CN215414675U - Adsorption tube for thermal desorption instrument - Google Patents
Adsorption tube for thermal desorption instrument Download PDFInfo
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- CN215414675U CN215414675U CN202022479476.1U CN202022479476U CN215414675U CN 215414675 U CN215414675 U CN 215414675U CN 202022479476 U CN202022479476 U CN 202022479476U CN 215414675 U CN215414675 U CN 215414675U
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Abstract
An adsorption tube for a thermal desorption instrument comprises a tube body and adsorption filler, and is characterized in that the adsorption tube comprises the adsorption tube body and loaded graphene filler; the adsorption tube body sequentially comprises a screen layer, an adsorption resin film layer, an adsorption packing layer, an adsorption resin film layer and a screen layer, wherein the adsorption packing layer is a loaded graphene packing layer; the inner wall of the adsorption pipe body is an inert coating.
Description
Technical Field
The utility model relates to a adsorption tube, in particular to an adsorption tube for a thermal analyzer.
Background
Polycyclic Aromatic Hydrocarbons (PAHs) are a class of Persistent Organic Pollutants (POPs) that are ubiquitous in the environment. Mainly exists in petroleum products, rubber, plastics, incompletely combusted compounds and the like. PAHs have high lipid solubility, are not easy to degrade and easily accumulate in organisms, have carcinogenic, teratogenic and mutagenic effects, seriously threaten the environment and human health, and become one of the key environmental monitoring objects. Therefore, the method has great significance for detecting the content of PAHs in materials and the environment.
The sampling of polycyclic aromatic hydrocarbon compounds in ambient air generally adopts a Summa tank sampling technology or an adsorption tube concentration method. The adsorption tube concentration method for sampling is a widely used sampling technology at present due to the characteristics of simple equipment, easy operation, long sample preservation time and the like.
The adsorbents commonly used in the adsorption tube of the thermal desorption instrument at present comprise activated carbon, Tenax adsorbents and the like, the collected sample is subjected to solvent desorption or thermal desorption, and the polycyclic aromatic hydrocarbon adsorbed on the solid adsorbent is transferred to a gas chromatograph for analysis. However, the adsorption tubes using activated carbon and Tenax as adsorbents have poor selectivity to specific species, and the species of adsorbed substances are wide, thereby causing mutual interference in the test process. Graphene is a polymer made of carbon atoms in sp2The two-dimensional carbon nanomaterial with a hexagonal honeycomb crystal structure formed by the hybrid tracks has high mechanical strength and chemical stability, and has wide development prospects in the fields of electronics, photonics, energy, environmental protection, biomedical health and the like. In the field of environmental protection, graphene as a novel efficient adsorption material has higher specific surface area and larger adsorption capacity and faster adsorption response compared with common adsorbents such as activated carbon, zeolite, mesoporous materials, resin and high molecular polymers, and has the characteristics of simple preparation process and the like compared with other adsorption materials such as Carbon Nanotubes (CNTs), and the like, and has great application prospects in the fields of environmental protection, materials and the like. Sp of graphene2The hybridized planar structure can have special adsorption response to polycyclic aromatic hydrocarbon through pi-pi interaction and has strong selective adsorption capacity to organic compounds of the type.
However, the production cost of graphene materials is high, and thus, graphene materials become one of barriers for large-scale application. According to the utility model, the loaded graphene filler is prepared by adopting an impregnation method, and the loaded graphene is used as an adsorbent to manufacture a corresponding adsorption tube for selectively adsorbing the polycyclic aromatic hydrocarbon compound in a sample, so that the graphene can be rapidly contacted with gas to realize effective adsorption, the cost of the adsorption tube can be reduced, the production process is simple, and the novel graphene adsorption tube is beneficial to popularization and application.
SUMMERY OF THE UTILITY MODEL
In order to solve the problem that the selective adsorption of polycyclic aromatic hydrocarbon compounds is difficult in the prior art, the utility model provides an adsorption tube for a thermal desorption instrument.
The utility model relates to an adsorption tube for a thermal desorption instrument, which comprises a tube body and adsorption filler; the adsorption tube comprises an adsorption tube body and a loaded graphene filler; the adsorption tube body sequentially comprises a screen layer, an adsorption resin film layer, an adsorption packing layer, an adsorption resin film layer and a screen layer, wherein the adsorption packing layer is a loaded graphene packing layer; the inner wall of the adsorption pipe body is an inert coating.
Further, the air conditioner is provided with a fan,
the loading length of the loaded graphene filler of the adsorption filler layer is preferably 30-60mm, and more preferably 35-50 mm;
the loading amount of the loaded graphene filler in the adsorption filler layer is preferably 90-140mg, and more preferably 100-120 mg.
The above-mentioned sieve mesh layer comprises a glass wool layer and/or a stainless steel sieve mesh layer, preferably a combination of a stainless steel sieve mesh layer and a glass wool layer, and the glass wool layer is within the stainless steel sieve mesh layer.
The pore size range of the mesh layer is preferably 100-150 meshes, and more preferably 100-130 meshes;
the thickness of the above-mentioned screen layer is preferably 1mm to 10mm, more preferably 1mm to 5 mm.
The resin film layer preferably comprises a polytetrafluoroethylene film layer;
the adsorption filler layer is preferably a graphene-loaded quartz fiber cotton filler layer.
The above-mentioned resin film layer is preferably 0.1mm to 5mm in thickness, more preferably 0.4 to 1mm in thickness;
the pore diameter range of the membrane is preferably 0.1-3 μm, more preferably 0.3-1 μm;
the film of the above-mentioned resin film layer is preferably 1 to 9 layers, more preferably 2 to 5 layers.
In a preferred embodiment of the present invention, the adsorption pipe body is a curved pipe.
The inlet and the outlet of the adsorption tube preferably have a height difference, the height difference preferably ranges from 5mm to 30mm, more preferably ranges from 15mm to 25mm, and the inlet end is lower than the outlet end.
The length range of the adsorption tube body is preferably 80-140 mm; the pipe diameter range of the pipe body is preferably 5-10 mm.
The adsorption tube for the thermal desorption instrument can adsorb and enrich the polycyclic aromatic hydrocarbon compound from various samples such as environment, materials and the like with high selectivity, and the content of the polycyclic aromatic hydrocarbon compound in the samples can be efficiently and accurately analyzed and measured through the thermal desorption instrument-gas chromatography or the thermal desorption instrument-gas chromatograph-mass spectrometer.
Drawings
FIG. 1 is a schematic structural diagram of the present invention.
2-a screen layer; 3-an adsorption resin film layer; 4-an adsorption packing layer.
Fig. 2 is a total ion flow chromatogram of a mixed sample of petroleum ether and a polycyclic aromatic hydrocarbon compound obtained by the supported graphene adsorption tube in example 1.
FIG. 3 is a total ion flow chromatogram of a mixed sample of petroleum ether and a polycyclic aromatic hydrocarbon compound obtained from a commercial Tenax sorbent tube in comparative example 1.
Detailed Description
While the present invention will be described in detail with reference to the following examples, it should be understood that the following examples are illustrative of the present invention and are not to be construed as limiting the scope of the present invention.
The adsorption tube for the thermal desorption instrument comprises a tube body and adsorption filler, the adsorption tube comprises an adsorption tube body and load type graphene filler, the inner wall of the adsorption tube body is an inert coating, and the adsorption tube body sequentially comprises a screen layer, an adsorption resin film layer, an adsorption filler layer, an adsorption resin film layer and a screen layer.
In the technical scheme, the adsorption filler layer is a loaded graphene filler layer, and the loading length of the adsorption filler layer is 30-60mm, preferably 35-50 mm; the loading amount is 90-140mg, preferably 100-120 mg.
The load type graphene filler can be the existing load type graphene filler in the prior art, preferably is quartz fiber cotton loaded with graphene, and is prepared by the following method: (1) ultrasonically dispersing graphene in water and/or ethanol to serve as mother liquor for later use; (2) and (2) soaking the quartz fiber cotton in the mother liquor obtained in the step (1), standing for a period of time, taking out the quartz fiber cotton, and drying in a muffle furnace to obtain the graphene-loaded quartz fiber cotton filler. The adsorption tube prepared by the loaded graphene filler has special adsorption response to polycyclic aromatic hydrocarbon and has strong selective adsorption capacity to organic compounds of the type.
In the above technical solution, the mesh layer includes a glass wool layer and/or a stainless steel mesh layer, preferably a combination of a stainless steel mesh layer and a glass wool layer, and the glass wool layer is within the stainless steel mesh layer. The mode of combining the two screens is adopted, so that the adsorption can be more sufficient.
The aperture range of the sieve layer is 100-150 meshes, preferably 110-140 meshes; the thickness of the screen layer is 1mm-10mm, preferably 1-5 mm.
In the technical scheme, the resin film layer comprises a polytetrafluoroethylene film layer, and the thickness of the resin film layer is 0.1-5 mm, preferably 0.4-1 mm; the pore diameter range of the membrane is 0.1-3 μm, preferably 0.3-1 μm; the film of the resin film layer has 1 to 9 layers, preferably 2 to 5 layers.
In the above technical scheme, the adsorption tube body can be selected from a stainless steel tube or a glass tube, and preferably, the inner wall of the adsorption tube body is an inert coating.
The adsorption tube is preferably a bent pipeline, the left end and the right end of the adsorption tube have a height difference, and the height difference ranges from 5mm to 30mm, preferably from 15mm to 25 mm. The bent part of the adsorption tube is preferentially arranged at the position where the middle is filled with the adsorption filler layer. The crooked setting of adsorption tube and the difference in height setting of controlling both ends more are favorable to gaseous velocity of flow to accelerate, make to adsorb more abundant.
In the technical scheme, the length range of the adsorption tube body is 80-140 mm; the pipe diameter range is 5-10 mm.
Compared with the prior art, the utility model has the following beneficial effects:
the adsorption tube for the thermal desorption instrument can adsorb and enrich the polycyclic aromatic hydrocarbon compound from various samples such as environment, materials and the like with high selectivity, and the content of the polycyclic aromatic hydrocarbon compound in the samples can be efficiently and accurately analyzed and measured through the thermal desorption instrument-gas chromatography or the thermal desorption instrument-gas chromatograph-mass spectrometer. The method fully exerts the advantage of strong selectivity of the graphene material to the polycyclic aromatic hydrocarbon compound, realizes the application of the graphene material to the adsorption tube of the analytical instrument at low cost, solves the defects in the prior experimental technology, and aims to realize the large-scale application of the graphene material in the field.
The starting materials used in the following examples and comparative examples are commercially available.
Example 1
As shown in fig. 1, the adsorption tube comprises an adsorption tube body and a loaded graphene filler, the adsorption tube is a curved pipeline, the tube body of the adsorption tube is a stainless steel tube with an inert coating on the inner wall, and the outer diameter of the adsorption tube is 6.4mm, and the length of the adsorption tube is 95 mm; the height difference of 15mm is formed at the left end and the right end of the pipe body;
and sequentially filling the screen layer 2, the adsorption resin film layer 3, the adsorption filler layer 4, the adsorption resin film layer 3 and the screen layer 2 into the adsorption tube body to obtain the adsorption tube for the thermal desorption instrument.
The adsorption filler layer is a filler layer of 120mg of graphene-loaded quartz fiber cotton, and the filling length is 50 mm; preparing the graphene-loaded quartz fiber cotton:
(1) taking 1g of graphene, and ultrasonically dispersing the graphene in 100ml of water to serve as mother liquor for later use.
(2) And (2) soaking 200mg of quartz fiber cotton in the mother liquor obtained in the step (1), standing for a period of time, taking out the quartz fiber cotton, and drying in a muffle furnace at 200 ℃ for 2 hours to obtain the supported graphene filler.
The sieve layer 2 adopts a stainless steel sieve mesh with the aperture range of 120 meshes; the thickness of the screen layer is 5 mm.
The resin film layer 3 is a polytetrafluoroethylene film layer with the thickness of 0.4 mm; the pore diameter range of the membrane is 0.3 mu m; the resin film layer is 3 layers.
Example 2
As shown in fig. 1, the adsorption tube comprises an adsorption tube body and a supported graphene filler, the adsorption tube is a curved pipeline, the tube body of the adsorption tube is a stainless steel tube with an inert coating on the inner wall, and the outer diameter of the adsorption tube is 6.4mm, and the length of the adsorption tube is 110 mm; the left end and the right end of the pipe body have a height difference of 25 mm;
and sequentially filling an activated carbon layer 1, a sieve layer 2, an adsorption resin film layer 3, an adsorption filler layer 4, an adsorption resin film layer 3, a sieve layer 2 and the activated carbon layer 1 into the adsorption tube body to obtain the adsorption tube for the thermal desorption instrument.
The adsorption filler layer is a filler layer of 150mg of graphene-loaded quartz fiber cotton, and the filling length is 50 mm; preparing the graphene-loaded quartz fiber cotton:
(1) taking 1g of graphene, and ultrasonically dispersing the graphene in 100mL of ethanol to serve as mother liquor for later use;
(2) and (2) soaking 200mg of quartz fiber cotton in the mother liquor obtained in the step (1), standing for a period of time, taking out the quartz fiber cotton, and drying in a muffle furnace at 200 ℃ for 2 hours to obtain the supported graphene filler.
The screen layer 2 adopts a stainless steel screen and glass wool, the glass wool layer is within the stainless steel screen layer, and the aperture range is 100 meshes; the thickness of the screen layer is 10mm (the thickness of the glass wool layer is 5mm, and the thickness of the stainless steel screen layer is 5 mm).
The resin film layer 3 is a polytetrafluoroethylene film layer with the thickness of 0.7 mm; the pore diameter range of the membrane is 0.5 mu m; the resin film layer is 5 layers.
Example 3
Before use, the adsorption tube is aged for 15min at 300 ℃ to remove gas adsorbed in the adsorption filler.
(1) A1 mu L mixed sample of petroleum ether and polycyclic aromatic hydrocarbon was taken with a microinjector and blown into the graphene adsorption tubes of example 1 or example 2, respectively, under a nitrogen flow purging condition.
(2) The loaded graphene adsorption tubes were tested using a thermal analyzer-gas chromatograph or a thermal analyzer-gas chromatograph-mass spectrometer.
(3) The test conditions of the thermal analyzer-gas chromatograph-mass spectrometer are as follows:
the instrument comprises the following steps: marks thermal Analyzer, United kingdom, Agilent 7890B-7000C GC gas chromatograph-Mass spectrometer, USA.
Thermal resolution conditions: the desorption temperature is 120 ℃, the desorption time is 5min, the cold trap temperature is 0 ℃, and the desorption is carried out at 300 ℃.
Chromatographic conditions are as follows: chromatographic column HP-5MS (30 × 0.25mm × 0.25 μm), temperature programming, starting at 80 deg.C and raising the temperature to 280 deg.C at 15 deg.C/min, and holding the temperature for 10 min. The transfer line temperature was maintained at 200 deg.C with He as carrier gas and a flow rate of 1.0 mL/min.
Mass spectrum conditions: and (3) bombarding an ionization source by electrons, wherein the electron energy is 70eV, the source temperature is 230 ℃, and a full-scanning acquisition mode is adopted, and the mass range is 40-500 amu.
FIG. 2 is a GC-MS total ion flow chromatogram of the sorbent tube of example 1. According to the analysis result, four polycyclic aromatic hydrocarbons, namely acenaphthene, fluorene, fluoranthene and pyrene cannot be detected, and no interference peak brought by petroleum ether exists in the chromatogram.
Comparative example 1
(1) The petroleum ether and polycyclic aromatic hydrocarbon mixed sample in example 1 was adsorbed using a Tenax adsorption tube: a mixed sample of petroleum ether and polycyclic aromatic hydrocarbon (1 μ L) was taken with a microinjector and blown into a Tenax adsorption tube under nitrogen flow purging.
(2) The Tenax sorbent tube was tested using a thermal desorption-gas chromatography mass spectrometer.
(3) The test conditions of the thermal analyzer-gas chromatograph-mass spectrometer are as follows:
the instrument comprises the following steps: marks thermal Analyzer, United kingdom, Agilent 7890B-7000C GC gas chromatograph-Mass spectrometer, USA.
Thermal resolution conditions: the desorption temperature is 120 ℃, the desorption time is 5min, the cold trap temperature is 0 ℃, and the desorption is carried out at 300 ℃.
Gas chromatography conditions: chromatographic column HP-5MS (30 × 0.25mm × 0.25 μm), programmed heating, keeping the temperature at 35 deg.C for 10min, heating to 280 deg.C at 5 deg.C/min, and keeping the temperature for 10 min. The transfer line temperature was maintained at 200 deg.C with He as carrier gas and a flow rate of 1.0 mL/min.
Mass spectrum conditions: and (3) bombarding an ionization source by electrons, wherein the electron energy is 70eV, the source temperature is 230 ℃, and a full-scanning acquisition mode is adopted, and the mass range is 40-500 amu.
FIG. 3 is a GC-MS total ion flow chromatogram of comparative example 1. The analysis result shows that only four polycyclic aromatic hydrocarbons, namely acenaphthene, fluorene, fluoranthene and pyrene, are detected, and the chromatogram has more interference peaks brought by petroleum ether.
Claims (16)
1. An adsorption tube for a thermal desorption instrument comprises a tube body and adsorption filler, and is characterized in that the adsorption tube comprises the adsorption tube body and loaded graphene filler; the adsorption tube body sequentially comprises a screen layer, an adsorption resin film layer, an adsorption packing layer, an adsorption resin film layer and a screen layer, wherein the adsorption packing layer is a loaded graphene packing layer; the inner wall of the adsorption pipe body is an inert coating.
2. The adsorption tube of claim 1, wherein the loading length of the loaded graphene packing of the adsorption packing layer is 30-60 mm.
3. The sorbent tube of claim 2, wherein the graphene filler loading length is 35-50 mm.
4. The sorbent tube of claim 1, wherein the mesh layer comprises a glass wool layer and/or a stainless steel mesh layer.
5. The sorbent tube of claim 4, wherein the mesh layer is a combination of a stainless steel mesh layer and a glass wool layer, the glass wool layer being internal to the stainless steel mesh layer.
6. A sorbent tube according to claim 3,
the pore size range of the sieve layer is 100-150 meshes; and/or the presence of a gas in the gas,
the thickness of the screen layer is 1mm-10 mm.
7. A sorbent tube according to claim 6,
the pore size range of the sieve layer is 100-130 meshes; and/or the presence of a gas in the gas,
the thickness of the screen layer is 1-5 mm.
8. A sorbent tube according to claim 1,
the resin film layer comprises a polytetrafluoroethylene film layer.
9. A sorbent tube according to claim 5,
the thickness of the resin film layer is 0.1mm-5 mm; and/or the presence of a gas in the gas,
the pore diameter range of the membrane is 0.1-3 μm.
10. A sorbent tube according to claim 9,
the thickness of the resin film layer is 0.4-1 mm; and/or the presence of a gas in the gas,
the pore diameter range of the membrane is 0.3-1 μm.
11. A sorbent tube according to claim 5, wherein the resin membrane layer comprises 1-9 layers.
12. A sorbent tube according to claim 11, wherein the resin membrane layer is 2-5 layers in film.
13. A sorbent tube according to any one of claims 1-7, wherein the sorbent tube body is a curved conduit.
14. The sorbent tube of claim 8, wherein the inlet and outlet ends of the sorbent tube have a height differential in the range of 5-30mm, wherein the inlet end is lower than the outlet end.
15. The absorption tube according to claim 14, wherein the height difference between the inlet and the outlet of the absorption tube is 15-25 mm.
16. A sorbent tube according to claim 8,
the length range of the adsorption tube body is 80-140 mm; and/or the presence of a gas in the gas,
the diameter range of the adsorption tube is 5-10 mm.
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| CN115372525A (en) * | 2022-07-06 | 2022-11-22 | 重庆市生态环境监测中心 | Sampling detection method based on benzene series adsorption of graphene material and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115372525A (en) * | 2022-07-06 | 2022-11-22 | 重庆市生态环境监测中心 | Sampling detection method based on benzene series adsorption of graphene material and application thereof |
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