LU501729B1 - Sampling Tank for Storing Ambient Air Samples - Google Patents

Sampling Tank for Storing Ambient Air Samples Download PDF

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Publication number
LU501729B1
LU501729B1 LU501729A LU501729A LU501729B1 LU 501729 B1 LU501729 B1 LU 501729B1 LU 501729 A LU501729 A LU 501729A LU 501729 A LU501729 A LU 501729A LU 501729 B1 LU501729 B1 LU 501729B1
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LU
Luxembourg
Prior art keywords
tank
filled
sampling
sampling tank
nitrogen
Prior art date
Application number
LU501729A
Other languages
German (de)
Inventor
Hui Wang
Xiao Liang
Yonggang Zhao
Yuan Li
Xingwei Song
Original Assignee
Env Monitoring Center Of Jiangsu Province
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
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Priority to LU501729A priority Critical patent/LU501729B1/en
Application granted granted Critical
Publication of LU501729B1 publication Critical patent/LU501729B1/en

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/02Devices for withdrawing samples
    • G01N1/22Devices for withdrawing samples in the gaseous state
    • G01N1/2273Atmospheric sampling

Abstract

The invention relates to the technical field of ambient air sampling devices, and specifically to a sampling tank for storing ambient air samples. The sampling tank of the invention is a integrated sphere structure with a gas port and a valve corresponding to it in the upper part of the sampling tank. The inner wall of the tank is coated with a silicon film, and the steps of the coating are as follows: (1) the sampling tank is vacuumed and then filled with nitrogen, and the cycle is repeated until the nitrogen content is more than 99%; (2) in the same way as (1), high-temperature hydrogen is filled until the hydrogen content is more than 99%; (3) the tank is filled with high-temperature silane in the above treatment until a silicon film with a thickness of more than 200 nm is formed on the inner wall of the tank. The sampling tank provided by the invention uses a specific silicon film layer that is passivated, which is passivation inert and adapted to the storage of air samples containing sulfur and bromine components. The sample is free of adsorption in the tank and valve, ensuring the accuracy of the results. It is suitable for a wide variety of ambient air sample collection requirements and has a wide range of applications.

Description

DESCRIPTION LU501729
Sampling Tank for Storing Ambient Air Samples
TECHNICAL FIELD
The invention relates to the technical field of ambient air sampling devices, and specifically to an ambient air sample sampling tank.
BACKGROUND
The sampling bag is very ineffective at collecting low concentrations (100 ppbv) of sulfur-containing VOCs, with samples changing in less than 24 hours.
The sulfur component will react with the electropolished metal surface. Therefore, this sampling bag is not suitable for collecting and storing sulfur-containing VOC samples.
Common sampling tanks used for complex ambient air sampling applications have the following challenges:
Challenge I: It is not resistant to corrosion. Industrial environments or explosion sites have a large number of harmful components such as sulfides, and water molecules in the air combined to form corrosive substances on the inside of the tank walls continue to erode. The interaction generates new substances, so that the collected gas composition changes cause sampling failure, but also causes the effective life of the tank greatly shortened.
Challenge II: It is susceptible to adsorption. The most basic requirement of the sampling tank is that the sample properties do not change. If the collected sample is partially adsorbed in the inner wall of the tank, sampling is also equal to failure.
Therefore, the resistance to adsorption of the inner wall of the tank is very demanding, and the materials that can be found in the market basically do not meet LU501729 this requirement.
Therefore, there is a need to improve on the above-mentioned challenges and invent a corrosion-resistant, non-absorbable sampling tank to meet the needs of collecting and storing ambient air samples.
SUMMARY
In order to solve the above technical problems, the invention provides a sampling tank for storing ambient air samples with a silicon film on the inner wall of the tank, which can ensure that the sample does not adsorb in the tank to further ensure the accuracy of the analytical results.
The sampling tank is a integrated sphere structure with a gas port and a valve corresponding to it in the upper part of the tank.
The steps for coating the sampling tank of the invention are as follows:
S1: The sampling tank is vacuumed, filled with nitrogen, vacuumed, filled with nitrogen again, and so on repeatedly until the nitrogen in the sampling tank accounts for more than 99% of the gas in the tank; the vacuuming and nitrogen filling process are carried out at room temperature; the pressure is maintained at 0.2-0.6Mpa during the nitrogen filling process.
S2: The sampling tank is vacuumed and filled with high-temperature hydrogen gas at 400-600°C; vacuumed again and filled with high-temperature hydrogen gas, and so on repeatedly until the hydrogen gas in the sampling tank accounts for more than 99% of the gas in the tank; the pressure when filling the hydrogen gas 1s 0.2-0.6Mpa.
S3: The tank in S2 is filled with high-temperature silane at 400-600°C until a LU501729 silicon film with a thickness of 200-300 nm 1s formed on the inner wall of the tank; the pressure is maintained at 0.2-0.6 MPa while filling the silane.
S4: Clean the tank. The preferred thickness of the silicon film is 200 to 300 nm; the thickness of the tank is 1.4 to 1.7 mm. The preferred condition is that the tank is resistant to high pressure of more than 1 MPa.
S4 preferred cleaning method is high-pressure vacuum filling nitrogen cleaning, nitrogen filling to maintain the temperature below 60 [J, nitrogen filling when the pressure is maintained at 0.2-0.6MPa; or high pressure under the water spray cleaning, high-pressure water cleaning to maintain the pressure of 0.5 to 0.8MPa.
The advantages of the invention are: (1) The sampling tank of the invention is coated on the inner wall of the tank by a specific process, thus making the silicon film layer passivated and inert and adapted to the storage of air samples containing sulfur and bromine components.
Through the physical performance and functional performance tests, the sampling tank was proved to meet the testing requirements of the standard method for VOCs in ambient air; the gradient difference tests of 12 hours, 24 hours, 48 hours and 72 hours were conducted for 104 VOC standard gases stored in the sampling tank of the present invention, and the results showed that no physical and chemical changes occurred in any of the gases in the tank, which indicates that there is no significant difference in the key performance of the sampling tank in terms of gas tightness and inertness of the inner wall, and the stable storage LU501729 performance is good. (2) The non-adsorption of the sample in the tank and valve ensures the accuracy of the results. (3) The sampling tank of the invention is suitable for various sampling requirements and has a wide range of applications.
BRIEF DESCRIPTION OF THE FIGURES
FIG. 1 is a schematic view of the structure of example 2 of the present invention.
FIG. 2 is a schematic view of the structure of example 2 of the present invention after the addition of a pressure gauge.
FIG. 3 is a top view of example 2 of the present invention.
FIG. 4 is a comparison table of the sampling tank of the present invention with the test results of commercially available sampling tanks (12-hour standard gas test result comparison).
FIG. 5 is a comparison table of the test results of the sampling tank of the present invention with those of commercially available sampling tanks (comparison of the results of 48-hour standard gas test).
FIG. 6 shows a chromatogram of 104 VOCs.
In the figure, 1 - handle, 2 - connecting strip, 3 - ring, 4 - tank, 5 - base, 6 - gas port, 61 - valve, 7 - pressure gauge.
DESCRIPTION OF THE INVENTION LU501729
In order to enable those skilled in the art to fully understand the invention, the invention is further elaborated with specific implementations.
Example 1A
The air sampling tank provided by the invention includes the following structure:
The sampling tank includes the following structure: the tank 4 formed by seamless welding of two hemispheres; the upper part of the tank 4 has a gas port and a valve 6; a pressure gauge 7 is connected to the valve 6; the inner wall of the tank 4 has a silicon film layer, and the coating steps are as follows:
S1: The sampling tank is vacuumed, filled with nitrogen, vacuumed, filled with nitrogen again, and so on repeatedly until the nitrogen in the sampling tank accounts for more than 99% of the gas in the tank; the vacuuming and nitrogen filling process are carried out at room temperature; the pressure is maintained at 0.3Mpa during the nitrogen filling process.
S2: The sampling tank is vacuumed and filled with high-temperature hydrogen gas at 500°C; vacuumed again and filled with high-temperature hydrogen gas, and so on repeatedly until the hydrogen gas in the sampling tank accounts for more than 99% of the gas in the tank; the pressure at the time of filling the hydrogen gas is 0.3 MPa.
S3: The tank of S2 is filled with high temperature silane at 500°C until a silicon film of 250 nm thickness is formed on the inner wall of the tank; a pressure of 0.3 MPa is maintained while filling the silane.
S4: Clean the tank. The specific steps are as follows: the tank is vacuumed at LU501729 a pressure of 0.4Mpa, and then filled with nitrogen at 60°C or below for nitrogen cleaning process.
Tank 4 is made of 316 stainless steel.
The lower bottom of the sampling tank has a circular-shaped base 5, the diameter of the base 5 is smaller than the maximum diameter of the central position of the tank 4; the upper part of the sampling tank has a plurality of connecting strips 2, above the connecting strips 2 has a circular-shaped handle 1; each of said connecting strips 2 is welded to the handle 1 as an integral structure.
There is a gas port 6 on the upper top surface of the tank 4, and the gas port is used for evacuating or filling with gas such as hydrogen or nitrogen right silane gas, and there is a valve 61 and a pressure gauge 7 near the gas port 6.
The process of making the sampling tank is as follows:
The production of the sampling tank consists of the following steps: (1) Tank 4 production: place the 316 stainless steel water in the mold; make two hemispherical shape tank 4, weld the upper and lower part of the tank 4 hemisphere seamlessly, the specific steps are: Weld 1.5 mm thick 316L material half ball by automatic welding machine tungsten protection welding, welding seam than the periphery of about 0.5 thick. (2) Electronic polishing: It will achieve a super mirror effect on the flatness of the inner wall of tank 4. The super mirror effect stainless steel surface will reduce the molecular adhesion of most external gases to the lowest value.
Electropolishing treatment out of the super mirror effect in the physical level can solve more than 99% of the adsorption and corrosion problems. The material used LU501729 for electropolishing is any of ETA-ETR, DTA-ETR, DTA-DTR materials. (3) Silanization treatment: Silane deposition method is applied to the inner wall of tank 4 for polycrystalline silicon film plating treatment. Silicon molecules are very stable in the natural environment, and silicon plating on the super mirror 316 material can further achieve the effect of zero action and zero adhesion of gas molecules, while solving the problem of weld seams. The silanization process is detailed in the coating step process above. (4) Production of base 5 and handle: 304 material, 8mm bar press ring, 1.5mm thick plate circle edge base 5, argon arc welding fixed. (5) Piping and valve 61: EP material 1/4 piping, 316L stainless steel diaphragm valve, with negative pressure function pressure gauge 7, all NPT connections.
Example 1B
The preparation process of the tank is the same as in Example 1A, and the coating steps are as follows:
S1: The sampling tank is vacuumed, filled with nitrogen, vacuumed, filled with nitrogen again, and so on repeatedly until the nitrogen in the sampling tank accounts for more than 99% of the gas in the tank; both the vacuuming and nitrogen filling process are carried out at room temperature; the pressure is maintained at 0.2MPa during the nitrogen filling process.
S2: The sampling tank is vacuumed and filled with high-temperature hydrogen gas at 400°C; vacuumed again and filled with high-temperature hydrogen gas, and so on repeatedly until the hydrogen gas in the sampling tank LU501729 accounts for more than 99% of the gas in the tank; the pressure at the time of filling the hydrogen gas is 0.2MPa.
S3: The tank of S2 is filled with high temperature silane at 400°C until a silicon film of 200 nm thickness 1s formed on the inner wall of the tank; the pressure 1s maintained at 0.2 MPa while filling the silane.
S4: Clean the tank, vacuum at a pressure of about 0.4Mpa, and fill it with nitrogen at 600] or less for nitrogen cleaning treatment.
Example 1C
The preparation process of the tank is the same as in Example 1A, and the coating steps are as follows:
S1: The sampling tank is vacuumed, filled with nitrogen, vacuumed, filled with nitrogen again, and so on repeatedly until the nitrogen in the sampling tank accounts for more than 99% of the gas in the tank; both the vacuuming and nitrogen filling process are carried out at room temperature; the pressure 1s maintained at 0.6MPa during the nitrogen filling process.
S2: The sampling tank is vacuumed and filled with high-temperature hydrogen gas at 600°C; vacuumed again and filled with high-temperature hydrogen gas, and so on repeatedly until the hydrogen gas in the sampling tank accounts for more than 99% of the gas in the tank; the pressure at the time of filling the hydrogen gas is 0.6Mpa.
S3: The tank of S2 is filled with high temperature silane at 600°C until a LU501729 silicon film of 300 nm thickness 1s formed on the inner wall of the tank; the pressure 1s maintained at 0.6 MPa while filling the silane.
S4: Clean the tank. The tank is cleaned by water spray under high pressure of about 0.7MPa.
Example 2
The remaining part of the connecting strip 2 is a vertical strip; the middle of the connecting strip 2 is attached to the outer wall of the sampling tank 4, and the upper part of the connecting strip 2 is attached to the inner wall of the ring-shaped handle 1 and has a one-piece structure; there is an annular ring 3 in the upper part of the outer wall of the sampling tank body 4, and the annular ring 3 is located at the bend of the connecting strip 2. The diameter of the ring 3 is the same as that of the handle 1. There is a gas port 6 at the upper top of the tank 4, and a valve 61 corresponding to it and a pressure gauge 7 are provided near the gas port 6 for reading the gas pressure inside the tank.
The connection strip 2 is in the form of a strip; its material is 316 stainless steel.
Example 3 3.1 The air sampling tank provided by the present invention has excellent storage stability for low levels of sulfur containing VCO (1-20 ppbv) under dry and humid conditions due to its passivated inert surface treatment on the inner surface.
It is more suitable for collecting and storing TO-14 or TO-15 components.
Table 1 Ambient Air Sampling Tank Information
3.2 It is made of 1.5 thick 316L mirror stainless steel semicircle made of tank, LU501729 manually welded, with 1/4 of 316L stainless steel pipe with the same material diaphragm valve (temporarily not installed pressure gauge).
Table 2 Performance Test Results of Manually Welded Sampling Tank
The experiment verified that 1.5 thick 316L stainless steel can basically solve most of the molecular interaction problems, but there is still 0.3%o composition change. The analysis shows that it may be artificially welded at high temperatures to destroy the stability of the material, resulting in a decrease in the corrosion and adsorption resistance of the material around the weld, the standard gas into the interaction and adsorption residue, resulting in experimental failure. 3.3 It is made of 1.5 thick 316L mirror stainless steel semicircle made of tank, automatic welding machine long tungsten protection welding, with 1/4 of the 316L stainless steel pipe with the same material diaphragm valve (temporarily not installed pressure gauge).
Table 3 Automatic Welding Machine Tungsten Protection Welding Sampling
Tank Performance Test Results
The experiment verified that the automatic welding machine tungsten protection welding does effectively solve most of the weld problems, but still some of the standard gas composition has changed. The experimental tank was cut and analyzed to show that the surface finish of the inner wall was not sufficient. 3.4 It is made of 1.5 thick 316L mirror stainless steel semicircle made of tank, automatic welding machine tungsten protection welding, electronic polishing of the inner wall of the tank before welding, to achieve super mirror effect before welding, with 1/4 of 316L stainless steel pipe with the same material diaphragm LU501729 valve (temporarily without pressure gauge).
Table 4 Performance Test Results of Electronically Polished Sampling Tank
The above experiment proves that electropolishing 1s effective. The present inventor judged that the weld problem was not solved thoroughly.
Example 4
The inner inert stability of the sampling tank of the present invention was tested against commercially available sampling tanks. Three parallel examples of
Example 1 of the present invention were tested for 12 hours of standard gas stability, 24 hours of standard gas stability, 48 hours of standard gas stability, and 72 hours of standard gas stability, of which the results of Example 1A are shown in
Table 5.
Table 5 Test Data of Inert Stability Examination of the Internal Wall of the
Sampling Tank of the Present Invention and Commercially Available Sampling
Tanks
Figures 4 and 5 attached are the comparison table of the test results of the sampling tank of the present invention and the commercially available sampling tanks (12-hour standard gas test result comparison); the results are consistent with the results in Table 5.
Figure 6 attached shows the chromatogram of 104 VOCs in Table 5.
The sampling tank of the present invention is significantly superior to commercially available sampling tanks. And the sampling tank of the present invention also has the significant advantage of low cost. Compared with similar commercially available sampling tanks, the production cost of the present LU501729 invention saves about 4,000 yuan per unit.
The sampling tank of the present invention has been tested in terms of physical properties and core functions to demonstrate that it has met the requirements of the standard method for the detection of volatile organic compounds in ambient air.
In terms of physical properties, the inventor has conducted comparison tests from various aspects such as temperature, oxidation, corrosion, pressure resistance, high temperature resistance, and adhesion to meet the requirements of sampling and monitoring of volatile organic compounds in ambient air.
In terms of functional testing, the inventors conducted gradient difference tests of 12 hours, 24 hours, 48 hours, and 72 hours for 104 VOC standard gases stored in the sampling tank of the present invention, and the results showed that none of the gases in the tank underwent physicochemical changes. The sampling tanks of the present invention showed no significant differences in key properties such as gas tightness and inertness of the inner wall, and good stable storage performance.
In terms of manufacturing process, the invention can manufacture tanks of different sizes in multiple sizes such as 3L, 6L and 12L as needed through key steps such as mechanical forging, automatic welding, electronic polishing, nano-coating, vapor deposition and silanization treatment.
In addition, the test data of Example 1B and Example 1C are close to
Example 1A, and there is only a small difference in the determination of different substances, and the difference is within the allowable error range.
It proves that the LU501729 physical and functional properties of the tanks manufactured under the coating process of the present invention are close, and will not be presented here for analysis.

Claims (10)

CLAIMS LU501729
1. The sampling tank for storing ambient air samples has an integrated spherical structure with a gas port and a valve corresponding to it in the upper part of the sampling tank.
2. The sampling tank for storing ambient air samples as claimed in claim 1, wherein the inner surface of the sampling tank is coated with a silicon film. The steps described for coating the sampling tank are as follows: S1: The sampling tank is vacuumed, filled with nitrogen, vacuumed, filled with nitrogen again, and so on repeatedly until the nitrogen in the sampling tank accounts for more than 99% of the gas in the tank. S2: The sampling tank is vacuumed and filled with high-temperature hydrogen; vacuumed again and filled with high-temperature hydrogen, and so on repeatedly until the hydrogen in the sampling tank accounts for more than 99% of the gas in the tank. S3: The tank in S2 is filled with high-temperature silane until a silicon film with a thickness of 200 nm or more 1s formed on the inner wall of the tank. S4: Clean the tank.
3. The sampling tank for storing ambient air samples as claimed in claim 1 or 2, with a silicon film thickness of 200 to 300 nm; a wall thickness of 1.4 to 1.7 mm, and a tank resistant to high pressure of 1 MPa or more.
4. The sampling tank for storing ambient air samples as claimed in claim 2, wherein S1 is vacuumed and nitrogen filled at ambient temperature.
In S1, the pressure is maintained at 0.2-0.6 MPa during nitrogen filling LU501729 treatment.
5. The sampling tank for storing ambient air samples as claimed in claim 2, wherein S2 is first vacuumed at ambient temperature.
6. The sampling tank for storing ambient air samples as claimed in claim 2, wherein S2 is filled with high temperature hydrogen gas at 400 to 600°C.
7. The sampling tank for storing ambient air samples as claimed in claim 2, wherein S2 is filled with hydrogen gas at a pressure of 0.2-0.6 MPa.
8. The sampling tank for storing ambient air samples as claimed in claim 2, wherein S3 is filled with high temperature silane at 400 to 600°C and the pressure is maintained at 0.2-0.6 MPa when the silane is filled.
9. The sampling tank for storing ambient air samples as claimed in claim 2, wherein S4 is cleaned by high-pressure vacuum filling with nitrogen, maintaining the temperature below 60°C when filling with nitrogen, and maintaining the pressure at 0.2-0.6 MPa when filling with nitrogen. Or it is cleaned by water spray under high pressure, and the pressure is maintained at 0.5 to 0.8 MPa when high pressure water cleaning.
10. The sampling tank for storing ambient air samples as claimed in claim 2 as follows: S1: The sampling tank is vacuumed, filled with nitrogen, vacuumed, filled with nitrogen again, and so on repeatedly until the nitrogen in the sampling tank accounts for more than 99% of the gas in the tank; the vacuuming and nitrogen filling process are carried out at room temperature; the pressure is maintained at LU501729
0.2-0.6Mpa during the nitrogen filling process. S2: The sampling tank is vacuumed and filled with high-temperature hydrogen gas at 400-600°C; vacuumed again and filled with high-temperature hydrogen gas, and so on repeatedly until the hydrogen gas in the sampling tank accounts for more than 99% of the gas in the tank; the pressure when filling the hydrogen gas 1s 0.2-0.6Mpa. S3: The tank in S2 is filled with high-temperature silane at 400-600°C until a silicon film with a thickness of 200-300 nm 1s formed on the inner wall of the tank; the pressure is maintained at 0.2-0.6 MPa while filling the silane.
LU501729A 2022-03-25 2022-03-25 Sampling Tank for Storing Ambient Air Samples LU501729B1 (en)

Priority Applications (1)

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LU501729A LU501729B1 (en) 2022-03-25 2022-03-25 Sampling Tank for Storing Ambient Air Samples

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
LU501729A LU501729B1 (en) 2022-03-25 2022-03-25 Sampling Tank for Storing Ambient Air Samples

Publications (1)

Publication Number Publication Date
LU501729B1 true LU501729B1 (en) 2023-09-25

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Family Applications (1)

Application Number Title Priority Date Filing Date
LU501729A LU501729B1 (en) 2022-03-25 2022-03-25 Sampling Tank for Storing Ambient Air Samples

Country Status (1)

Country Link
LU (1) LU501729B1 (en)

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Effective date: 20230925