and faster in operation process and more accurate in experimental result, reducing unnecessary errors, saving resources, completing acquisition of BVOCs released by living plants more efficiently, and contributing to purification of forestry environment.
Description
Technical Field
the invention belongs to the technical field of detection, and particularly relates to a device and a method for collecting plant-derived volatile organic compounds.
Background
the traditional collection method of plant-derived volatile organic compounds (BVOCs) mainly comprises the following steps: steam distillation, solvent extraction, liquid nitrogen condensation, and the like.
in recent years, in order to collect the VOCs from plants in the natural state as much as possible, researchers have developed a novel extraction method, which mainly includes: dynamic headspace collection, solid phase microextraction, supercritical fluid extraction, and the like.
In the novel method, the dynamic headspace collection method is mainly used for collecting BVOCs of living plants in a natural state; according to the size difference of the collected objects, the method can be divided into three modes of horizontal collection of the whole plant, branches and leaves.
however, in the actual sampling process, the dynamic headspace acquisition method has the following problems:
1) The use is limited: the sealing bag used by the method at present is a specific Reynolds microwave oven bag, and the purchase way of the microwave oven bag is narrow, so that the method is inconvenient to popularize and use;
2) The error is large: in the method, gas is purified by an active carbon drying tower at present, and although the active carbon is dried at high temperature, the filtering effect is general; meanwhile, in the existing method, Tenax-TA is used as an adsorbent, so that more impurities exist; these problems lead to large experimental errors;
3) The operation is complicated: before and after the implementation of the method, complicated preparation work and post-treatment work are required to be carried out on the adsorbent material Tenax-TA; the preparation steps before implementation are as follows:
Soaking and cleaning with acetone, wherein the amount of the acetone is 100ml/g, and chloride or aromatic compounds are not used;
② filling the adsorbent into a chromatographic column, and leaching with 20ml of acetone;
③ blowing and drying 20ml/min of high-purity nitrogen at room temperature;
fourthly, washing with methanol, wherein the using amount of the methanol is 100 ml/g;
Blowing and drying at room temperature by using high-purity nitrogen of 20 ml/min;
Sixthly, putting the chromatographic column into a gas chromatographic column box, drying for 2 hours at 270 ℃, wherein the flow rate of N2 is 100 ml/min; the dried adsorbent was packed in separate adsorption tubes (16 cm in length, 3mm in inner diameter, manufactured by Chrompack, Inc., in an amount of 180 mg).
and sealing two ends of the adsorption tube by using a polytetrafluoroethylene (Teflon) cover.
The post-treatment working steps after implementation are as follows:
the adsorption tube to be activated is installed before GC, and the tube number, the activation date and time are recorded. Connecting an adsorption tube to be activated with a sample inlet in a gas chromatographic column box, introducing N2 (flow rate of 100ml/min), and checking airtightness by using soapy water; keeping for 2.5h after the temperature of the column box rises to 270 ℃, then cooling to below 100 ℃, sealing two ends of the adsorption tube by polytetrafluoroethylene (Teflon) covers, putting the adsorption tube into a box for standby, and sealing without plastic or rubber.
the invention is especially provided in view of the problems of the existing dynamic headspace collection method.
Disclosure of Invention
In order to overcome the defects, the invention provides a novel collecting device for plant-derived volatile organic compounds. The existing dynamic headspace collection method is improved, so that the operation process is more convenient and faster, the experimental result is more accurate, unnecessary errors are reduced, and resources are saved, so that the BVOCs released by living plants are collected more efficiently, and the forestry environment is purified to contribute to one strength.
The plant source volatile organic compound collecting device comprises a gas circulation system formed by sequentially connecting an atmosphere sampling instrument, a sealing bag for wrapping plants, a allochroic silica gel drying tower and an active carbon drying tower; wherein the content of the first and second substances,
The air outlet of the atmosphere sampling instrument is connected with the air inlet pipe at the top of the active carbon drying tower;
The bottom air outlet of the activated carbon drying tower is connected with the top air inlet pipe of the allochroic silica gel drying tower;
the bottom air outlet of the allochroic silica gel drying tower is connected with the bottom hole pipe of the sealing bag for wrapping the plants;
and the top hole of the sealing bag for wrapping the plants is connected with an air inlet pipe of the atmosphere sampling instrument.
according to the invention, the allochroic silica gel drying tower is additionally arranged on the basis of the existing dynamic headspace collecting device, and the gas is limited to pass through the allochroic silica gel drying tower and then pass through the active carbon drying tower, so that the synergistic effect of the allochroic silica gel drying tower and the active carbon drying tower can be exerted to the greatest extent, the filtering effect of the gas is obviously improved, the error is reduced, and the collecting accuracy is improved.
An adsorption tube is further arranged in a connecting tube of the atmosphere sampling instrument and the sealing bag for wrapping the plants, and the adsorption tube is filled with Tenax-GR.
The sealing bag for wrapping the plants is selected from food-grade PE plastic bags.
In order to ensure the collection effect, a switch A is arranged on a connecting pipe between the atmosphere sampling instrument and the sealing bag for wrapping the plants; and a switch B is arranged on a connecting pipe between the sealing bag for wrapping the plants and the allochroic silica gel drying tower. During actual collection, technicians adjust the switch to realize air suction and inflation. Further, the switches a and B may be manually/automatically operated.
the invention also provides a method for collecting plant source volatile organic compounds by using the device, which comprises the following steps: and circularly pumping and inflating, collecting and recording.
In the collection process, the sampling flow is 10-200 ml/min; the sampling volume is greater than 1L.
In order to obtain better collection effect, before collection, the collection device is pretreated, including air extraction and air refilling; wherein the content of the first and second substances,
Air extraction: selecting branches and leaves which comprise a sunny leeward side of a crown and are healthy and non-incised as collection objects, and installing the device; opening the switch A, closing the switch B, simultaneously opening the atmosphere sampler, and starting to extract air until the air in the sealing bag is basically not available;
And (3) inflating: opening switch B, closing switch A, simultaneously opening the atmosphere sampling instrument, and starting to inflate until the gas volume in the sealing bag reaches 1/2-3/4 of the total volume of the sealing bag, preferably 2/3;
in order to ensure the collection effect, the processes of air suction and air inflation can be repeated, the last time is sufficient, the atmosphere sampling instrument is reset, and the standing is carried out for 10 min;
After the sample is collected, the adsorption tube is quickly taken down, the copper caps at two ends of the adsorption tube are screwed down, and a layer of tin foil paper is wrapped outside the adsorption tube for later use.
And recording information such as sampling point positions, time, environment temperature, atmospheric pressure, wind speed, flow, adsorption tube numbers and the like, and taking the information to a laboratory for analysis.
In order to obtain better collection effect, the collection method should be carried out by selecting sunny and windless weather; the day before sampling ensures that no strong wind and heavy rain exist, and the air humidity of the day of sampling is also lower than 60%.
The invention has the following beneficial effects:
1) The method selects the allochroic silica gel drying tower to be matched with the active carbon drying tower, so that the experimental result is more accurate.
2) The invention adopts the Tenax-GR adsorption material which contains more active carbon components, can simplify the experimental steps in the operation process and improve the accuracy of the experimental result.
3) The method adopts the food-grade PE thickened plastic bag as the sealing bag, ensures the sealing quality requirement, has low cost and easy replacement, does not need to be cleaned every time, and thus can avoid the problem that the experimental result is influenced by improper operation in the cleaning process.
drawings
FIG. 1 is a schematic drawing of the evacuation of the collection method of the present invention.
Fig. 2 is a schematic view of the inflation of the acquisition method of the present invention.
Fig. 3 is a schematic acquisition diagram of the acquisition method of the present invention.
Detailed Description
the following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
example 1
The embodiment provides a BVOCs collecting device, which comprises a gas circulation system, a first collecting device and a second collecting device, wherein the gas circulation system is formed by sequentially connecting an atmosphere sampling instrument, a sealing bag for wrapping plants, a color-changing silica gel drying tower and an active carbon drying tower; wherein the content of the first and second substances,
the air outlet of the atmosphere sampling instrument is connected with the air inlet pipe at the top of the active carbon drying tower;
The bottom air outlet of the activated carbon drying tower is connected with the top air inlet pipe of the allochroic silica gel drying tower;
The bottom air outlet of the allochroic silica gel drying tower is connected with the bottom hole pipe of the sealing bag for wrapping the plants;
And the top hole of the sealing bag for wrapping the plants is connected with an air inlet pipe of the atmosphere sampling instrument.
Furthermore, the acquiring further comprises:
An adsorption tube is further arranged in a connecting tube of the atmosphere sampling instrument and the sealing bag for wrapping the plants, and the adsorption tube is filled with Tenax-GR.
The sealing bag for wrapping the plants is selected from food-grade PE plastic bags.
A switch A is arranged on a connecting pipe of the atmosphere sampling instrument and the sealing bag for wrapping the plants; and a switch B is arranged on a connecting pipe between the sealing bag for wrapping the plants and the allochroic silica gel drying tower. During actual collection, technicians adjust the switch to realize air suction and inflation.
further, the switches a and B may be manually/automatically operated.
example 2
The embodiment provides an acquisition method of BVOCs, which includes: and circularly pumping and inflating, collecting and recording.
As shown in fig. 1, 2 and 3, the specific steps are as follows:
1) sampling weather: sampling is carried out in sunny and windless weather, the condition that no strong wind and heavy rain exist in the days before sampling is guaranteed, and the air humidity in the sampling day is also lower than 60%.
2) Sampling flow and sampling time: 200ml/min, the sampling volume reached 2/3 of the total volume of the sealed bag.
3) Air extraction: selecting healthy and non-incised branches and leaves with the height of 1.5m on the sunny and leeward side of the crown; connecting the device, opening the switch A, closing the switch B, simultaneously opening the atmosphere sampler, and starting to extract air until the air in the sealing bag is basically not available;
4) and (3) inflating: and opening the switch B, closing the switch A, simultaneously opening the atmosphere sampling instrument, and starting to inflate until the gas volume in the bag reaches about 2/3 of the total volume of the bag.
5) and (3) circulation: repeating the processes of air suction and air inflation for 3 times, ensuring sufficient air for the last time, resetting the atmosphere sampling instrument, and standing for 10 min.
6) collecting: and inserting the activated adsorption tube filled with Tenax-GR into the middle of the tube, and opening the switch A and the switch B to form a closed loop in the whole experiment. And adjusting the time of the atmosphere sampler to 20min for sampling, and adjusting the flow meter to rotate until the gas flow is 200 ml/min.
7) recording: after the sample is collected, the adsorption tube is quickly taken down, copper caps at two ends of the adsorption tube are screwed down, and a layer of tin foil paper is wrapped outside the adsorption tube;
The information was recorded and the results are shown in Table 1.
the specific information is as follows,
Daily extraction: 6 and 18 months in 2019.
And (3) tree species: cortex pini koraiensis.
TABLE 1
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (7)
1. A plant source volatile organic compound collection device is characterized by comprising a gas circulation system formed by sequentially connecting an atmosphere sampling instrument, a sealing bag for wrapping plants, a allochroic silica gel drying tower and an active carbon drying tower; wherein the content of the first and second substances,
the air outlet of the atmosphere sampling instrument is connected with the air inlet pipe at the top of the active carbon drying tower;
the bottom air outlet of the activated carbon drying tower is connected with the top air inlet pipe of the allochroic silica gel drying tower;
The bottom air outlet of the allochroic silica gel drying tower is connected with the bottom hole pipe of the sealing bag for wrapping the plants;
And the top hole of the sealing bag for wrapping the plants is connected with an air inlet pipe of the atmosphere sampling instrument.
2. The collection device according to claim 1, wherein an adsorption tube is further arranged in a connecting tube of the atmosphere sampler and the plant-wrapping sealing bag, and the adsorption tube is filled with Tenax-GR.
3. The harvesting device of claim 1 or 2, wherein the sealed bag enclosing the plant is selected from food grade PE plastic bags.
4. The collecting device according to any one of claims 1 to 3, wherein a switch A is arranged on a connecting pipe between the atmosphere sampling instrument and the sealing bag for wrapping the plants; and a switch B is arranged on a connecting pipe between the sealing bag for wrapping the plants and the allochroic silica gel drying tower.
5. A method for collecting plant-derived volatile organic compounds using the collecting device according to any one of claims 1 to 4, comprising: and circularly pumping and inflating, collecting and recording.
6. The collection method according to claim 5, wherein in the collection process, the sampling flow is 10-200 ml/min; the sampling volume is greater than 1L.
7. the method of claim 6, wherein the collection device is pre-treated prior to collection, including evacuation and re-aeration; wherein the content of the first and second substances,
Air extraction: selecting branches and leaves which comprise the sunny and leeward sides of tree crowns and are healthy and have no nicks as collection objects; after the connecting device is connected, the switch A is opened, the switch B is closed, the atmospheric sampler is opened at the same time, and air starts to be pumped until the air is basically not contained in the sealing bag;
And (3) inflating: opening switch B, closing switch A, simultaneously opening the atmosphere sampling instrument, and starting to inflate until the gas volume in the sealing bag reaches 1/2-3/4 of the total volume of the sealing bag, preferably 2/3;
Repeating the processes of air suction and air inflation, fully inflating for the last time, resetting the atmosphere sampling instrument, and standing for 10 min.
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Cited By (4)
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| CN112285236A (en) * | 2020-10-22 | 2021-01-29 | 山西林业职业技术学院 | Method for detecting herbaceous peony volatile substances |
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| CN113092647A (en) * | 2021-04-09 | 2021-07-09 | 江苏省林业科学研究院 | Non-damage collection and quantitative analysis method for plant volatile matter |
| CN117367899A (en) * | 2023-12-08 | 2024-01-09 | 河北科技大学 | Portable living plant VOCs releases sampling device |
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